Sol for applying sol-gel coating on surface, method of applying sol-gel coating, preparation method thereof and use

FIELD: chemistry.

SUBSTANCE: invention relates to sol for applying sol-gel coating onto a surface. The sol contains at least one organometallic compound of zirconium, aluminium or titanium, at least one organosilane compound, at least one compound selected from acids, bases, glycols and ethoxy ethanol as a catalyst. The sol also contains demineralised or distilled water. The total amount of at least one organometallic compound of zirconium, aluminium or titanium and at least one organosilane compound is greater than 50%. The sol also contains less than 5% harmless organic solvent such as non-toxic aliphatic alcohols. The sol also contains at least one surfactant and organic binder. The invention also relates to a set comprising a first container which contains a first portion in form of liquid which contains at least one organometallic compound of zirconium, aluminium or titanium, at least one compound selected from acids, bases, glycols and ethoxy ethanol, and a second container which contains a second portion in form of a liquid which contains an organosilane compound. The sol-gel layer is obtained by depositing the said sol onto a substrate. The layer is dried to obtain a sol-gel layer on the substrate. The sol-gel layer is used to endow the surface of the substrate with corrosion resistance. The surface of the substrate can have one or more sol-gel layers.

EFFECT: method enables obtaining the desired coating thickness without deterioration of anti-corrosive properties, as well as obtaining a coating with uniform thickness without overlapping.

65 cl, 2 ex

 

The technical field

The invention relates to solo for applying the Sol-gel coating on the surface, more specifically, on the surface containing the metal or metal alloy, preferably on the surface, formed from metal or metal alloy.

Similarly, the invention relates to a method of applying a Sol-gel coating on the surface, more specifically, on the surface containing the metal or metal alloy, which uses the above described Sol.

The level of technology

The technical field of the invention in a broad sense can be defined as the area of technology related to the processing surfaces, obtained from a metal or metal alloy, such as, in particular, to a coating on the surface, obtained, for example, from metal or metal alloy, such as titanium, aluminium and their alloys, which are used in particular in the aviation industry.

More specifically, the invention relates to the field of surface coatings, known under the name of Sol-gel surface coatings on the surfaces of substrates made of, for example, from metals or metal alloys, in order to give the surface characteristics of the chemical and/or mechanical resistance, such as resistance to corrosion and abrasive is the first resistance, and/or for the promotion of adhesion to the substrate, e.g. made of metal or alloy, a layer of organic coating, such as a layer of primer, paint, mastic, glue or resin; in this case, the function of the Sol-gel coating such functions are commonly used conversion processing or adhesion promoters.

The conversion processing result (surface) structural modification of the metal substrate (aluminum alloys, titanium and other metals) by way of electroplating (electrolysis, for example, anodic oxidation using chromium, sulfuric or phosphoric acid) or by way of a simple chemical transformations (e.g., chromate or phosphate).

Anodizing makes it possible growing very strongly cohesive layer of oxide (or hydroxide) due to the metal framework, with the above-mentioned layer is placed in the position of the anode. In particular, in the case of aluminum alloys bath chromic acid lead to the formation of thin (a few microns) layer, which is porous and demonstrates a good capacity for adhesive connection with organic coatings.

Among the methods of chemical chromate conversion makes possible the formation of very strongly cohesive thin deposited layer of chromium metal in the injection surface is exposed STI processing component (usually aluminum alloys, zinc or steel) in contact with acid solution on the basis of dichromate and fluorine-containing activators. This treatment improves the corrosion resistance of the substrate, and it is also used as the basis for the linking of colors.

These surface treatments many shortcomings, particularly in relation to their impact on the environment, due to the use of strong acids or bases and toxic materials such as chromates, immersion tanks.

This is due to the fact that these methods require the use of significant quantities of water to remove subjected to processing components of excess amounts of working solutions for processing; wash water and waste technology solutions must be processed in order to remove dissolved metals, before the solutions will be sent for recycling or reuse; removing metals results in additional toxic wastes that are difficult to clean and recycle.

The entire array of data processing, following the implementation of the methods, increases the cost of using conventional wet chemistry methods.

Similarly, the components are subjected to processing at the end of their service life or phases is vosstanovleniya, become a source of toxic wastes that are harmful to users.

Accordingly, methods have been proposed that use the technique of applying the Sol-gel coating in order to eliminate the disadvantages of the above-mentioned liquid chemical methods. Such methods are described in particular in documents US-A-5814137, US-A-5849110, US-A-5789085, US-A-5869141, US-A-5958578, US-A-5869140, US-5939197 and US-A-6037060.

In the document US-Bl-6605365, in particular, describe the use of sols containing derived alkoxysilane, such as Tetra-n-propoxycarbonyl (TPOC), and organosilane, such as 3-glycidylmethacrylate (GTMS), together with the catalyst based on an organic acid such as acetic acid.

Sols are vysokorazvetvlennyi sols, characterized, for example, the level of solids magnitude in the range from 3% to 5%; for the case of higher concentrations mentioned problems with adhesion of the film.

Data diluted sols make possible the deposition of thin layers or films, having a thickness in the dry state, for example, in the range from 200 up to 500 mm, as a result of prolonged stay in contact with the surface. The obtained film is actually well-bonded to substrate and makes possible the subsequent adhesion primer or paint, but not found what supports its own characteristics corrosion resistance.

In other words, this document refers to the films of adhesion promoters and did not mention the presence of specific anti-corrosion properties inherent in the Sol-gel film and an integral associated with it, in combination with the application of concentrated products by way of sputtering.

And finally, in the case of paint, primer, glue or mastic their application must be for a very short period of time after drying of the film.

In the document US-A-5814137 describe the surface treatment for metal surfaces, formed, in particular, alloys of titanium or aluminum, which is used as a Sol-gel film to obtain a surface coating that is used as the interfacial surface to improve adhesion between the metal and the organic resin or glue.

The Sol-gel film applied by itself, provides mild corrosion resistance or not provide it at all and promotiom adhesion using ORGANOMETALLIC sizing on the metal surface.

The Sol used for the Sol-gel film on the surface of the metal substrate; the Sol is a diluted solution of stable ORGANOMETALLIC salt alkoxysilane, such as tetraisopropoxide or t the tra-n-propoxycarbonyl (TPOC), organosilanols sizing, such as 3-glycidylmethacrylate (GTMS)for epoxy or polyurethane systems or the appropriate primary amine to polyimide compositions and catalyst, such as acetic acid, to the aqueous composition. Also describes and structures on the basis of alcohol.

The Sol is applied on the metal surface by immersion, spraying or dipping and then dried to obtain a Sol-gel film.

Sol is a dilute solution in the sense that the concentration of reagents in the ash are 2% (vol.) GTMS and 1% (vol.) TPI; but it is noted that the best results can give a slightly higher concentration of reactants, namely, the total concentration of TPI and GTMS, equal to 4.4%.

The amount of acetic acid, which mainly functions as a catalyst for hydrolysis, is 0.13 mol of glacial acetic acid at 0,091 mole organosilane - doubling the concentration of acetic acid to 0.26 mol leads to improved adhesion, but the transition to 0.39 mol leads to its deterioration.

In conclusion, it is pointed out that the amount of acetic acid is preferably minimized.

In column (13) of this document mention the ashes, which is a solution in isopropanol 2% GTMS, 1% of TPI and 1% acetic acid with conc is of 80%.

To obtain the Sol-gel coating that can reach a thickness up to several tens of microns, in the case of the methods and solutions described in the above documents are necessary sequential deposition of two or more layering on each other layers and/or spray or continuous irrigation, since the thickness per one layer at deposition, small.

Through the use of a substantial number of stages required for the deposition of coatings with adequate thickness, Sol-gel processing described in these documents, it is difficult to use on an industrial scale and can be inserted into the sequence of chemical steps of processing a metal surface only when investing considerable expense and with considerable loss of performance.

In addition, the Sol-gel film obtained in the above-mentioned documents and used by themselves, i.e. without primers, still find unsatisfactory performance in regard to corrosion protection, which is determined in the test for resistance to saline mist or resistance to filiform corrosion.

Other composition of the sols used to gain Sol-gel coatings are described in documents US-A-484017 and US-A-4754012. These sols inherent disadvantage of high levels of organic solvents.

Even among other documents relating to the compositions, intended for the production of Sol-gel coatings are the documents US-A-6008285, US-B1-6228921 and US-B1-6482525 and US-B1-6361868. In these documents and, in particular, the first three of these again describe compositions characterized by high levels of organic solvents. In addition, a significant objective of the obtained coatings is to make the substrate of polycarbonate resistance to scratching that appropriately involves pre-processing of polycarbonate using silane.

Summarizing the above, we can say that the dry residue of the earlier text is that the shortcomings of the sols and Sol-gel methods of the prior art in substantially its source have the presence of high levels of solvents and/or complexity and/or poor corrosion performance specifications alone, the Sol-gel film.

Therefore, in light of the foregoing there is a need in the ashes or the solution and the method of surface treatment, for example a metal surface, which would make it possible to obtain a Sol-GE is avago coverage, characterized by a relatively substantial thickness in the dry state and the corresponding requirements and consider the case when using a limited number of stages.

There is also a need in the ashes or the solution and the surface finish is obtained, for example, of metal, which would make it possible to obtain the Sol-gel coating, which would have improved corrosion resistance, which is determined, in particular, with the use of tests when processing with exposure to salt fog.

This enhanced protection must be achieved without compromising other properties of the Sol-gel coating, described in particular in documents mentioned above and includes, for example, adhesion to the carrier, for example, metal media, flexibility, resistance to filiform corrosion, adhesion of primers and paints to the Sol-gel coating and the resistance to scratching, chemical resistance and wear resistance.

Also, there is a need in the ash, which is characterized by low or zero content of the solvent, in particular in regard to harmful or toxic solvents, and in regard to other compounds, which could have adverse effects on the environment.

In conclusion, there is a need for a method of producing the Sol-Geleva the coating on the surface, for example, a metal surface, which would be simple, reliable, easy to implement, which would include a limited number of stages and which could easily be integrated into existing methods of surface treatment, such as metal surfaces, without causing any significant modifications of these methods and provide low levels of investments.

Disclosure of the invention

The purpose of the invention is to offer Zola, which is intended for applying the Sol-gel coating on a surface such as the surface containing the metal and method of producing the Sol-gel coating on the surface, for example surface containing the metal or metal alloy, which uses the above-mentioned Sol, which, inter alia, correspond to the previously presented requirements and that meet the criteria and requirements mentioned earlier in this document.

An additional objective of the invention is to offer Zola and method designed to obtain a Sol-gel coating on the surface, for example surface containing the metal or metal alloy, which is not peculiar to the drawbacks, defects, limitations and flaws of the sols and methods of the prior art and which solves the problems of the sols and methods of the prior art.

This objective and other objectives and in accordance with the invention are achieved with Zola for applying the Sol-gel coating on the surface, these Sol contains, wt%:

a) from 3% to 30%, preferably from 5% to 20%, more preferably from 7% to 15%, in particular from 8% to 14%, more particularly from 10% to 13%, for example 10,8% or 12%, of at least one ORGANOMETALLIC compound of zirconium, aluminum or titanium;

b) from 5% to 50%, preferably from 5% to 40%, more preferably from 10% to 40%, particularly from 15% or 20% to 30%, for example 22% or 23%, of at least one organosilane connection;

c) from 1% to 15%, preferably from 2% to 10%, more preferably from 3% to 8%, for example 5%, of at least one compound selected from acids, bases, glycols and ethoxyethanol;

d) the remainder to 100% in demineralized or distilled water,

while the total number of a) and b) is equal to, greater than 30%, preferably greater than 31,2%; 31,5%; 32% or 33%, more preferably greater than 35%, in particular greater than 40%, more particularly greater than 50%.

The earlier mass percentage in the General case is equivalent to the volumetric percentage of the contents.

Preferably the above-mentioned Sol contains less than 5%, predpochtite is) less than 3%, more preferably less than 1 wt.%, non-toxic or harmless organic solvents, preferably selected from alcohols, such as non-toxic or harmless1-C10aliphatic alcohols, such as isopropanol.

Sol, corresponding to the invention, in principle differs from the sols of the prior art, such as those described in the documents mentioned earlier in this document, in the sense that the concentration of components a), b) and C), namely ORGANOMETALLIC compound, organosilane and catalyst, such as acid, significantly above the concentrations used in these documents. In addition, the total number of - concentrated - a) and (b) is an amount greater than 30%, significantly higher than the total concentration of (a) and (b) prior art.

