Method for composite material receiving

FIELD: metallurgy.

SUBSTANCE: invention concerns method for composite material receiving, including padding, containing stratum of thermoplastic compound, at that padding contains deposited from vapor phase stratum, containing aluminum or aluminum oxide or silicon oxide, including stage of deposition from vapor phase of triazine-bearing compound to padding at pressure 1x10-6 Pa or higher, but not less than 1000 Pa. During the deposition stage temperature of padding is in the range between -15°C and +90°C. Triazine-bearing compound corresponds melamine, melam, melem, melon or its mixtures. Padding before deposition stage from vapor phase is treated by plasma, corona discharge, ultraviolet radiation, electron-beam radiation or reactionary gas.

EFFECT: creating of effective method of composite material receiving.

11cl, 1 ex

 

The present invention relates to a method for producing a composite material that includes a substrate and a layer on the substrate, and the method includes the stage of deposition from the vapor phase, in which the compound containing triisostearate connection, is deposited on the substrate at a pressure below 1000 PA, resulting in a layer.

This method is known from WO 99/66097. In WO 99/66097 treasasturgis layer acts mainly as a barrier layer to reduce, for example, the oxygen permeability ((CRC) (OTR)) substrate. WO 99/66097 specifies various suitable treasasturgis compounds such as melamine.

The disadvantage of this method is that the barrier properties are not always sufficient.

The aim of the present invention is to reduce the above-mentioned drawback.

The purpose of the present invention is achieved by the fact that in the process stage of deposition from the vapor phase, the temperature of the substrate is in the range from -15°C to +125°C.

The advantage of the present invention is that the obtained composite material with improved properties, in particular with improved barrier properties. Surprisingly, the choice of a relatively high substrate temperature gives a composite material with improved barrier properties, whereas in industry the temperatures of the substrate are -20° With or below.

A composite material obtained by the method according to the present invention contains a substrate. Substrate is the material that serves as a carrier layer; it is the object, which is applied to the layer. The substrate can consist essentially of a homogeneous material, or it can itself be non-homogeneous or composite material. The substrate may contain various layers. The substrate may be essentially flat, or it can have a complex three-dimensional shape. Examples of suitable substrates are flexible packaging such as film, fixtures, rigid packaging, such as bottles or pre-molded packaging boxes. Preferably, the substrate includes a polymeric material, paper, cardboard, metal, a compound of the metal, metal oxide, ceramic or a combination of both. Examples of polymer compounds are thermoplastic compounds and thermotherapies connection. Examples of thermoplastic compounds are polyethylene (PE), polypropylene (PP) and polyethylene terephthalate (PET). These thermoplastic compounds are often used in the form of a film either as such or oriented; this orientation may be biaxial, such as, for example, biaxial oriented polypropylene film ((VOR)(TOP)). Preferably, the substrate is HDMI is Tim material, containing precipitated from the vapor phase layer containing aluminum, aluminum oxide, aluminum and aluminum oxide or silicon oxide, resulting in a layer according to the present invention is applied on top of the aluminum - or silicon-containing layer.

A composite material according to the present invention contains a layer on the substrate. The layer is applied to the substrate through the stage of deposition from the vapor phase. The vapor deposition is known as such. As is known, phase vapour deposition is performed under reduced pressure, i.e. a pressure below atmospheric. In the method according to the present invention the pressure is below 1000 PA. At the stage of deposition from the vapor phase compound is deposited on the substrate, forming in the layer. The specified connection according to the invention contains triisostearate connection. In principle, can be selected any triisostearate connection; preferably, triisostearate compound contains melamine, chalk, melon, melamine with polymerizable functional groups, salts of melamine, or a mixture thereof. More preferably, triisostearate compound contains melamine; most preferably, triisostearate compound consists essentially of melamine.

The thickness of the layer being formed on the substrate under deposition from the vapor phase depends on t the left of the destination and can thus vary within wide limits. Preferably, the thickness of the layer is less than 100 microns, more preferably less than 10 μm, and even more preferably less than 1 μm; minimum thickness is preferably not less than 2 nm, more preferably not less than 10 nm.

In the process stage of deposition from the vapor phase, the temperature of the substrate is in the range from -15°C to 125°C. the Temperature of the substrate is defined here as the temperature of the portion of the substrate which is not subjected to vapor deposition. For example, if the stage of the deposition from the vapor phase is carried out on the film that goes over the causes of the drum with adjustable temperature, temperature of the substrate is temperature, which is regulated by causing the drum, thus, the temperature of the portion of the film surface, which is in direct contact with damaging the drum. In this case, and due to the fact that the deposited compounds often have a temperature much above 125°usually takes place (as you know), that the temperature of the side of the substrate, which is covered, is higher than the temperature of the parties, which are not covered.

