Electricity-conductive compound in the form of flocculent particles and electricity-conductive composition

FIELD: electrical engineering; electricity-conductive compound in the form of flocculent particles.

SUBSTANCE: proposed compound has titanium oxide with mean large diameter of 1 to 100 μm and mean thickness of 0.01 to 1.5 μm, potassium in amount of 0.03 to 5 mass percent in the form of potassium oxide (K2O), as well as first electricity-conductive layer which is formed on surface and has in its composition tin oxide and antimony, and second electricity-conductive layer which is formed on first electricity-conductive layer and has in its composition tin oxide. Proposed electricity-conductive composition in the form of flocculent particles is capable of imparting good electricity-conductive properties even when formed in layer of 1 to 10 μm in thickness.

EFFECT: improved properties of electricity-conductive composition.

6 cl 3 tbl, 6 ex

 

The technical FIELD

This invention relates to a conductive composition in the form of flocculent particles and electrically conductive composition.

The LEVEL of TECHNOLOGY

For the manufacture of bumpers, side door cables, door reflectors and other exterior finishing parts of the car usually use various synthetic resins, such as polyolefin, polyamide and styrene resin in order to achieve the reduction of weight of the vehicle and, therefore, savings in fuel consumption. This was clearly demonstrated in the recent sales of passenger cars with doors made of synthetic resin.

Exterior decoration parts cars, made of synthetic resin (hereinafter called "made of resin exterior finishing details"), usually colored dye, the appropriate color on the main body of the car. When applying coatings on these are made of resin exterior finishing details, which usually have insulating properties inherent in synthetic resins, typically use a method that includes providing a surface conductive layer of primer that contains astringent resin and electroconductive composition, and then electrostatic powder coating color film on the primer layer. In circumstances when the pre is brasenia global warming requires a reduction of exhaust emissions, reducing the thickness of the conductive layer of primer and a layer of color film becomes one of the important technical goals in the specified method of electrostatic coating for additional fuel economy. In particular, the film thickness of the conductive layer of primer, as expected, can be reduced to a level of 1-10 microns, while maintaining its specific surface resistance at the level of 104-108Ωthat is required for the formation of a homogeneous thin layer of color film.

Examples of electrically conductive materials contained in the conductive primer layer are powdered electrically conductive material such as carbon black, graphite and metal powder; fibrous conductive materials such as carbon fiber, potassium titanate coated on the outside of the carbon soot or other carbon materials, and fiber titanium oxide; and conductive materials in the form of flocculent particles, such as Nickel-covered mica and metal flocculent particles; and others (see, for example, Japanese patent published application Nos. Sho 57-180638, Sho 58-76266, Sho 61-218639, Hei 2-120373, Hei 2-194071, Hei 10-309513 and 2001-98092). However, if the conventional conductive materials used in the formation of a conductive layer of primer with a level of specific surface, the resistivity of 10 4-108Ωthat is suitable for subsequent electrostatic coating, the required load make it difficult to decrease the thickness of the conductive layer of primer. When attempting to reduce the thickness of the film can be reduced loading of conventional conductive materials. When these reduced loads surface resistivity may not reach the desired level and can vary widely in different locations. This feature causes uneven coating. Thus, the conductive primer layer containing the specified standard of electrically conductive materials that are difficult to reconcile level specific surface resistance of 104-108Ω and the film thickness of 1-10 microns.

Known conductive material in the form of flocculent particles obtained by the sequential formation of the first conductive layer containing tin oxide and antimony oxide, and the second conductive layer containing tin oxide on the front side of the substrate (Japanese patent published application No. Hei 10-147891). It is also known that the substrate material may be selected from such flocculent particles, as mica, talc, glass flakes, flakes of aluminum oxide and flakes titanium dioxide (flakes of titanium oxide). However, these electraprobe the materials in the form of flocculent particles sometimes painted. Accordingly, in the case when there is a layer color film of beige, light blue or other bright colors, the use of such electrically conductive materials for the primer layer adversely affect the color of the colored layer film. None of these standard known flaky electroconductive material does not give a thin film, which satisfies both the level of the specific surface resistance of 104-108Ωand the level of film thickness of 1-10 microns.

The INVENTION

The purpose of this invention is to provide an electrically conductive composition in the form of flocculent particles, which, even being formed in a layer of thickness of 1-10 microns, able to tell a good conductive properties, as well as to provide electrically conductive composition comprising the composition is introduced into the binder.

An electrically conductive composition in the form of flocculent particles of the present invention is distinguished by the content of titanium oxide with an average largest diameter of 1-100 μm and an average thickness of 0.01 to 1.5 μm, and 0.3-5 wt.% potassium in the calculation of the oxide of potassium (K2About), and the first conductive layer contains tin oxide containing antimony, and placed on the surface of titanium oxide, and the second conductive layer contains tin oxide and placed on the first conductive layer.

In the invention, the average major diameter and the average thickness can be determined (using) scanning electron microscope (SEM) or transmission electron microscope (TEM). Medium large diameter can be approximately measured by laser diffraction device for measuring the size distribution of the particles. Inorganic lamellar structures, flocculent or sheet form, such as conductive compositions in the form helpguide particles of the present invention, typically have a rectangular or polygonal configuration. Due to such uneven configuration, the diameters of the particles are different in different measurement. The term "large diameter"as used in this application refers to the longest of these diameters of the particles.