This increase in the concentration carried out due distilled or demineralized water. In accordance with this, the concentration of the ORGANOMETALLIC compound, such as TPI, is in the range from 3% to 30 wt.%, while in the prior art it does not exceed 1.25 wt.%; similarly, the concentration of organosilane compounds, such as GLIMA, is in the range from 5% to 50 wt.%, while in the prior art it is e more than 2.50 wt.%; in conclusion, the concentration of the catalyst, for example an acid catalyst such as acetic acid, is in the range from 1% to 15 wt.%, while it does not exceed to 0.60 wt.% in the prior art.

Similarly, a significant increase in the number of each component in the case of the sols of the invention is demonstrated by the increased value of the level of bulk solids, which changes from a value in the range from 2% to 4% for the sols of the prior art to values greater than 4%, and may, for example, goes up to 37%, preferably to values in the range of from 4% to 37%, more preferably to values in the range of from 18% to 37%, in particular from 20% to 30%.

Increasing the concentration of compounds that can be defined as compounds, the precursors for the Sol-gel coating, namely ORGANOMETALLIC compound and organosilane compounds, specifically, achieve due to the increase in the percentage content of component (C), for example, acids, such as acetic acid, which concentrated mixtures makes it possible to achieve compatibility and solubility with simultaneous essentially the absence of bands of the same ratios between the amounts of ORGANOMETALLIC compound (a) and organosilanols soy is inane b), as in the documents mentioned earlier in this document.

The ratio organosilane compounds and ORGANOMETALLIC compounds in General is in the range from 1.5 or 1.6 to 6, preferably from 1.8 to 2.5.

In the light of the documents of the prior art is absolutely unclear what could be obtained concentrated sols of this type; indeed, the entire range of these documents largely tends to dissuasion practice in requiring the use of high concentrations of components a) and b) and component (C), such as acetic acid. In particular, in the document US-B 1-6605365 indicate problems with adhesion in the case of concentrated sols, such as nuclei, characterized by the level of solids, greater than 4% or 5%.

Therefore, in case of increasing concentrations of the components a), b) and (C) providing to the excess of the total quantity or concentration of a) and b) 30%, preferably exceeding 31,2%; 31,5%; 32% or 33%, without the use of additional organic solvents or co-solvents or using a very small share of inventors go against the widespread point of view in the art and demonstrate that, surprisingly, but sols which are stable is ini and easy to use, can be obtained even at high concentrations by increasing simultaneously with the concentration of components (a) and (b) the concentration of component (C), for example acid), distilled or demineralized water.

Sols corresponding to the invention, surprisingly, and, specifically, due to its high concentration makes it possible to obtain dry Sol-gel films having a relatively high thickness generally in the range from 500 mm to 20 microns or even more, depending on the composition, preferably from 1 or 2 to 10 μm, more preferably from 4 to 5 microns. This thickness will receive in a single layer in one operation of the application (or pass) in accordance with methods such as dipping, spraying or sputtering. Films of this type can be obtained with the use of the sols of the prior art only in the sequential deposition of two or more layers, and during the several operations of the application.

In addition, the films obtained from the concentrated sols, corresponding to the invention have excellent quality and, in particular, have a uniform thickness without flows.

Increasing the concentration of the sols, corresponding to the invention, achieved without increasing the content of organic solvent; this is due to the fact that h is about sols, corresponding to the invention, in contrast to many of the sols of the prior art, contain less than 5 wt.%, preferably less than 3 wt.%, more preferably less than 1 wt.%, organic solvents.

In addition, in the case of inclusion of organic solvents of this type in the composition of the invention under these very low concentrations of the considered solvents are non-toxic or harmless solvents, such as alcohols, preferably1-C10and especially With1-C4, aliphatic alcohols, such as isopropanol.

In particular, by increasing the thickness in the dry state per layer during the deposition, which is in the range of, for example, from 0.5 to 2, 3, 4, 5 or even 20 μm or more in the General case, instead of a few hundred nanometers in the prior art, the Sol-gel films obtained from sols, corresponding to the invention significantly improves its own performance characteristics for corrosion protection in comparison with what takes place in Sol-gel films obtained from the sols of the prior art.

Thus, by way of example, you can say that depending on the brand of aluminum or metal considered and substrate in accordance with the temperature of the drying angry the gel film, which may be in the range from 0 to 500°C, preferably from 80 to 150°C., more preferably from 110 to 130°C., and which, in the case of treatment with fusion ceramics, can reach even up to 2500°C, in the case of Sol-gel films obtained using Zola, corresponding to the invention, it is possible to achieve levels of protection when exposed to salt fog in the range from several tens to several hundreds or even thousands of hours (tested in accordance with ASTM B). In order of matching with the Sol-gel coatings of the prior art can be said that the resistance to salt fog only one Sol-gel film is less than 24 hours on a medium aluminium T, who had previously been subjected to deoxidation.

Excellent results were also obtained in respect of filiform corrosion.

In other words, demonstrated that the film corresponding to the invention allows to achieve corrosion protection provided by the action of the protective layer due to the presence of the film itself, and allows you to do despite the fact that in the film, corresponding to the invention, no corrosion funds do not include.

This excellent level of protection achieved in the presence of one tol is to the Sol-gel film, provided in the case of film, the thickness of which in the dry state in General is in the range from 500 nm to 20 μm, comprising, for example, 1, 2, 3, or 4 microns, without deterioration of the properties traditionally exhibited Sol-gel films and described, in particular, in the above-mentioned documents of the prior art, namely adhesion to a wide range of media, such as aluminum, titanium, stainless steel, composite materials, plastics, glass and the like, which may be subjected to preliminary treatment; flexibility; adhesion of primers and paints to the Sol-gel film, but also the resistance to scratching; chemical resistance; wear resistance, and the like.

One additional benefit of "concentrated" Zola, corresponding to the invention lies in the fact that it has a much wider scope in comparison with dilute sols of the prior art, described in particular in documents mentioned earlier in this document.

This is because the sols, corresponding to the invention can be used not only for producing Sol-gel coatings, which are bonded products chromate conversion or adhesion promoters for paints, mastics, and adhesives, as argued in the above documents is about and also to obtain a Sol-gel coatings, the Sol-gel paint and Sol-gel coatings for special applications.

Similarly the invention provides a method of obtaining a Sol-gel layer on the surface of the substrate, where

- Sol, described earlier, are precipitated on the surface to obtain on the surface of the substrate layer Zola;

- mentioned layer Zola dried to obtain on the surface of the substrate by the Sol-gel layer.

The Sol can be precipitated using any known deposition method such as sputtering, spraying or dipping.

Preferably, the Sol is applied in the spray on a very simple way, similar to that used when applying paint or varnish.

The method corresponding to the invention, detects all the advantages resulting from the use of Zola, corresponding to the invention and described earlier in this document; in particular, the method corresponding to the invention makes it possible to obtain layers having a greater thickness in the dry state, namely in General in the range from 500 nm to 20 μm, in one stage, in one move (one pass), instead of two or more stages in the methods of the prior art in which the use of dilute sols. The result is a significant gain in time. By way of example, you can say that a film having the first thickness in the range from 2 to 10 μm, you can apply for a few seconds by the method similar to that used in the varnish or paint.

Similarly, for the case of the method of the invention to achieve the deposition of a layer having the same thickness, there is no need for irrigation or continuous spraying as described in certain documents of the prior art.

Obtain the desired thickness of the deposited layer in a dry state can be easily achieved in the modification, for example, facilities for spray or spray type dispenser, the amount of data sprayers and distance when applying. A thick layer of very long without being in contact or irrigation. Received a thick layer characterized by excellent quality, homogeneity, and lack of flows.

Therefore, the method corresponding to the invention is simple, reliable, fast and less expensive in comparison with what takes place in the methods of the prior art. This method of obtaining a Sol-gel layer corresponding to the invention, can be easily built in a conventional existing production line, which includes other options for processing the substrate before or after receipt of the Sol-gel layer, at low cost, without any doubt is any significant modifications or loss of performance.

In conclusion, the method corresponding to the invention, is harmless from the point of view of ecology and complies with the latest regulations related to environmental protection, due to the fact that Sol is characterized by a very low content of organic solvent, generally less than 5 wt.%, preferably less than 3 wt.%, more preferably less than 1 wt.%, and that these solvents are solvents that are neither toxic nor harmful, such as alcohol.

This is the difference and the added advantage of being detected when comparing Zola and method of the invention and methods of the prior art, which utilize the elevated levels of solvents, which in some cases are toxic, harmful and flammable.

In the best case, the Sol pre and/or during deposition can be heated; it was found that this heating makes it possible, in particular, the catalysis of a reaction that proceeds in the ashes, and improved acceleration - pass hydrolysis, drying and coating, as well as improving the quality and uniformity-uniformity for the resulting film.

Such heating may be particularly advantageous in the case of repairs or repairs to already with westwoodi Sol-gel film, because this significantly reduces the aging time. In addition, preferable and much easier is to conduct heat damage Zola than the substrate on which the Sol must be applied, since the size and geometry of the substrate may be such that they impede the conduction of heat.

Such heating is particularly advantageous in the case of selection organosilanols connection, as will be seen later in this document, from among the compounds for which the hydrolysis reaction does not lead to the formation of methanol. The reason for this is that the hydrolysis of these compounds is slower, and the heat makes it possible acceleration; furthermore, the controlled heating can also improve the quality of the film obtained from Zola.

Therefore, the Sol can be applied at temperatures in the range from 0 to 80°C, preferably from 20 to 60°C.

In the best case, the Sol can be filtered prior to its application. This filtering can be performed, for example, as a result of placing the filter in front of the spray or spray nozzle or any other system application.

This filtering can be a commonly used filter or finer filtration, such as ultrafiltration or nanofiltration, and it can be done on the Sabbath. ispolzovanie any device, well-known specialist in the relevant field of technology.

The purpose of this filtering is to hold any impurities, generally having a size ranging from several nanometers to 20 microns.

The reason for this lies in the fact that it was found that the operation of the filter leads to a significant improvement in the quality of the obtained film. The quality of the resulting mesh is actually improving as a result of the removal of any impurities present in the ash due to the operation of the filter.

Because the quality of the resulting mesh is of paramount importance in regard to the characteristics of corrosion resistance, respectively, as a result of this filtering will be improved and data properties.

In one preferred particularly advantageous variant of the method corresponding to the invention, the Sol precipitable (applied to the surface of the substrate, receive (prepared) as a result of simple mixing, optional when heated under the conditions specified earlier in this document, only two, concentrated, liquid products such as parts, called part a and part B, while in the prior art, a certain, for example, in most of the above documents, the Sol produced by mixing h is four or even more products or component parts.

Part a, which is present in the form of liquid, contains components (a), (C) and (d) Zola, which have already been described, while part b, which is also present in the form of liquid contains the component (b) Zola, which has already been described.

These two liquid components (part a and part b) is very easy to mix when using conventional mixing devices and even manually in case of small quantities.

The duration of mixing in General is in the range from 5 minutes to 1 hour. In the General case, the mixing can be conducted at a temperature in the range from 20 to 80°C, depending on the desired rate of hydrolysis.

Two parts a and b are stable during storage, and in the General case each of them is placed in suitable for packaging or container for periods of time in the General case lasting from several months to two years, making the necessary possible simple homogenization before use. A mixture of two parts a and b is also stable.

After mixing the above-mentioned parts a and b obtained by the Sol can be applied over a period of time in the General case duration from 0 minutes to 24 months, preferably from 0 minutes up to 12 months, more preferably from 30 minutes to 8 hours, for example over a period of time, or smaller p the ate 1 hour counting from the start of mixing.

In addition, the invention provides a kit including

the first container or packaging containing the first part And, in the form of a liquid containing components a), C) and d),

the second container containing the second part, in the form of a liquid containing the component (b).

For example, the part may consist of pure liquid silane.

Part a in the range of from 50% to 90%, preferably from 60% to 90 wt.%, from the obtained final product in the form of Zola, and part of it In General ranges from 10% to 50%, preferably from 10% to 40 wt.%, from the obtained final product in the form of Zola. The kit of this type is convenient in storage and in use.