It was found that when the temperature of the substrate rises to -15°and With higher barrier properties of the composite material is improved in comparison with the stage of deposition from the vapor phase, where the temperature of the substrate composition is employed, -20° C or lower. On the other hand, in order to maintain an acceptable deposition rate, and in order to ensure that the substrate remained whole (i.e. undeformed, nerasplativshegosya or destroyed), it is usually necessary that the temperature of the substrate remained below 125°With, or much less than that required its own properties of the substrate, at the same time staying above -15°C. Preferably, the temperature of the substrate during a stage of deposition from the vapor phase is at -5°, 0°or 5° (C or higher; more preferably, this temperature is at 10°, 15°or 20°C or higher. It was found that when the temperature of the substrate increases fairly above -15°installed even further improve the barrier properties. As stated above, because of the stability of the substrate and/or the savings rate may be useful or necessary to ensure that the temperature of the substrate during a stage of deposition from the vapor phase remained at or below 125°With, preferably, at or below 90°S, more preferably at or below 60°s or 50°With, in particular, at or below 40°and most preferably, at or below 30°C.

Ways providing certain temperature of the substrate, known as such. One such way in which particularly the th temperature of the substrate, is applicable in the case where there is at least one section, plane or side of the substrate, where the layer is not deposited from the vapor phase; and the said section plane or side may then come into contact with a cooled or heated surface by bringing the temperature up to the desired level and to maintain it. As an example, it is known that in the case where the substrate is a film, stage and deposition from the vapor phase is carried out as a semi-continuous or continuous method, resulting in a deposited layer on the side of the film, the film can be directed over a roller with an adjustable temperature, also called causing the drum, so that the other side of the film (where not deposited layer) is in contact with the roller with adjustable temperature before and/or during and/or after the stage of deposition from the vapor phase.

Stage deposition from the vapor phase according to the present invention is carried out at a pressure equal to or below 1000 PA. You know, essentially what stage of deposition from the vapor phase can be carried out at a pressure below atmospheric, such as at the specified 1000 PA, or at a lower pressure, such as at 100 PA or 10 PA or lower. In the examples of WO 99/66097 pressure was even reduced to the range from 5x10-3PA to 1x10-2PA. It was unexpectedly set, h is about properties of the composite material, such as barrier properties, can be even further improved by reducing the pressure at which stage of deposition from the vapor phase, preferably up to 4x10-3PA or lower. More preferably, the phase deposition from the vapor phase is carried out at a pressure of 2x10-3PA or lower or 1x10-3PA or lower; in particular, the stage of deposition from the vapor phase is carried out at a pressure of 5x10-4PA or lower or 1x10-4PA or lower; more specifically, the stage of deposition from the vapor phase is carried out at a pressure of 5x10-5PA or lower or 1x10-5PA or lower; most preferably, the phase deposition from the vapor phase is carried out at a pressure of 5x10-6PA or lower or even 1x10-6PA or lower. Currently, it is believed that the pressure below 1x10-10PA does not provide additional benefits, as specified.

In an alternative method according to the present invention the effect of the pressure reduction phase deposition from the vapor phase to 4x10-3or below on the properties, for example, the barrier properties of the obtained composite material is that this measure may be partially or even completely replace the favorable impact of measures to bring the temperature of the substrate during a stage of deposition from the vapor phase to range from -15°C to 125°C. In this alternative is ariante may be possible when the temperature of the substrate is at -15°C, at -20°C, at -40°or even at -60°With or below.

The layer usually contains cereals containing triisostearate connection. Grain, in which the compound is present in crystalline and unpolymerized form and separated by boundary surfaces are generally for crystallizing compounds well-known to specialists in this field of technology. The optimal effect of the properties of a given layer, in particular related to barrier properties, can be achieved if the layer consists essentially of grains containing triisostearate connection. If the layer consists entirely or almost entirely of grains containing triisostearate connection, it may be preferable that the entire layer essentially consists of createnodeviewer connection.