The invention also provides a Sol-gel layer obtained by the above method, and the substrate or the product, at least one surface of which is coated in the form of at least one Sol-gel layer. Examples of these substrates or products, such as aircraft.

In addition, the invention relates to the use of the above-mentioned Sol-gel layer obtained by the method corresponding to the invention, to impart corrosion resistance to the surface of the substrate, in particular a surface obtained from a material selected from metals, metal alloys and composite is of materials, containing the metal or metal alloy.

In the best case, the above-mentioned surface put only the coating in the form of the above-mentioned Sol-gel layer; in other words, on the surface using only one mentioned Sol-gel layer.

The reason for this is that, as has been discovered, the Sol-gel layer, corresponding to the invention or obtained by the method corresponding to the invention, surprisingly, but by itself, without any other covering of paint, primer or other of the coatings makes it possible making this surface corrosion resistance. This eliminates the deposition of other layers and results in saving money, time and reduce mass that is of particular interest, for example, in the field of aviation.

In addition, the invention provides a method of obtaining a coating comprising two or more layers on the surface of the substrate, with at least one of the data layer is a Sol-gel layer obtained by the method described previously.

In particular, the invention additionally provides a method of obtaining a coating comprising two or more layers, on the surface of the substrate, where

- on these surfaces receive the Sol-gel layer; then

- mentioned Sol-gel layer is applied one or more other layers, these other layers is chosen, for example, of layers of paint, primer, mastic, glue or resin.

The said layer or layers other than the Sol-gel layer can be applied to the Sol-gel layer immediately after its receipt, and after drying, or the said layer or layers can be applied to the Sol-gel layer within a certain period of time after its receipt, for example during the period of time ranging from one month to ten years.

The reason for this is that, since the Sol-gel layer itself has anti-corrosive properties, there is no need for immediate supply of other layers, such layers can be obtained subsequently, during repair or inspection where it is appropriate, after easy cleaning.

The coating may include two or more identical or different Sol-gel layers selected from, for example, Sol-gel layers with specific properties, described later herein, and optionally one or more other layers, select, for example, of layers of paint, primer, mastic, glue or resin.

The invention will be better understood after reading the following further detailed description, which is essentially due to the method of obtaining a Sol-gel with the HH on the surface of the substrate.

This method first involves the deposition on said surface Zola in order to obtain on the surface of the substrate layer Zola.

Substrate corresponding to the invention, may be any material capable of receiving the Sol-gel layer. The method corresponding to the invention, used for very dissimilar materials while obtaining excellent results, expressed through the properties of the resulting layer.

In the General case, the substrate is produced from a material selected from metals; metal alloys; organic or inorganic mineral glass; and organic materials such as plastics; wood; paper; ceramics; textiles; concrete; stone and composite materials composed of two or more of these materials. These optional materials can be subjected to the cladding and/or the surface treatment and/or coating, for example colouring.

In particular, the substrate material can be selected from aluminum; titanium; copper; iron and their alloys, such as steel, for example stainless steel, and Inconel".

Aluminum alloys include brand 6056, 2024 and 7075.

Titanium alloys include alloys of Ti-6-4, Ti-15-3-3-3 Ti-6-2-2-2-2 and Ti-3-2 .5.

The substrate can take any shape, but in the General case takes the form of plate, sheet or foil. However, the method corresponding to izopet the tion, makes possible the deposition of layers on surfaces, even characterized by the geometry of high complexity. The surface on which the precipitated layer may represent only part of the total surface of the substrate, but also can represent all the said surface as a whole; for example, when using a method corresponding to the invention, the layer can be beset on both the front surface of the substrate in the form of foil.

Before deposition of ash on the surface of the surface in the General case, it is preferable to clean and/or aktivirovannoi and/or etching, for example, as a result of chemical and/or physical and/or mechanical processing.

This is due to the fact that this cleaning is critical for effective adhesion layer, which was besieged. These methods of cleaning professionals in the relevant field of technology known: they may include cleaning by a wet method, for example, using acidic or basic solutions, or degreasing using alkali or solvent or cleaning using a dry method, for example, when using shot blasting and/or sand blasting machines and/or processing of the flame (fire of processing).

For specific media you can add specific processing related to the type of promoting adhesion.

About isaudio and/or activating the processing of this type of specialists in the relevant field known in the art and widely described in the prior art, more specifically, in the documents of the prior art mentioned earlier in this document, such as document US-A-5869141, whose description can be used for reference.

On the surface optionally can be coated as a layer obtained by the surface treatment chosen from simple and chromate conversion layers, anodizing layers or other layers, it is, in particular, in the context of the renovation of existing materials. Therefore, the surface of this last layer is the surface on which the precipitated Sol.

On the surface, is preferably subjected to a cleaning and activating, precipitated Sol, which is in accordance with the invention is a concentrated colloidal solution containing the following compounds, the number of which is expressed in mass percentage content of:

a) from 3% to 30%, preferably from 5% to 20%, more preferably from 7% to 15%, in particular from 8% to 14%, more particularly from 10% to 13%, for example 10,8% or 12%, of at least one ORGANOMETALLIC compound of zirconium, aluminum or titanium;

b) from 5% to 50%, preferably from 5% to 40%, more preferably from 10% to 40%, particularly from 15% or 20% to 30%, for example 22% or 23%, of at least one organosilane connection;

c) from 1% to 15%, preferably from 2% on the 10%, more preferably from 3% to 8%, for example 5%, of at least one compound selected from acids, bases, glycols and ethoxyethanol;

d) the remainder to 100% in demineralised or distilled water;

while the total number of a) and b) has a value of greater than 30%, preferably greater than 31,2%; 31,5%; 32% or 33%, more preferably greater than 35%, in particular greater than 40%, more particularly greater than 50%.

The Sol corresponding to the invention, is concentrated Sol, in which in comparison with the sols of the prior art, the level of bulk solids in General is in the range from 2% to 4%. Sol, corresponding to the invention, generally characterized by the level of bulk solids, greater than 4%, and may, for example, goes up to 37% or more; preferably, the content of the solid phase is in the range from 4% to 37%, more preferably the level of solids is in the range from 18% to 37%, and more preferably from 20% to 30%.

In comparison with the sols of the prior art various components a), b) and C) are characterized by their significantly increased concentrations; in particular, the increase in the percentage content of component (C), for example acids, in Kosovo the total composition makes it possible to achieve compatibility and solubility data in concentrated mixtures for higher concentrations of components a) and b).

However, the ratio of ORGANOMETALLIC compound (a), such as TPI, and organosilane compounds, such as GLIMA, remains within the same proportions as in the prior art. In a broad sense, the ratio organosilane compounds, such as GLIMA, and ORGANOMETALLIC compounds, such as TPI, is in the range from 1.5 or 1.6 to 6, preferably from 1.8 to 2.5.

Obviously, the degree of dilution, that is, the amount of solvent (a), for example water, is included in the Sol, corresponding to the invention, can be adjusted depending on the desired operational characteristics and thickness. Similarly, the ratio of ORGANOMETALLIC compound, such as TPI, and organosilane compounds, such as GLIMA, can be modified in accordance with the required parameters of the priority operational characteristics. In the General case due to the increase in this ratio will improve the hardness of the obtained film and corrosion performance characteristics in regard to testing for exposure to salt fog, and filiform corrosion.

ORGANOMETALLIC compound (a) selected from compounds of the metal which is selected from zirconium, titanium and aluminum. Still the compounds are described, for example, in the documents mentioned earlier in this document and in the document US-B1-6361868, the description of which can be used for reference.

In General, the compound (a) described by the following formula (I) or formula (II):

,

,

in which M represents Zr or Ti, R represents a detachable removed - for example, hydrolyzable radical, R' represents a detachable part, undeletable - for example, neytralizuya radical, and x is in the range from 1 to 4 in the case of the formula (I) or in the range from 1 to 3 in the case of formula (II), and in the presence of the connection, vpisivaushiesya formula (I) or formula (II), two or more radicals R and/or R' they respectively may be the same or different.

Detachable removed - for example, hydrolyzable radicals is a radical, which undergoes separation or removal from the metal atom M (Zr, Ti or Al) when introducing the compound into contact with a solvent, such as water (hydrolysis), and which does not remain attached to the metal atom.

Detachable part, undeletable - for example, digitalisieren - radical is the radical, which is not separated or not removed from the metal atom M and introducing the compound into contact with the solvent (d), such as water (hydrolysis), and which remains in the United States to the metal atom M

Remove, discharge, hydrolyzable radical or radicals R in the General case are selected from halogen, such as F, Cl, Br and I, in particular Cl and Br; alkoxygroup, preferably C1-C10more preferably C1-C5especially With2-C4linear or branched alkoxygroup, such as, for example, methoxy, ethoxy-, n-propoxy, isopropoxy, h-butoxy, isobutoxy-, second -, butoxy-, tert-butoxy-, n-pentyloxy and n-hexyloxy; cycloalkylation, preferably3-C10cycloalkylation, such as, for example, cyclopropylamino and cyclohexyloxy; aryloxy, preferably6-C10aryloxy, such as, for example, fenoxaprop; acyloxy, preferably C1-C4acyloxy, such as, for example, acetoxy and propionyloxy; alkylcarboxylic groups such as acetyl group; and (C1-C6)alkoxy(C2-C3)alkyl groups (specifically, groups derived from C1-C6alkylamidoamines or propylene glycol). Preferred hydrolyzable radicals are alkoxygroup, in particular a methoxy group, and more particularly ethoxypropan.

In addition, the group or groups R may not necessarily have one or more substituents, in General, wybir the most from Halogens and alkoxygroup.

A non-removable, detachable part - for example, neytralizuya - radical or radicals R' in the General case, are selected from hydrogen; hydroxyl group; alkyl groups, preferably With1-C10more preferably C1-C4linear or branched alkyl groups such as, for example, methyl, ethyl, through n-bucilina, isobutylene, second-bucilina and tert-bucilina group; alkenyl groups, preferably2-C4alkenyl groups, such as, for example, vinyl, 1-protanilla, 2-protanilla and bucinellina group; etkinlik groups, preferably2-C4etkinlik groups, such as, for example, acetylenyl and propargyl group; aryl groups, preferably With6-C10aryl groups such as phenyl and naftalina group; methacryloyl and methacryloxypropyl groups. In addition, the group or groups R' optionally may have one or more substituents, generally selected from halogen and alkoxygroup.

Preferred ORGANOMETALLIC compounds are compounds vpisivaushiesya formulas MR4(M=Zr or Ti) or AlR3where R has already been defined previously.

Among these compounds, more preferred compounds are compounds that have 3 or 4 radicals R are identical predstavljaet a same group, such as alkoxy, aryloxy or cycloalkylation.

The most preferred compounds are Tetra(alkoxide(s)) titanium or zirconium and three(alkoxide(s)) of aluminum, more particularly Tetra(alkoxide(s)) zirconium. Even more preferred compounds are Tetra-n-propoxycarbonyl ("TPI") and tetraisopropoxide.

The Sol may contain only one ORGANOMETALLIC compound such as an alkoxide of aluminum, titanium or zirconium, for example Tetra-n-propoxycarbonyl (TPOC).

Alternatively, the Sol may contain two or more ORGANOMETALLIC compounds selected, for example, of the above alkoxides of metals and other compounds.

Examples of ORGANOMETALLIC compounds of the component (a) are the following:

Al(och3)3, Al(OS2H3)3, Al(O-n-s3H7)3,

Al(O-ISO-From3H7)3, Al(OS4H9)3, Al(O-ISO-From4H9)3,

Al(O-sec-C4H9)3, AlCl3, AlCl(OH)2, Al(OC2H4OC4H9)3,

TiCl4, Ti(OC2H5)4, Ti(OS3H7)4,

Ti(O-ISO-From3H7)4, Ti(OC4H9)4, Ti(2-ethylhexoxy)4,

ZrCl4, Zr(OC2H5)4, Zr(OS3H7)4 , Zr(O-ISO-From3H7)4, Zr(OC4H9)4,

ZrOCl2, Zr(2-ethylhexoxy)4.

Preferably the Sol, corresponding to the invention contains one ORGANOMETALLIC compound selected from alkoxides of zirconium, such as TPI.

ORGANOMETALLIC compounds that can be used in the ashes, corresponding to the invention are described, in particular, in the above-mentioned documents, and in particular in the documents US-A-6008285, US-B1-6228921, US-B1-6482525, US-B1-6361868, the description of which can be used for reference.

Organosilanols connection is the connection, which, as in numerous documents of the prior art, such as document USA-5814137, can be called celanova the sizing.

Organosilanols the compound b) is preferably a compound containing at least one non-removable, detachable part, preferably neytralizuya, radical attached to the silicon, preferably a radical capable of imparting specific properties, and at least one detachable, removable, hydrolyzable moiety attached to silicon. The terms "removable and non-removable" have already been defined previously.

Organosilane compound preferably contains 2 or 3, in particular 3 to be removed, separated - for example, hydrolyzable radical and tinily two, in particular, one detachable part, undeletable - for example, neytralizuya - radical(s).

Mentioned detachable removed - for example, hydrolyzable radical or radicals in the General case are selected from halogen, such as F, Cl, Br and I, in particular Cl and Br; alkoxygroup, preferably C1-C10preferably C1-C5especially With2-C4linear or branched alkoxygroup, such as methoxy, ethoxy-, n-propoxy, isopropoxy, h-butoxy, isobutoxy-, second -, butoxy-, tert-butoxy-, n-pentyloxy and n-hexyloxy; cycloalkylation, preferably3-C10cycloalkylation, such as, for example, cyclopropylamino and cyclohexyloxy;

aryloxy, preferably6-C10aryloxy, such as fenoxaprop;

acyloxy, preferably1-C4acyloxy, such as, for example, acetoxy and propionyloxy, and alkylcarboxylic radicals, such as acetyl radical. The preferred detachable removed - for example, hydrolyzable radicals are alkoxyalkyl and, in particular ethoxypropan.

Mentioned detachable part, undeletable - for example, neytralizuya - radical or radicals in the General case, are selected from hydrogen; hydroxyl groups; mercaptopropyl; ceanography; alkyl groups,preferably C 1-C10more preferably C1-C4, linear or branched alkyl groups such as methyl, ethyl, through n-bucilina, isobutylene, second-bucilina and tert-bucilina group; alkenyl groups, preferably2-C4alkenyl groups such as vinyl, 1-protanilla, 2-protanilla and bucinellina group; etkinlik groups, preferably2-C4etkinlik groups such as acetylenyl and propargyl group; aryl groups, preferably With6-C10aryl groups such as phenyl and naftalina group; alcylaryl groups; arylalkyl groups; (meth)acrylic and (meth)Acrylonitrile groups; Picadilly and glycidyloxy; and groups such as alkyl, Alchemilla, Alchemilla, alcylaryl and arylalkyl groups that have at least one group chosen from primary, secondary or tertiary amino group, in this case neytralizuya radical is, for example, aminoaniline or aminoalkyl group - amide, alkylcarboxylic, substituted or unsubstituted aniline, aldehyde, ketone, carboxyl, anhydrite, hydroxyl, alkoxy, alkoxycarbonyl, mercapto, cyano, hydroxiproline, alkylcarboxylic groups, sulfonic acid groups, phosphoric acid, (meth)and is relaxometry, groups containing epoxy ring such as Picadilly, glycidyloxy-, allyl and vinyl groups.

In addition, the aforementioned detachable, removable, hydrolyzable radicals and said detachable part, undeletable, neytralizuya radicals optionally may be substituted by one or more substituents, in the General case choose from alkoxygroup and halogen atoms.

Particularly preferred organosilane compounds described by the formula below:

,

where the radicals R1identical to each other or different from each other, preferably identical, and are detachable to be removed - for example, hydrolyzable group as defined previously, preferably C1-C4alkoxygroup, more preferably, ethoxy - or methoxy group; R1' is a detachable part, undeletable - for example, neytralizuya - radical, as defined previously, preferably glycidyloxy or glycidyloxy(C1-C20)-, preferably -(C1-C6)-, -alkylenes group, for example, γ-glycidyloxy radical, β-glycidyloxy radical, τ-glycidyloxy radical, ε-glycidyloxy radical, ω-glycidylmethacrylate radical and 2-(3,4-epoxycyclohexyl)ethyl radical; or a group having the General, at least one primary, secondary or tertiary amino group, preferably selected from 3-aminopropyl, N-(2-amino-ethyl)-3-aminopropyl and N-[N'-(2'-amino-ethyl)-2-amino-ethyl]-3-aminopropyl groups.

In the best case organosilane compound selected from the following compounds:

- allyltriethoxysilane,

- N-(2-amino-ethyl)-3-aminopropyltrimethoxysilane,

- N-[N'-(2'-amino-ethyl)-2-amino-ethyl]-3-aminopropyltrimethoxysilane,

- 3-aminopropyltrimethoxysilane,

- 3-glycidylmethacrylate (PIMO),

- 3-mercaptopropionylglycine,

- 3-methacryloxypropyltrimethoxysilane,

- 3-methacryloxypropyltrimethoxysilane,

- N-phenylaminopyrimidine,

- VINYLTRIMETHOXYSILANE.

Among the above compounds, the preferred connection is GLIMA.

In accordance with one particularly preferred and advantageous variant of the invention organosilane compound selected from compounds for which the hydrolysis reaction does not lead to the formation of methanol. The reason for this lies in the fact that methanol is very toxic product formation to be avoided.

Most of the documents of the prior art and, in particular, patents United States, above, is absolutely not prinimayutsa attention to this criterion, which is very important for the safety of personnel conducting the deposition Zola, and lists of silane, which include many compounds that can lead to the formation of methanol. An advantageous use of such silanes becomes even more clear in the case of nuclei, corresponding to the invention, the concentration of silane in which far exceeds the corresponding concentration of the prior art.

Organosilane of this type, which do not lead to the formation of methanol during the hydrolysis, in the General case are compounds that do not have groups, such as metoxygroup, and may be selected from the following compounds:

- 3-aminopropyltriethoxysilane,

- p-aminopenicillin,

- 3-aminopropyltriethoxysilane,

- 3-goldilocksisableachblond,

- 3-glycidylmethacrylate,

- (3-glycidyloxy)metildigoxin,

- 3-mercaptopropionate,

- 3-methacryloxypropyltrimethoxysilane,

- vinylpyridinium,

- vinyltriethoxysilane,

- N-[(3-(triethoxysilyl)propyl]-4,5-dihydroxyindole.

Thus, more specifically, GLIMA can be replaced by GLIA or 3-glycidylmethacrylate that does not contain metacritical. In laboratory tests demonstrated that the replacement GLIMA on GLIA in the ashes, in other respects, containing the same components, leads to the production of the film, which finds the same operational characteristics as regards the quality of the film, and corrosion performance.

Silane compounds that can be used in the method of the invention, in particular, are described in the aforementioned documents in the document EP-A-0195493, the description of which can be used for reference.

Component (C), which can be called the catalyst can be selected from acids, bases, glycols and other compounds, such as ethoxyethanol.

If component C) is an acid, then it preferably can be selected from organic acids, inorganic acids and mixtures thereof.

Organic acids, in particular, can be selected from carboxylic acids, such as aliphatic monocarboxylic acid, for example acetic acid, polycarboxylic acids such as dicarboxylic acids and tricarboxylic acids such as citric acid, and mixtures thereof.

Among the inorganic acids can be used nitric acid or hydrochloric acid, and mixtures thereof.

If the connection is the basis, then it can be selected from amines, such as ethanolamine, triethylamine, and mixtures thereof. The basis, in particular, use when using acids will be prohibited due to the nature of the used substrate or silane.

In the above-mentioned documents describes and other compounds that can be used as component (C).

The solvent (d) is demineralized or distilled water. In the solvent (d) may be optionally includes one or more non-toxic or harmless solvents, such as alcohols, preferably aliphatic alcohols which contain from 1 to 10, particularly from 1 to 4, carbon atoms, such as ethanol, n-propanol, isopropanol and n-butanol.

The preferred solvent is distilled or demineralized water.

Components a), b), C) and d) are significant connections Zola, corresponding to the invention, and form the composition of the base to which depending on the requirements and desirable properties, you can add one or more additional optional components, which are described next.

In addition, the Sol may contain at least one surfactant that improves the characteristics of wetting and spreading on different substrates, but also the quality of the mesh and its own anti-corrosion properties of the Sol-gel film.

Data surfactants include ionic surfactants, which include sarcosinate, such as lauroylsarcosine sodium, FD is IU, for example, an aqueous solution with a concentration of 30%, and non-ionic surfactants, such as ethoxylated fatty alcohols.

In General surfactants are present to share in the range from 0.05% up to 2% or 3 wt.% when calculating the mass of Zola.

Improved wetting by adding suitable for use surfactants makes it possible to obtain homogeneous films, without the occurrence of phenomena of buckling or phenomena of shrinkage during drying on properly prepared surfaces. In addition, possible corrosion properties of surfactants can improve the quality of protection.

In addition, the Sol may contain at least one organic binder, which in General are resin or polymer selected from, for example, epoxy resins, polyurethane binders, vinyl binders, binder based on a complex of the polyester diol binders, acrylic binders and binders, which react or produce crosslinking under the action of UV radiation, or photopolymerizable binder and glycerietum resins. In particular, a binder selected from binders that are compatible with strong acid mixtures, which can be used in the colloidal solution, corresponding to the invention.

Example and resins, which are particularly well suited for use are the product sold under the name URADIL AZ554 in the company DZM Resins, which has the form of an oil emulsion of an alkyd resin, and the product sold under the name Incorez 170 at Industrial Copolymer Limited, which is an epoxy resin based on bisphenol A.

Organic binder and, in particular, the above-mentioned preferred binder based on alkyd resins or preferred epoxy binder in General used in amounts in the range from 0% to 30% when calculated on the total weight of Zola.

Organic binder makes it possible to improve the properties of the film at the bend in order to optimize its characteristics of resistance under the action of voltage, such as its flexibility, resistance to shock loads, the low-temperature limit of the tensile strength and the like.

The organic binder may also make possible the improvement of the corrosion resistance properties of the film obtained from Zola, because it allows you to get even thicker films that are more like those of the film of paint.

In addition, the Sol may contain a filler selected from the grades of mica or talc, which due to its lamellar structures can make sure that certain optimization is waist Sol-gel film, such as anti-corrosion properties and characteristics of resistance to scratching.

Talc and/or mica can be entered in the range from 1% to 20 wt.%, preferably from 3% to 10 wt.%.

In addition, the Sol may contain a filler selected from kaolin, which apparently reacts with alkoxides or directly involved in the formation of the grid and, thus, makes it possible to obtain thicker films while reducing the cost of the product.

In the General case, the filler of this type, if available ranges from 3% to 15%, preferably from 5% to 10 wt.% when calculating the mass of Zola.

In addition, Sol, corresponding to the invention may contain at least one additional compound selected from ORGANOMETALLIC compounds and organosilane compounds, different from the previously described ORGANOMETALLIC compounds and organosilane compounds a) and b). In General, these compounds when present are present to share in the range from 1% to 10 wt.% for additional ORGANOMETALLIC compounds and fractions in the range from 2% to 5 wt.% for additional organosilane connections.

Additional ORGANOMETALLIC compound other than the compounds (a)may include all of the ORGANOMETALLIC compound containing a metal other than zirconium, aluminum is occurring and titanium, such as cerium, yttrium, lanthanum, lead, tin, antimony, boron, vanadium, indium, niobium, bismuth and hafnium.

We can mention, for example, all the alkoxides/alcoholate of a metal other than zirconium, aluminum and titanium, and compounds such as the trihydrate or other hydrates of yttrium acetate; yttrium nitrate; hydrate of cerium acetate; hydrate of sodium acetylacetonate; cerium stearate; uranyl nitrate lanthanum; hydrate acetate lanthanum and lanthanum acetylacetonate.

Among the additional organosilane compounds other than organosilane compounds (b)include the compounds vpisivaushiesya formula (IV)

,

where R1is a delete, detachable, hydrolyzable radical, already defined earlier; preferably R1is alkoxygroup containing from 1 to 4 carbon atoms, such as methoxy, ethoxy, n-propoxy, isopropoxy, sec-butoxy or tert-butoxy.