Grains in the layer have a size, which is defined here as the largest dimension parallel to the substrate surface (i.e. as seen from above), in grain. It was found that the average size treasasturgis grains in the second layer can be as important or even more important than the thickness of the second layer in the determination of important characteristics, such as barrier properties. Without binding itself to any specific theoretical explanation, it is assumed that the optimal barrier properties are achieved as opposed to what can be expected of the person skilled in the technical field) with the concentration on the number and size of interfaces between grains in a greater degree than concentrating on the thickness of the deposited layer. It is believed that the interface between grains are relatively weak in places, giving the barrier properties of the composite material; thus, if the average grain size is too small, there are so many interfaces that it negatively affects the barrier properties. On the other hand, if the average grain size becomes too large, it is assumed that the surface of the partition become disproportionately more, so again deteriorate barrier properties. The average grain size is preferably not less than 10 nm, more preferably not less than 50 nm, even more preferably at least 100 nm, and most preferably not less than 200 nm. The average grain size is preferably the largest 2000 nm, more preferably, at most 1000 nm, even more preferably, at most 600 nm, and most preferably, at most 400 nm. The average size in the context of the present invention means srednekamennogo value. In a preferred embodiment, the layer essentially consists of createnodeviewer connection triazine crystallize is the cue structure in the grains was not significantly interrupted.

In the method according to the present invention stage of deposition from the vapor phase, preferably carried out in such a way that the average size treasasturgis grains is in the range from 10 nm to 2000 nm. It was found that the average amount deposited from the vapor phase grains and other depends on the number of nucleation points on the surface, on which grow the grain: the greater the number of nucleation points, the smaller the average grain size. The average size of precipitated grains can thus be varied by regulation of the conditions during the stage of deposition from the vapor phase, which affect the number of nucleation points from which to grow grain. It was found according to the invention that the number of points of nucleation increases with increasing difference between the temperature of deposition, i.e. the temperature at which the heated triisostearate connection, and the temperature of the substrate. Preferably, the temperature difference is in the range of 150°370°With respect to the temperature interval substrate according to the invention. It was also found that the number of points of nucleation decreases when increasing the pressure at which stage of deposition from the vapor phase. Preferably, the pressure at the stage of deposition from the vapor phase find the camping in the range from 10 -6PA to 10-2PA. In addition, it should be noted that the nature of the substrate also affects the number of nucleation points, which are formed. Specialist in the art can, therefore, use descriptions, considering the specified temperature difference and pressure, to determine through experimentation, what are the conditions of the method are optimal for the stage of deposition from the vapor phase to obtain an average grain size in the preferred range, as given above.

It may be useful to improve the properties of the composite material in the method according to the present invention, even when passing the additional substrate stage way before or during the stage of deposition from the vapor phase. Examples of such additional stages of the process are: stage stitching, which triisostearate connection layer interacts with itself or with another compound, which was either put together in a layer, or separately brought into contact with the layer; plasma treatment; treatment by corona discharge; the use of ultraviolet radiation; application of electron beam radiation. This additional step of the method may be useful in improving some of the set layer properties, such as adhesion, moisture resistance, or the resistance to scratching. An additional with the pushing method can lead to changes in grain size and/or structure of the layer.

Preferably, the substrate before or during the stage of deposition from the vapor phase is treated with plasma, corona discharge, ultraviolet radiation, electron beam radiation or reactive gas. The reaction gas is a gas that is capable of interacting with trainstation connection and/or with the substrate. This interaction may occur immediately or may take place later. This interaction can take place either without help or with the help of auxiliary means, such as temperature or radiation treatment. The reaction gas contains, preferably water and/or formaldehyde. In a preferred embodiment, the substrate is a composite material containing aluminium-containing layer, so treasasturgis layer is deposited on top of the aluminium-containing layer and the reaction layer contains water vapor. Through a chemical reaction of water vapor with aluminum on the surface of the aluminium-containing layer formed compounds that improve adhesion createnodeviewer layer to the substrate.

Preferably, the composite material during the stage of deposition from the vapor phase or after it is treated with plasma, corona discharge, ultraviolet radiation, electron beam radiation or reactive gas. The reaction gas contains, preferred is entrusted, water and/or formaldehyde.

In a variant of the method according to the present invention to a composite material is added to the second layer deposited from the vapor phase layer, which contains triisostearate connection (which in this case is called the first layer). The second layer can be deposited from the vapor phase on the first layer, but can also be caused by any other known method, such as lamination. The second layer may contain any connection depending on options and/or the desired properties of the composite material. Examples are thermoplastic or thermoturbidimetry polymeric compound, triisostearate connection, which may be the same connection as in the first layer, or different compound, a metal compound, such as aluminum, a metal oxide, such as, for example, aluminum oxide. The second layer can be a composite material.