Additional organosilane connection other than organosilane compounds (b), you can also choose from Versilov. Such porcelany are described, for example, in document DE-A-4118184 in the document US-Bl-6361868, descriptions of which can be used for reference. Examples of data Versilov represent the following:

C2F5CH2-CH2-SiY3,

n-C6F13 CH2CH2-SiY3,

n-C8F17CH2CH2-SiY3,

n-C10F21CH2CH2-SiY3,

(Y=co3OC2H5or Cl),

ISO-C3F7O-(CH2)3-SiCl2(CH3),

n-C6F13CH2CH2SiCl2(CH3),

n-C6F13CH2CH2SiCl(CH3)2.

Other porcelany are described in the document US-B1-6482525 in the document EP-A-587067, descriptions of which can also be used for reference.

In addition, Sol, corresponding to the invention may contain one or more metal salts, such as one or more salts of rare earth metals. Salts of rare earth metals can be selected from esters of rare-earth metals, such as acetates and oxalates of cerium chlorides of lanthanum and cerium. The vanadates, alkaline and alkaline earth metals, such as metavanadate sodium and metavanadate calcium. Other metal salts are the borates of alkali and alkaline earth metals, such as metaborate barium. Sol, corresponding to the invention can contain any combination of metal salts. Links in connection with these salts can be made to document US-A-5806562.

In the General case, metal salts when present are present in amounts ranging from 0.5% to 5 wt.% p is to calculate the mass of Zola.

In addition, Sol, corresponding to the invention may contain one or more conductive materials selected from, for example, salts, electrolytes, redox pairs, conductive polymers, related to polianilinovyh type ferrocene, sulfonated polystyrene, grades of carbon black and all other compatible products that detect characteristics of the conductivity against the electric charges.

In addition, Sol, corresponding to the invention may contain a matrix coloring substance selected from dyes, pigments and mother-of-pearl.

The pigments can be chosen from decorative pigments and pigments used to improve the conductive and/or reflective abilities of the film.

One particularly preferred Sol, corresponding to the invention, contains, wt%:

a) from 3% to 30%, preferably from 5% to 20%, more preferably from 7% to 15%, in particular from 8% to 14%, more particularly from 10% to 13%, for example 10,8% or 12%, Tetra-n-propoxycarbonyl (TPOC), aluminum or titanium;

b) from 5% to 50%, preferably from 5% to 40%, more preferably from 10% to 40%, particularly from 15% or 20% to 30%, for example, 22% or 23%, 3-glycidylmethacrylate (GLIMA);

c) from 1% to 15%, preferably from 2% to 10%, more preferably from 3% to 8%, for example 5%, at measures which, one compound selected from acids, bases, glycols and ethoxyethanol;

d) the remainder to 100% in demineralized or distilled water,

thus the total mass number (a) and (b) is an amount greater than 30%, preferably greater than 31,2%; 31,5%; 32% or 33%, more preferably greater than 35%, in particular greater than 40%, more particularly greater than 50%.

In the best case GLIMA can be replaced by GLIA.

The Sol can be obtained for a certain period of time prior to deposition on the substrate, resulting in the mixing of the previously defined four main components a), b), C) and d); however, in one preferred implementation, corresponding to the invention, the Sol can be obtained from a set consisting of two parts (a and b).

The first part And, in the form of liquid, contains the previously described components (a), (C) and (d) Zola, and the second part, in the form of liquid, contains previously defined component b) Zola. The first part (A) usually contains, for example, a zirconium alkoxide (for example, TPI), hydrolyzed in solution in distilled water containing acetic acid, and optionally one or more additives, and part b contains silane (such as GCMS) or a mixture of pure silane.

Sol applied, deposited on a substrate, just get in the var is shivani two liquid products, formed by the parts a and b, instead of four or more products, some of which are solid, in the prior art. Two liquid components (part a and b) is very easy to mix when using conventional mixing devices or even manually in case of small quantities. Two parts a and b are stable when stored in a properly adjusted the packaging or container for periods of time ranging, for example, from 1 month to 2 years in the case of a simple homogenization before use.

In General, part a is from 50% to 90 wt.% when calculating the mass obtained Zola and, respectively, in the General case, the part is from 10% to 50 wt.% when calculating the mass obtained Zola.

After mixing of all components, or two parts a and b obtained by the Sol can be applied for a period of time ranging from 0 minutes to 24 months, preferably from 0 minutes up to 12 months, more preferably from 0 minutes up to 6 months, in particular from 30 minutes to 8 hours.

The time which elapses after receipt of Zola in the mixing of four components or two parts a and b, makes it possible aging Zola. This time depends on the speed of hydrolysis of ORGANOMETALLIC compounds such as alkoxides of zirconium, and organosilane.

In General the optimum aging time is the fact during which the connection of the zirconium and the silane will undergo hydrolysis to a degree sufficient to complete the reaction between silicon and zirconium, and a surface, e.g. a metal surface of the substrate.

It should be noted that the connection of zirconium is already present in the hydrolyzed form in part a, which contains distilled water.

The deposition of ash on the surface, which is preferably pre cast cleaning and/or activation can be carried out in accordance with any method known to the expert in the relevant field of technology, such as sputtering, spraying or dipping, where one preferred technique is the technique of spray.

In General the operation of the deposition - deposition - Sol on the surface is carried out at a temperature in the range from 0 to 80°C, preferably from 20 to 60°C., for example 50°C.

After deposition receiving substrate, the surface of which is coated in a layer of Zola.

After this layer Zola dried according to the method known in the art. In General, drying is carried out at a temperature in the range from 0°C to 500°C, preferably from 50 to 150°C., more preferably from 80°to 130°C., for a period of lying is no duration, for example, from 1 second to 2 hours, preferably from 5 minutes to 1 hour, more preferably from 20 to 30 minutes, depending on the mode of drying, which is used.

Drying can be performed by heating the substrate in the open air or in a drying Cabinet or by using devices for very fast heating, which are commercially available and known to experts in the relevant field of technology. In addition, the drying can be combined with crosslinking under the action of UV radiation.

You can also implement and drying cycle, similar to what is described in the document US-A-5814137 in column 11, lines 15 to 23.

Alternatively, you can apply with melting ceramics at temperatures likely to reach up to 2500°C, for example be in the range of from 800 to 1500°C.

In the best case, the layer of Sol can be dried using portable thermal devices such as heat device for removing coatings with pulsed air supply (burner for burning coatings), devices for heating under the action of infrared radiation and the like, in particular, in the context of repair of existing equipment or equipment that is difficult to put a hot drying in closed chambers.

By the way, sootvetstvuyuschemu the invention, it is possible to carry out the deposition of only one Sol-gel layer; in the General case the Sol-gel layer has a thickness in the dry state in the range from 0.5 to 20 μm. According to the observations due to the high concentration of the components Zola, corresponding to the invention, and when using one Sol-gel layer corresponding to the invention, can be obtained excellent results, expressed in corrosion resistance. In the General case the layer has a thickness greater than the thickness of the Sol-gel layers of the prior art obtained from dilute sols, namely the thickness in the dry state in the range from 0.1 to 0.4 μm, preferably from 0.2 to 0.3 microns.

In order to obtain a multilayer coating can surround the two or more Sol-gel layers, with each layer characterized by a composition different from compositions of the preceding layer and the subsequent layer, and each deposited layer detects properties different from the properties of the other layers and select properties below. In a broad sense you can spend deposition from 1 to 5 layers, preferably from 2 to 3 layers.

In accordance with various additives included in the Sol deposited Sol-gel layer may have a wide range of properties.

Specialist in the relevant field of technology will easily be able to determine to which such Supplement or supplements out there, where it is appropriate, you will need to enter in the Sol, corresponding to the invention, which necessarily contains the above components (a), b), C) and d), in order to obtain the Sol-gel layers, which have the following properties. Thus, it will be possible to obtain a Sol-gel layers, demonstrating the presence of resistance to scratching, resistance to abrasion; antifriction properties; resistance to fogging; antistatic properties, anti-reflection skills; characteristics of electroluminescence; variable optical properties; conductivity (at high and low degrees K); superconductivity; ferroelectric properties (piezoelectric and pyroelectric properties); characteristics of impermeability (with respect to gases; to bases, acids, various chemical products, including compositions for coatings removal, hydraulic fluids for hydraulic systems, such as Skydrob"); characteristics of gazettelive; thermochromic properties; characteristics of luminescence; nonlinear optical properties; flame retardant properties; characteristics of Sol-gel coatings for composites; resistance to coalescence (resistance bonding); insulation properties, resistance to fouling; characteristics of primers; characteristics of the paint; hydrophobicity; hydrophilicity; porosity; biocide the properties; deodorizing ability, wear resistance and the like.

In accordance with the invention it is also possible to obtain a multilayer coating, which shows the presence of any combination of the properties selected from among the above.

Now the invention will be described with reference to the examples which follow and which are given by way of illustration and not limitation.

EXAMPLES

EXAMPLE 1

In this example, the Sol, corresponding to the invention, obtained from the first part or component and the second part or component In the Sol is applied to the samples of aluminum and evaluate properties obtained by the Sol-gel layer.

1.1. The mixture And

In spotlessly clean chemical glass 1 litre weighed exactly 108 g of TPI at a concentration of 70% in 1-propanol;

- with careful stirring, add exactly 50 g of 96%acetic acid;

after homogenization with stirring, add exactly 622 g of distilled water;

the stirring is continued up to obtain a transparent homogeneous liquid (approximately 1 hour);

to expedite the passage of hydrolysis can be heated up to approximately 60°C;

the mixture is filtered through filter paper and then store in a perfectly airtight flask.

1.2. aluchemie Zola

In spotlessly clean chemical glass 2-liter pour exactly 680 g of a mixture of component or part a), and then with stirring, poured into precision 220 g GLIMA (glycidylmethacrylate at a concentration of 98%) (component b or part C);

the stirring is continued up to obtain a transparent homogeneous phase (approximately 1 hour);

- to increase the reaction rate of hydrolysis can be heated up to approximately 60°C;

the mixture is filtered through laboratory filter paper and then store in a tightly stoppered flask.

Note: the mass content of the solid phase in such a mixture is of the order of magnitude of 20%.

1.3. Application Zola

In accordance with the methodology described below, receive samples of aluminium 2024 T3:

- degreasing using diluted in water alkaline detergent at 60°C for period of time with a duration of 10 minutes with stirring;

- rinse using tap water and distilled water;

- deoxidation using sulfuric-nitric acid mixture, for example, for 10 minutes at a temperature in the range from 20 to 50°C;

- rinse using tap water and distilled water;

- drying of the sample using pulsed supply g the hot air.

Samples are placed on a carrier in the spray chamber.

- During the period of time lasting several hours in advance of the obtained solution (1.2.) applied using pneumatic sprayer, such as a pneumatic atomizer Grace Delta-spray, while the air pressure is set to approximately 5-6 bars.

Effectively carry out the coating surface, exactly in the same way as in the case of applying primer or paint, and then for a period of time lasting from several minutes to 1 hour, the samples are placed in a drying Cabinet, which exhibit, for example, at 110°C.

- After a period of time lasting from several minutes to 1 hour samples take out and leave to cool.

1.4. The examination of samples of the

After cooling, the obtained Sol-gel layer detects the following characteristics:

- adhesion to aluminum media;

- very good adhesion of the applied paints and coatings by Sol-gel layer;

very good protection for your media corrosion (corrosion when exposed to salt fog and filiform corrosion);

the thickness of deposition in the range from 1 to 10 microns (as measured using the apparatus Elcometer 355)) in accordance with the selected application.

The test, known the od name tests on the effect of salt fog, the samples are placed in the chamber for environmental testing device for cyclic corrosion test Q-FOG from the Q-Panel. Samples subjected to processing by Sol corresponding to the invention, no corrosion not find after 168 hours.

EXAMPLE 2

In this example, the Sol corresponding to the prior art, is obtained from components a, b, C and D. the above-Mentioned Sol is applied to the samples of aluminum and evaluate properties obtained by the Sol-gel layer.

2.1. Getting Zola

Component And formed from a few grams of acetic acid, mixed with component b composed of a few grams of zirconium alkoxide at a concentration of 70% in n-propanol;

- a component formed from a few grams of silane GLIMA, mixed with component D, formed from approximately 950 g of distilled water;

connection (a+b) is mixed with a compound (C+D);

the mixture is left to act for approximately 30 minutes. Note: the level of solids in the mixture is less than 5 wt.%.

2.2. Application Zola

Samples of aluminium receive the same method as in example 1, and the Sol is applied by spraying using the same equipment and the same conditions as described previously in the example is 1.

2.3. The examination of samples of the

- Adhesion to aluminum media;

- very good adhesion of the applied paints and coatings by Sol-gel layer;

- a very large flows, the difficulty homogeneous wetting the entire surface as a whole (which can be observed, in particular during drying);

the thickness measured after drying: maximum of 200 to 400 nanometers;

- test the impact of salt fog held the same way as in example 1, demonstrates that the protection afforded by the presence of the Sol-gel layer, obtained using Zola prior art corresponds to less than 24 hours. Corrosion pitting on the metal see even after a few hours.

1. Sol for applying the Sol-gel coating on the surface containing the following components in wt.%:
a) from 3 to 30%, preferably from 5 to 20%, more preferably from 7 to 15%, in particular from 8 to 14%, more particularly from 10 to 13%, most preferably about 10.8 or 12%, of at least one ORGANOMETALLIC compound of zirconium, aluminum or titanium;
b) from 5 to 50%, preferably from 5 to 40%, more preferably from 10 to 40%, in particular from 15 or 20 to 30%, most preferably 22%or 23%, of at least one organosilane connection;
(C) from 1 to 15%, preferably from 2 to 10%, more FAV is preferably from 3 to 8%, most preferably, 5%, of at least one compound selected from organic and inorganic acids, bases, glycols and ethoxyethanol;
d) the remainder to 100% in demineralised or distilled water; the total number of a) and b) has a value of greater than 30%, preferably greater than 31,2; 31,5; 32; 33%, more preferably greater than 35%, in particular greater than 40%, more particularly greater than 50%.

2. The Sol according to claim 1, which further comprises less than 5%, preferably less than 3%, more preferably less than 1 wt.%, non-toxic or harmless organic solvents, preferably selected from alcohols, such as non-toxic or harmless With 1-10 aliphatic alcohols.

3. The Sol according to claim 1, in which the level of bulk solids, more than 4%, preferably in the range from 4 to 37%, more preferably from 18 to 37%, most preferably from 20 to 30%.

4. Sol according to any one of claims 1 to 3, in which the ratio organosilane compounds and ORGANOMETALLIC compound is in the range from 1.5 or 1.6 to 6, preferably from 1.8 to 2.5.

5. The Sol according to claim 1, in which the ORGANOMETALLIC compound has the formula (I) or formula (II):
,
in the cat the matrix M represents Zr or Ti, R is a detachable, removable, preferably hydrolyzable radical, R' represents a detachable part, undeletable, preferably, neytralizuya radical, and x is in the range from 1 to 4, when the compound has formula (I), or in the range from 1 to 3, when the compound has formula (II), and subject to the presence in the compound of formula (I) or formula (II) two or more radicals R and/or R' they are, respectively, can be identical or different.

6. The Sol according to claim 5, in which the deleted, detachable, preferably hydrolyzable radicals R are selected from the group consisting of halogen, such as F, Cl, Br and I, in particular Cl and Br; alkoxy groups, preferably With1-C10more preferably C1-C5especially With2-C4linear or branched alkoxygroup, such as methoxy, ethoxy-, n-propoxy, isopropoxy, h-butoxy, isobutoxy-, second -, butoxy-, tert-butoxy-, n-pentyloxy and n-hexyloxy; cycloalkylation, preferably3-C10cycloalkane groups, such as cyclopropylamine-group and cyclohexyloxy; aryloxy, preferably6-C10aryloxy, such as phenoxy group; acyloxy groups, preferably C1-C4acyloxy groups, such as, for example, acetoxy and propionyloxy; alkylcarboxylic the x groups, for example, acetyl groups; and (C1-C6)alkoxy(C2-C3)alkyl groups (specifically, groups derived from C1-C6alkylamidoamines or propylene glycol); in addition, the group or groups R may not necessarily have one or more substituents selected from halogen and alkoxygroup.

7. Sol according to any one of subparagraph 5 or 6, in which a non-removable, detachable part, practicelink, neytralizuya radical or radicals R' are selected from the group consisting of hydrogen; hydroxyl group; alkyl groups, preferably C1-C10more preferably C1-C4linear or branched alkyl groups such as methyl, ethyl, through n-bucilina, isobutylene, second-bucilina and tert-bucilina group; alkenyl groups, preferably C2-C4alkenyl groups such as vinyl, 1-protanilla, 2-protanilla and bucinellina group; etkinlik groups, preferably C2-C4etkinlik groups such as acetylenyl and propargyl group; aryl groups, preferably With6-C10aryl groups such as phenyl and naftalina group; methacrylic and methacryloxypropyl groups;
moreover, the group or groups R' optionally may have one or more substituents, in the General case, the choice is emich from Halogens and alkoxygroup.

8. The Sol according to claim 5, in which the ORGANOMETALLIC compound has the formula MR4or AlR3where M represents Zr or Ti, and R are separated, removed, gidrolizuemye radical.

9. The Sol of claim 8, in which all 4 or 3 radicals R are identical and represent the same group, such as alkoxy, aryloxy or cycloalkylation.

10. The Sol according to claim 9, in which the ORGANOMETALLIC compound is Tetra-n-propoxycarbonyl ("TPOC") or tetraisopropoxide.

11. The Sol according to claim 1, in which organoselenium compound is a compound containing at least one non-removable, detachable part, preferably neytralizuya radical and at least one removed, separated, preferably hydrolyzable moiety attached to silicon.

12. The Sol according to claim 11, in which organosilane compound contains 2 or 3, preferably 3 to be deleted, detachable, preferably hydrolyzable radical and one or two in particular, one detachable part, undeletable, for example neytralizuya radical(s).

13. Sol indicated in paragraph 12, in which the detachable removed, preferably hydrolyzable radical or radicals selected from the group consisting of halogen, such as F, Cl, Br and I, preferably Cl and Br; alkoxygroup, preferably C1-C10preferably C1-C5b is more preferably 2-C4linear or branched alkoxygroup, such as methoxy, ethoxy-, n-propoxy, isopropoxy, h-butoxy, isobutoxy-, second -, butoxy-, tert-butoxy-, n-pentyloxy and n-hexyloxy; cycloalkylation, preferably3-C10cycloalkylation, such as cyclopropylamine and cyclohexyloxy; aryloxy, preferably6-C10aryloxy, such as fenoxaprop; acyloxy, preferably C1-C4acyloxy, such as acetoxy and propionyloxy; and alkylcarboxylic radicals, such as acetyl radical.

14. Sol according to any one of § § 11 or 12, in which the detachable part, undeletable, preferably neytralizuya radical or radicals selected from the group consisting of hydrogen; a hydroxyl group; mercaptopropyl; ceanography;
alkyl groups, preferably C1-C10more preferably C1-C4linear or branched alkyl groups such as methyl, ethyl, through n-bucilina, isobutylene, second-bucilina and tert-bucilina group; alkenyl groups, preferably C2-C4alkenyl groups such as vinyl, 1-protanilla, 2-protanilla and bucinellina group; etkinlik groups, preferably2-C4etkinlik groups, such as acetylenyl the traveler and propargyl group; aryl groups, preferably With6-C10aryl groups such as phenyl and naftalina group; alcylaryl groups; arylalkyl groups; (meth)acrylic and (meth)Acrylonitrile groups; Picadilly, glycidyloxy groups; and groups such as alkyl, Alchemilla, Alchemilla, alcylaryl and arylalkyl group having at least one group chosen from primary, secondary or tertiary amino group, and neytralizuya radical represents aminoaniline or aminoalkyl amide group, alkylcarboxylic, substituted or unsubstituted aniline, aldehyde, ketone, carboxyl, anhydrous, hydroxyl, alkoxy, alkoxycarbonyl, mercapto, cyano, hydroxyproline, alkylcarboxylic groups, sulfonic acid groups, phosphoric acid, (meth)acryloyloxy, groups containing an epoxy ring such as Picadilly, glycidyloxy-, allyl and vinyl groups.

15. The Sol according to claim 11, in which detachable and detachable part of the radicals optionally substituted by one or more substituents, in the General case choose from alkoxygroup and halogen atoms.

16. The Sol according to claim 11, in which organosilane compound has the formula (III):
Si(Ri')(Ri)3where the radicals R1identical to each other or different from each other, preferably identically and are detachable, removed, preferably hydrolyzable group 13, preferably C1-C4alkoxygroup, more preferably, ethoxy - or methoxy group; and R1' represents a non-removable, detachable part, preferably neytralizuya radical, as defined previously, preferably glycidyloxy or glycidyloxy(C1-C20)-, preferably C1-C6, -alkylenes group, for example, γ-glycidyloxy radical, β-glycidyloxy radical, τ-glycidyloxy radical, ε-glycidyloxy radical, ω-glycidylmethacrylate radical and 2-(3,4-epoxycyclohexyl)ethyl radical; a group having at least one primary, secondary or tertiary amino group, preferably selected from 3-aminopropyl, N-(2-amino-ethyl)-3-aminopropyl and N-[N'-(2'-amino-ethyl)-2-amino-ethyl]-3-aminopropyl groups.

17. The Sol according to claim 11, in which organosilane compound selected from the group consisting of the following compounds:
- allyltriethoxysilane,
- N-(2-amino-ethyl)-3-aminopropyltrimethoxysilane,
- N-[N'-(2'-amino-ethyl)-2-amino-ethyl]-3-aminopropyltrimethoxysilane,
- 3-aminopropyltrimethoxysilane,
- 3-pipetransportedgelabel,
- 3-mercaptopropionylglycine,
- 3-methacryloxypropyltrimethoxysilane,
3-methacryloxypropyltrimethoxysilane,
- N-Fenelon nopropertiesrecyclebin,
- VINYLTRIMETHOXYSILANE.

18. Sol on 17, in which organoselenium compound is 3-glycidylmethacrylate(PIMO).

19. The Sol according to claim 1, in which organosilane compound selected from compounds for which the hydrolysis reaction does not lead to the formation of methanol.

20. The Sol according to claim 19, in which organosilane compound selected from the group consisting of the following compounds:
- 3-aminopropyltriethoxysilane,
- p-aminopenicillin,
- 3-aminopropyltriethoxysilane,
- 3-goldilocksisableachblond,
- 3-glycidylmethacrylate,
- (3-glycidyloxy)metildigoxin,
- 3-mercaptopropionate,
- 3-methacryloxypropyltrimethoxysilane,
- vinylpyridinium,
- vinyltriethoxysilane.

21. The Sol according to claim 20, in which organoselenium compound is 3-glycidylmethacrylate (GLIA).

22. The Sol according to claim 1, in which component C) is an acid selected from organic acids, such as carboxylic acids, preferably aliphatic monocarboxylic acids such as acetic acid, dicarboxylic acids and tricarboxylic acids such as citric acid, and mixtures thereof; and inorganic mineral acids, such as chloride-hydrogen acid, nitric acid or mixtures thereof.

23. The Sol according to claim 1 in which the compound is (C) is the base, selected from amines, such as ethanolamine, triethylamine, and mixtures thereof.

24. The Sol according to claim 1, which additionally contains at least one surfactant selected from ionic surfactants, such as sarcosinate, and nonionic surfactants such as ethoxylated fatty alcohols.

25. The Sol according to claim 1, which additionally contains at least one organic binder.

26. The Sol according to claim 1, which further comprises a filler selected from the grades of mica and talc.

27. Sol on p, which further comprises a filler in the range from 1 to 20 wt.%, preferably from 3 to 10 wt.%.

28. The Sol according to claim 1, which further comprises a filler selected from kaolin.

29. The Sol according to claim 1, which contains at least one additional compound selected from ORGANOMETALLIC compounds and organosilane compounds, different from ORGANOMETALLIC compounds (a) and organosilane compounds b).

30. Sol in clause 29, in which additional ORGANOMETALLIC compound other than the compound or compounds (a)selected from ORGANOMETALLIC compounds containing a metal other than zirconium, aluminum and titanium, such as cerium, yttrium, lanthanum, lead, tin, antimony, boron, vanadium, indium, niobium, bismuth and hafnium.

31. Sol on the .30, where additional ORGANOMETALLIC compound other than the compound or compounds (a)selected from alkoxides/alcoholate of a metal other than zirconium and compounds, such as the trihydrate or other hydrates of yttrium acetate; yttrium nitrate; hydrate of cerium acetate; hydrate of cerium acetylacetonate; cerium stearate; uranyl nitrate lanthanum; hydrate acetate lanthanum and lanthanum acetylacetonate.