From the point of view of technology deposition from the vapor phase, is used to create the first layer, and from the point of view of the characteristics treasasturgis compounds, it was found that the first layer can act as an intermediate layer. The intermediate layer here means a layer that straightens or smoothing at least a portion of any surface irregularities, when it is present on the surface of the substrate, h is of the second layer is applied on a much smoother surface (i.e. with less roughness of the surface); this has the advantage that it reduces the risk of destruction of the second layer. It was found, moreover, that, when smoothing the first layer should be the main function and when its function as a barrier layer is less important, the temperature of the substrate during a stage of deposition from the vapor phase can be in a wider range than the above, thus, preferably, in the range from -60°C to 125°S, more preferably from -30°C to 50°C.

The present invention also relates to a composite material obtained by the method according to the present invention, as described above. The specified composite material can be used in any number of applications, particularly in applications where the required barrier properties, such as low CRC, such as, for example, in a package kislorodozaschitny or perishable products such as food.

The present invention will be illustrated using the example and comparative experiment.

Example 1

Layer consisting of melamine, precipitated from the vapor phase on a substrate in the form of a film consisting of a biaxially oriented polypropylene ((BOPP)(TOP)). Stage vapour deposition is carried out at a pressure of 10 PA or about 1x10-4Athi. The temperature of the substrate is 20°C. Chalk is in evaporated from the crucible; melamine in the crucible is maintained at a temperature of 310°C.

Melamine is deposited on the substrate. The substrate is directed along the crucible with a speed of 7 m/s; this is a very high speed, reflecting the conditions that exist in industrial practice. The obtained composite material has an oxygen permeability ((OTR) (CRC)) 47 cm3/m2·bar·day.

Comparative experiment 1

A composite material was obtained in the same manner as in example 1, except that the temperature of the substrate is -20°instead of 20°C. the CRC is 120 cm3/m2·bar·day, reduced from 1600, as measured on the substrate (TOP film) without any layer deposited on it.

From the example and comparative experiment 1 it is easy to see that although there is a method already implements a favorable reduction in CRC compared to the uncoated substrate with the improvement in the barrier properties, the method according to the present invention realizes a further reduction of the CRC, that is, gives a further improvement of the barrier properties.

Used in the invention homologues of melamine:

The chalk - (1,3,5-triazine-2,4,6-triamine-n-(4,6-diamino-1,3,5-triazine-2-yl).

Grind (2,5,8-triamino-1,3,4,6,7,9,96-heptanophenone).

Melon (poly (8-amino-1,3,4,6,7,9,96-heptanophenone-2,5-diyl)imino).

1. A method of obtaining a composite material which, includes a substrate containing at least a layer of thermoplastic compounds, and the substrate contains precipitated from the vapor phase layer containing aluminum or aluminum oxide or silicon oxide, comprising the stage of deposition from the vapor phase, which triisostearate compound precipitated on the substrate at a pressure of 1·10-6PA or higher, but lower than 1000 PA in the resulting layer, and during the stage of deposition from the vapor phase, the temperature of the substrate is in the range between -15 and +90°and where triisostearate compound is a melamine, chalk, grind, melon, or a mixture thereof.

2. The method according to claim 1, wherein during stage vapour deposition temperature of the substrate is in the range between 0 and 50°C.

3. The method according to claim 1 or 2, in which stage of deposition from the vapor phase is carried out at a pressure below 5·10-3PA.

4. The method according to claim 1, in which triisostearate compound contains melamine.

5. The method according to claim 1, wherein the substrate before the stage of deposition from the vapor phase is treated with plasma, corona discharge, ultraviolet radiation or electron beam radiation.

6. The method according to claim 1, wherein the substrate before the stage of deposition from the vapor phase process of the reaction gas.

7. The method according to claim 6, in which the reaction gas contains water and/or formaldehyde.

8. The method according to claim 1, in which, after the stage of deposition from the vapor phase createnodeviewer connection, over a layer is applied an extra layer.

9. The method according to claim 8, in which the additional layer is applied by lamination.

10. The method according to claim 8 or 9, in which the additional layer contains a thermoplastic connection.

11. The method according to claim 1, wherein the substrate includes a polymer film, in particular biaxially oriented polypropylene film.



 

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