32. Sol according to any one of p-31, in which additional organosilane compound is a compound of formula (IV):
,
where R1is a delete, detachable, hydrolyzable radical under clause 16; preferably R1is alkoxygroup containing from 1 to 4 carbon atoms, such as methoxy, ethoxy, n-propoxy, isopropoxy, sec-butoxy or tert-butoxy.

33. Sol according to any one of p-31, in which additional organosilanols connection is Persian.

34. Sol on p in which Persian selected from the group consisting of the following compounds:
C2F5CH2-CH2-SiY3
n-C6F13CH2CH2-SiY3
H-C8F17CH2CH2-SiY3
H-C10F21CH2CH2-SiY3
(Y=co3OS2H5or Cl)
ISO-C3F7O-(CH2)3-SiCl2(sub> 3)
n-C6F13CH2CH2SiCl2(CH3)
n-C6F13CH2CH2SiCl(CH3)2.

35. The Sol according to claim 1, which contains one or more metal salts, preferably one or more salts of rare earth metals.

36. The Sol according to claim 1, which contains at least one conductive material.

37. The Sol according to claim 1, which contains a dye selected from dyes, pigments and mother-of-pearl.

38. The Sol according to claim 1, which contains the following components, wt%:
a) from 3 to 30%, preferably from 5 to 20%, more preferably from 7 to 15%, in particular from 8 to 14%, more particularly from 10 to 13%, especially preferably, to 10.8 or 12%, Tetra-n-propoxycarbonyl (TPOC), aluminum or titanium;
b) from 5 to 50%, preferably from 5 to 40%, more preferably from 10 to 40%, in particular from 15 or 20% to 30%, particularly preferably 22%or 23%, 3-glycidylmethacrylate (GLIMA);
c) from 1 to 15%, preferably from 2 to 10%, more preferably from 3 to 8%, most preferably 5%, of at least one compound selected from acids, bases, glycols and ethoxyethanol:
d) the remainder to 100% in demineralised or distilled water; thus the total mass number (a) and (b) has a value of greater than 30%, preferably greater than 31,2; 31,; 32; or 33%, more preferably greater than 35%, in particular greater than 40%, most preferably more than 50%.

39. The set includes:
the first container containing the first part And in the form of a liquid containing components (a), (C) and (d) Sol according to any one of claims 1 to 38;
a second container containing the second part, in the form of a liquid containing the component (b) Sol according to any one of claims 1 to 38.

40. Set in § 39, in which part a is from 50% to 90 wt.%, preferably from 60% to 90 wt.%, as part ranges from 10% to 50 wt.%, preferably from 10% to 40 wt.%, from Zola.

41. A method of obtaining a Sol-gel layer on the surface of the substrate, characterized in that:
Sol, as claimed in any one of claims 1 to 38 are precipitated on the surface to obtain on the surface of the substrate layer Zola;
deposited layer Zola dried to obtain on the surface of the substrate by the Sol-gel layer.

42. The method according to paragraph 41, wherein the Sol-gel layer is precipitated to obtain a thickness in the dry state in the range from 500 nm to 20 μm, preferably from 1 or 2 to 10 μm, more preferably from 4 to 5 microns.

43. The method according to any of PP and 42, characterized in that the Sol is heated in advance and/or during deposition.

44. The method according to any of PP-42, characterized in that before the deposition of the Sol is filtered.

45. The method according to any of PP and 42, is great for the decomposing those what Sol precipitated by sputtering, spraying or dipping.

46. The method according to paragraph 41, wherein the substrate is obtained from a material selected from the group consisting of metals; metal alloys; organic or inorganic mineral glass; and organic materials such as plastics; wood; ceramics; textiles; concrete; securities; stone; and composite materials composed of two or more of these materials; these materials may not necessarily be subjected to plating, and/or the surface treatment and/or coating, for example colouring.

47. The method according to item 46, wherein the substrate is obtained from a material selected from the group consisting of aluminum, titanium, copper, iron and their alloys, such as steel, for example stainless steel, and Inconel; and optionally subjected to plating, and/or the surface treatment and/or coating, for example colouring.

48. The method according to any of PP and 47, characterized in that the surface treatment is chosen from simple and chromate conversion layers, anodizing layers or other layers.

49. The method according to any one of p-42, characterized in that before the deposition of Zola surface is subjected to cleaning and/or activating and/or etching as a result of chemical and/or physical and/or mechanical processing.

Cab in paragraph 41, characterized in that mix part a and part b by § 39 or mix components a), b), C) and (d) obtaining Zola.

51. The method according to item 50, wherein after mixing parts a and b or components a), b), C) and (d) the Sol is applied to the surface of the substrate during the period of time from 0 minutes to 24 months, preferably from 0 min to 12 months, more preferably from 0 min to 6 months, in particular from 30 minutes to 8 hours

52. The method according to paragraph 41, wherein the drying layer Zola carried out at a temperature from 0 to 500°C, preferably from 50 to 150°C., more preferably from 80 to 130°C., for a period of time from 1 s to 2 h, preferably from 5 min to 1 h, more preferably from 10 to 30 minutes

53. The method according to paragraph 41, wherein the drying layer Zola spend portable thermal devices such as heat device for removing coatings with pulsed air supply (burner for burning coatings or devices for heating under the action of infrared radiation.

54. The method according to paragraph 41, wherein the deposited Sol-gel layer has a thickness in the dry state in the range from 0.5 to 20 μm, preferably from 1 or 2 to 10 microns.

55. The method according to paragraph 41, wherein the Sol-gel layer is a layer having resistance to scratching; abrasion resistance; low friction properties;resistance to fogging; antistatic properties; anti-reflection capacity; characteristics of electroluminescence; variable optical properties; conductivity (at high and low degrees K); superconductivity; ferroelectric properties (piezoelectric and pyroelectric properties); characteristics of impermeability (with respect to gases; to bases, acids, various chemical products, including compositions for coatings removal, hydraulic fluids for hydraulic systems, such as Skydrol)); characteristics of gazettelive; thermochromic properties; characteristics of luminescence; nonlinear optical properties; flame retardant properties; characteristics of Sol-gel coatings for composites; resistance to the sticking (resistance bonding); insulation properties; resistance to fouling; the characteristics of the primers; the characteristics of the paint; hydrophobic; hydrophilic; porosity; biocidal properties; deodorizing capacity; and the wear resistance and the like.

56. The Sol-gel layer obtained by the method according to any of PP-55.

57. A substrate having at least one surface coated in the form of at least one Sol-gel layer on p.

58. Application of the Sol-gel layer on p to impart corrosion resistance to the surface of the substrate, in particular the surface, is received from the material, selected from metals, metal alloys and composite materials containing metal or metal alloy.

59. The application of § 58, in which the surface is coated in the form of a Sol-gel layer.

60. A method of obtaining a coating containing two or more layers on the surface of the substrate, and at least one layer is a Sol-gel layer obtained by the method according to any of PP-55.

61. The method according to p, characterized in that it contains on the surface of the substrate, two or more layers, in which:
on the surface receive the Sol-gel layer; then
on the Sol-gel layer is applied one or more other layers, other layers is chosen, preferably, from layers of paint, primer, mastic, glue or resin.

62. The method according to p, characterized in that the layer is applied to the Sol-gel layer immediately after its receipt.

63. The method according to item 62, wherein the layer is applied to the Sol-gel layer during the period of time from one month to ten years after receipt of the Sol-gel layer.

64. The method according to any of PP-63, characterized in that the coating includes two or more identical or different Sol-gel layers and optionally one or more other layers.

65. The method according to p, characterized in that the Sol-gel layers are selected from the Sol-gel layer according to § 55.



 

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Fuel injector // 2411392

FIELD: engines and pumps.

SUBSTANCE: fuel injector includes valve body in which there is the main fuel inlet cavity and injection hole; and needle installed in a movable way in valve body and having on its front end the shutoff part, as a result of movement of which the shutoff part either diverts from inner surface of the valve body, or contacts with it, thus opening or shutting off the fuel flow from the main cavity to injection hole. The latter is covered with material with lower oxygen adsorption and low reaction capability for interaction with oxygen in comparison with material of the valve body itself; and shutoff part of the needle is equipped with the coating made from material with higher capability of pushing off the liquid in comparison with material of the needle itself and not forming metal surface. Gold is coating material of injection hole, and material on the basis of silicon dioxide is coating material of shutoff part.

EFFECT: fuel injector prevents formation of deposits and improves reliability owing to simple configuration.

3 dwg

FIELD: chemistry.

SUBSTANCE: invention can be used in inorganic chemistry. To obtain particles of doped metal oxides, an oxidisable and/or hydrolysable metal compound which is a dopant, together with an atomising gas, is atomised into a stream of particles of metal oxides in a carrier gas in a first reaction zone. The mass flow of metal oxide particles and mass flow of the dopant is chosen such that said particles contain from 10 parts/million to 10 wt % of the doping component. The amount of dopant is calculated in terms of the corresponding oxide. Temperature of the first reaction zone is lower than boiling point of the dopant, lower than the temperature of the reaction for converting the dopant to the corresponding oxide and ranges from 200 to 700 °C. Further, the stream from the first reaction zone as well as an optional amount of oxygen and/or steam which is at least sufficient for complete conversion of the dopant, are fed into the second reaction zone. Temperature in the second reaction zone is lower than boiling point of the dopant and ranges from 300 to 2000°C, preferably from 500 to 1000 °C. The reaction mixture is cooled or left to cool. Particles of doped metal oxides are then separated from gaseous substances.

EFFECT: invention enables to obtain metal oxides which are only doped on the surface.

11 cl, 1 dwg, 5 tbl, 5 ex

FIELD: metallurgy.

SUBSTANCE: invention refers to chemical application of metal coating. The procedure consists in bringing substrate into contact with a bath containing a surface active substance, reducer and metal chosen from a group Ag, Cu, Pd and Co. Also temperature of the bath is higher, than temperature of dimness of solution present in the bath in form of at least two phases. The bath contains water solution of silver salt, substituted alkylene-oxide compound, boric acid, reducer and complex former. The procedure includes silicon surface etching, immersion of silicon surface into the above described bath, leaving silicon surface till silver coating forms on it and extracting silicon surface coated with silver from the bath.

EFFECT: increased visual reflex and electrical conductivity.

34 cl, 2 ex

FIELD: metallurgy.

SUBSTANCE: invention refers to chemical application of metal coating. The procedure consists in bringing substrate into contact with a bath containing a surface active substance, reducer and metal chosen from a group Ag, Cu, Pd and Co. Also temperature of the bath is higher, than temperature of dimness of solution present in the bath in form of at least two phases. The bath contains water solution of silver salt, substituted alkylene-oxide compound, boric acid, reducer and complex former. The procedure includes silicon surface etching, immersion of silicon surface into the above described bath, leaving silicon surface till silver coating forms on it and extracting silicon surface coated with silver from the bath.

EFFECT: increased visual reflex and electrical conductivity.

34 cl, 2 ex

FIELD: metallurgy.

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34 cl, 2 ex

FIELD: process engineering.

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EFFECT: perfected production of coppered metal, higher efficiency and coppered products transfer rate, higher quality of cleaning.

5 cl, 4 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to metal-working and can be used in metallurgy, machine building and other industrial branches for processing wire, strips, tubes and other various-section products. Proposed method comprises, prior to applying copper from copper-containing solutions, coppering and processing products after coppering. Note here that at least a part of product processing process, prior to coppering, is performed by at least single vacuum-arc processing of a product-cathode, and at least with the help of electrode-anode. Note here that said vacuum-arc processing is performed in conditions of product cleaning without oxidising its surface in conditions of cleaning with oxidising at least a part of product surface, while blue copperas solution represents copper-containing solution.

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FIELD: process engineering.

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2 cl

FIELD: metallurgy.

SUBSTANCE: invention relates to application of coatings from noble metals, particularly to platinum and iridium on ceramic and can be used for receiving of protective coatings with high chemical stability in liquid and gaseous corrosive medium. Method includes application of coating on preliminary degreased and activated surface of product by means of chemical reduction of metal from water solution, containing ammonia complex of metal and 0.56 g/l potassium hydroxide, at temperature 170 - 210 °C in confined space during 130 - 180 min., herewith used aqueous solution is previously vacuumised during 20 - 30 min. and is saturated by nitrogen for removing of molecular oxygen. In the capacity of metal complex it is used tetramin platinum chloride (II) or pentammin iridium chloride (III), which are taken from consideration 0.003 g of metal per 1 cm2 of product surface, herewith operation of chemical reduction of metal is replicated multiple. After each two sequential operations of chemical reduction of metal product is heated at 550 - 650 °C during 4 h.

EFFECT: invention provides receiving of solid, uniform, temperature-stable, plastic coating of platinum or iridium of thickness up to 5 mcm on ceramics.

2 cl, 7 ex

FIELD: metallurgy.

SUBSTANCE: inventions relate to field of coating from gold and its alloys on metallic details without current application with usage of compositions, not containing cyanides and other noxious reactants. Method includes defatting, chemical etching, activation, washing and treatment of prepared details by composition for coating. Activation of details is implemented by treatment by composition, containing, wt %: chloroaurate hydrogen acid 0.1-0.3, silver chloride 0.05-0.2, cobalt chloride 0.1-0.3, sal ammoniac 0.1-0.5, propylene carbonate 5-22, dimethyl sulfoxide - the rest, at temperature 70-90 °C during 30-90 seconds, and coating is implemented by treatment of prepared details by composition, containing, wt %: gold halogenide or chloroaurate hydrogen acid, in accounting to metal 0.1-0.5, sal ammoniac 0.2-1.0, boric acid 0.1-1.5, sodium nitrite 0.1-0.5, and/or cobalt chloride 0.1-1.0, and/or metal chloride, forming alloy with gold 0.1-2.0, propylene carbonate 5-22, dimethyl sulfoxide - the rest. Additionally details during the activation process and coating is joggled at a rate 60-90 oscillations per minute.

EFFECT: invention provides creation of reliable and ergonomic method of coating from gold and its alloys on metallic details with ability of detail surface activation, including with sublayer of chemical nickel, composition, accelerating process of growing of gold coating with possible intensification of process at ecologically friendly no-current gilding of details of complex shape, including allowing sublayer of chemical nickel, with receiving of coating of thickness up to 1,5 mcm.

3 cl, 1 tbl, 9 ex

Coated articles // 2413746

FIELD: chemistry.

SUBSTANCE: invention relates to a method of coating articles made from valve metals which are used as component parts of turbomolecular pumps. An article made from a valve metal selected from aluminium, magnesium, titanium, niobium and/or zirconium and alloys thereof, is coated with an oxide ceramic layer formed from metal using a plasma-chemical method. The ceramic layer has a barrier inter-phase layer adjoining the metal, whose surface is coated with a polymer formed from monomers in form of dimers or halogenated dimers of general formula I where R1 denotes one or more hydrogens or halogens; each R2 denotes hydrogen or halogen; and each R3 denotes a xylylene residue with formation of a dimeric structure. Said monomers are incorporated into a capillary system and then polymerised on the surface of the oxide ceramic layer in a vacuum.

EFFECT: invention enables to obtain coatings with uniform surface porosity and high resistance to aggressive and corrosive media.

10 cl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an aqueous anti-corrosion agent for coating metal substrates. The aqueous anti-corrosion agent contains a water-dispersed and/or water-soluble polymerisation product P with covalently bonded ligands A, which form chelating compounds with metal ions freed during corrosion of the substrate and/or surface of the substrate, as well as with cross-linked functional groups B, which can form covalent bonds between themselves, other additional functional groups B' of the polymerisation product P and/or with other functional groups B and/or B' on cross-linking agents V. The polymerisation product P has a polymer base in form of one or more structural elements, selected from a group of polyesters, polyacrylates, polyurethanes, polyolefins, polyatomic alcohols, polyvinyl esters, polyvinylamides and polyalkylene amine. Groups B and B' are (meth)acrylate and ethylacrylate groups, ether and ester vinyl groups, crotonate and cinnamate groups, allyl groups etc. Ligands A are selected from a group comprising urea, amines, amides, imines, imides, pyridines, organosulphur compounds, organophosphorus compounds, organoboron compounds, oximes, acetylacetonates, polyatomic alcohols, acids, phytic acids, acetylenes and/or carbenes. The invention also describes a single- and a two-step method of treating metal substrates using the aqueous anti-corrosion agent described above.

EFFECT: coating provides high anti-corrosion protection of metal substrates.

11 cl, 1 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the paint industry, particularly to aqueous dispersions based on vinylidene fluoride for obtaining protective paints. The vinylidene fluoride-based aqueous dispersions contain polymer particles with average size of 0.260-0.3 micrometres, obtained via polymerisation of vinylidene fluoride-based emulsions, optionally in the presence of one or more fluorinated copolymers, in the presence of a bifunctional surfactant of formula: A - Rf - B (I), where: A = -O-CFX-COOM; B = -CFX-COOM; X = F, CF3; M=NH4 alkali metal, H; Rf denotes a straight or branched perfluorinated chain; or a (per)fluoropolyester chain.The average molecular weight (I) is in the range 650-800. Described also is use of vinylidene fluoride-based aqueous dispersions to produce water-based protective paints and protective paint for metal bases, obtained using vinylidene fluoride-based aqueous dispersions; use of aqueous dispersions of polymers based on vinylidene fluoride to obtain powder used in preparing protective paints for powder coatings.

EFFECT: coatings obtained using paints which contain vinylidene fluoride-based aqueous dispersions have good physical and mechanical properties.

17 cl, 5 tbl, 11 ex, 8 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to chemical industry and specifically to obtaining composite anticorrosion coating materials meant for protecting rusty metal surfaces from corrosion, applied directly onto the rusty metal surface, and obtaining a base - sorption materials from products of processing natural organic compounds of plant origin. The method of obtaining a base for composite anticorrosion coating material involves using cut high density wood as raw material which undergoes hydrolysis with 0.5-0.8% sulphuric acid solution, washing and pressing the hydrolysate, its ammonolysis which is carried out with a mixture containing ammounium hydroxide, sodium citrate, sodium hydroxide, citric acid sodium, water, repeated washing and pressing the ammoniated product, separation into fractions, drying the product to 5-15% moisture content. The product is activated in the presence of ammonium hydroxide, amine additives, catalyst and water, followed by grinding and activation with a composition containing ammonium hydroxide, amine additives, catalysts and water at normal pressure and temperature of 100-150°C until achieving 5-15% moisture content of the product and particle size of 1-10 mcm. The method of obtaining composite anticorrosion coating material involves preparation of a mixture of binding substance and a base for composite anticorrosion coating material, mechanical activation and dispersion of the composition with filler pigments, treatment in the chamber of an apparatus with a vortex layer of ferromagnetic particles, colouring and dilution with diluents-solvents. The material is taken for bottling and packaging.

EFFECT: method enables to shorten the time for obtaining the material and power consumption, while obtaining high-quality anticorrosion coating complex material.

10 cl

FIELD: metallurgy.

SUBSTANCE: in compliance with proposed method, metal is cleaned, subjected to conversion treatment by means of contact with conversion solution containing at least one simple or complex salt of at least one metal. Note here that conversion layer is formed that contains 0.01 to 0.07 mmole/m2 of metal M. If required, is it rinsed by water and/or dried, brought in contact with coating material containing c1) from 5 to 30 wt % of one or several cross-linking burn-in urethane resins with blocked isocyanate groups. Note also that not over 5% of available carbon atoms exist in aromatic and/or unsaturated groups, c2) from 10 to 30 wt % of one or several cross-linking agents for component (c1, c3) from 4 to 30 wt % of one or several antirust pigments, the rest making one or several organic solvents and/or water, and, if required, other auxiliary substances. Produced coat is hardened by heating substrate to at least 100°C.

EFFECT: simplified procedure.

10 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: composition contains epoxy-diane resin modified with copolymer of styrene, methylmethacrylate and methacrylic acid BMS-86, dioctylephthalate, wollastonite and microcalcite, technical carbon, polyethylene polyamine and organic solvent.

EFFECT: coating has high adhesion to metal surfaces 93-97 N/cm, high shear strength 183-189 N/cm and high water-absorption 1,75 - 2% at 20°C.

2 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to coating materials and can be used in anticorrosion fireproof bioresistant coating of different materials. The enamel is a set including the following (wt %): a semi-finished enamel product from brominated epoxy resin in an organic solvent in which filler materials are dispersed 8.52-13.5, pigments 18.27-25.29 and a rheological agent 1.7-2.7, as well as an amine type hardener. The resin base is synthesised from epoxy resin and tetrabromodiane in molar ratio of 3:1 and temperature 130-150°C in the presence of a catalyst - an oligomer of aromatically conjugated hydroxyphenylene in amount of 0.65-0.75 moles, which does not contain amines and is obtained via oxidative condensation of alkyl resorcin at 250°C.

EFFECT: resin base has long working life, good technological characteristics; the coating is fungus-resistant, has self-extinction after coming out of a gas burner flame UL - 94, V0 - 0.

6 cl, 7 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: heat resistant coating composition contains polyorganosiloxane resin, acrylic resin - isobutylmethacrylate polymer, heat resistant pigment, ground mica and/or porous silicate as an aggregate, a rheological additive - bentonite clay, pentaphtol lacquer, thickener - pangel or tixogel and an organic solvent. The porous silicate can be pearlite or kieselguhr and the heat resistant pigment can be aluminium powder or heat resistant pigments of different colours.

EFFECT: coatings obtained using the disclosed composition have good physical and mechanical properties.

3 cl, 3 tbl

FIELD: chemistry.

SUBSTANCE: inhibited composition for corrosion protection of the bottom of autoclaves for producing foamed concrete and other silicate articles contains sodium grease as a base, grade B still bottoms of free fatty acids, Asmol, inert aggregates - talc and titanium dioxide, hardener - magnesium oxide, organic inhibitor IKB-4V, IKB-4TM or TAL-11M, inorganic inhibiting additives - zinc oxide, mixture of sodium molybdate and potassium dichromate in ratio of 1:0.7, diluent - rubber solvent petrol, polymeric petroleum drying oil, monoethanolamine, diethanolamine and triethanolamine.

EFFECT: coatings with good physical-mechanical and anticorrosion properties.

1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an anticorrosion coating composition for metal components based on metal particles in an aqueous dispersion which is based on metal particles in an aqueous dispersion which contains 0.3-24 % organic titanate, 10-40% metal particles or mixture of metal particles, 1-25% silane based binder, and water - the remaining percentage up to 100%, provided that the sum of the percentage of the organic titanate and silane based binder is between 5 and 25%. The invention also relates to an anticorrosion coating for metal components made from the disclosed coating composition, as well a metal substrate onto which the anticorrosion coating is applied through sputtering, drainage-impregnation or centrifugation-impregnation, where the coating layer is then thermally treated, preferably at temperature between 180°C and 350°C for 10-60 minutes by supplying heat through convection or radiation, or for a period of time between 30 second and 5 minutes through electromagnetic induction. The invention also relates to an aqueous composition of C1-C8 tetraalkyl titanate for preparing a composition for coating a metal substrate in an aqueous dispersion obtained from a water-soluble organic solvent, silane-containing binder which has in its structure at least one functional group which can be hydrolysed to a hydroxyl group and water, as well as to use in preliminary processing of adhesives or coatings, for subsequent processing as a metal particle based sealant when passivating substrates based on steel, zinc, aluminium or steel having a zinc based coating, or in an additive for improving adhesion of coatings or adhesives in an aqueous phase.

EFFECT: design of a method of obtaining an efficient anticorrosion coating.

24 cl, 11 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an aqueous composition for coating outer, inner, front and roof surfaces, having bactericidal action. The water paint composition contains elementary silver and at least one additional component selected from a group comprising a silver salt, chitosan and/or chitosan derivatives. The water paint composition contains at least one organic or inorganic binder, and can additionally contain ZnO nanoparticles with average size of 500 nm. The invention also relates to use of silver nanoparticles combined with at least one additional component selected from a silver salt, chitosan, chitosan derivatives and optionally ZnO nanoparticles as a bactericidal agent in aqueous compositions for painting inner, front, roof and outer surfaces. The method of applying the coating on inner, outer, front and roof surfaces of a building involves depositing the water paint composition.

EFFECT: obtaining a composition having highly efficient bactericidal action and does not have allergenic and toxic effect on the human body.

17 cl, 2 dwg, 1 ex

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