In this invention, the first conductive layer preferably contains 0.1 to 50 wt.% antimony component in the form of antimony oxide (Sb2O3) per 100 wt. parts of the compound of tin as tin oxide (SnO2).

An electrically conductive composition in the form of flocculent particles of this invention can be obtained by the action of the connection of the main character, has the effect of swelling interlayers on the layered Titanic acid to delamination when this layered Titanic acid in cereals Titanic acid coating of tin compounds for the formation of the first conductive layer on the titanium acid in the form of flocculent particles, applying the compounds of SN to form the second elektroprovodnog the layer on the first conductive layer and subsequent heat treatment of this combination.

Electroconductive composition of the present invention differs in that it contains a binder and an electrically conductive composition in the form of flocculent particles of the present invention, introduced into the binder.

Preferably the conductive composition in the form of flocculent particle load in the amount of 5-50 wt. parts per 100 wt. parts of the binder.

A binder may be one or more types selected from thermoplastic resins, thermosetting resins, aggregates of inorganic compounds and metal-containing organic compounds.

DETAILED EXPLANATION of INVENTION

Characteristically, the conductive composition in the form of flocculent particles of the present invention uses as a substrate Titanic acid in the form of flocculent particles (hereinafter referred to simply as "Titanic acid in the form of flocculent particles, if not exactly specified otherwise)that have an average largest diameter of 1-100 μm, preferably 1-10 μm, have an average thickness of 0.01 to 1.5 μm, preferably from 0.01 to 1.0 μm, and contain 0.3-5 wt.% potassium in the form of potassium oxide (K2O).

Specified Titanic acid in the form of flocculent particles can be obtained, for example, processing of layered titanate (1)represented by the General formula(where M is a metal with a valence of 1-3, is a defective center at the location of the Ti, x represents a positive real number and satisfies the inequality 0 < x < 1.0, a, and y and z independently of one another represent 0 or a positive real number and satisfy the inequality 0 < y + z < 1,0), acid so that 75-90% of ions To and/or M gamestyles hydrogen ions or hydronium ions to obtain a layered Titanic acid; and the subsequent action of the compounds of basic character, with the effect of causing the swelling interlayers for laminated titanium acid with delamination with this layered Titanic acid.

In the General formula (1) M is a metal that is different from It has a valence of 1-3, and preferably is at least one metal selected from Li, Mg, Zn, Cu, Fe, Al, Ga, Mn and Ni.

Layered titanate (1) can be obtained, for example, the methods proposed in the prior art such as Japanese patent No. 3062497. In particular, the starting material is obtained from the corresponding metal oxides K, M and Ti, or related compounds, which when heated give these oxides. The indicated starting material and one or more compounds selected from halides or sulfates of alkali metals or alkaline earth metals, mixed so, copymessage the ratio of flux/initial substance 0,1-2,0. The mixture was then calicivirus at 700-1200°to obtain the layered titanate.

Thermal processing of layered titanate (1) is conducted according to a known method, for example, by adding acid to the aqueous suspension of layered titanate (1), preferably with stirring. The concentration of the layered titanate (1) is not specifically defined and may be appropriately selected from a wide range depending on the type of layered titanate (1) and the like. Taking into account the effective substitution of hydrogen ions or hydronium 70-99% of potassium ions and/or ions of M, their concentration is usually supported at the level of 0.01-10 wt.%, preferably 0.1 to 5 wt.%. The type of acid is not specifically defined. Apply the known state of the art acid without restrictions. Examples of acids are mineral acids such as hydrochloric acid, sulfuric acid and nitric acid; organic acids such as formic acid, acetic acid, propionic acid and oxalic acid; and the like. Among them, preferred inorganic acid. In particular, the preferred hydrochloric acid. These acids may be used individually or, if necessary, in combination. The acid is usually used in the form of its aqueous solution. The concentration of the aqueous acid solution is not specifically defined and may change the I in a wide range depending on the type of acid and the like. Taking into account the effective substitution of hydrogen ions or hydronium 70-99% of potassium ions and/or ions of M, the concentration of the acid is usually supported at the level of 0.0001-10 wt.%, preferably 0.001 to 0.1 wt.%. This acid treatment may be repeated. By displacing the hydrogen ions or hydronium in layered titanate (1) 70-99% of the ions and/or ions M polycut layered Titanic acid (1A).

Then on the specified layered Titanic acid (1A) of the act by the connection of the main character, can cause swelling layers, delamination, while receiving Titanic acid in the form of flocculent particles. More specifically, the connection of the main character, can cause swelling interlayers may be, for example, is added with stirring to the aqueous suspension of lamellar Titanic acid (1A).

The concentration of the layered Titanic acid (1A) in water suspension is not specifically defined and may be selected within a wide range depending on types of layered Titanic acid (1A) and joining the main character, the reaction conditions and the like.

Examples of compounds of the main character, can cause swelling interlayers are bonds alkylamines, such as methylamine, ethylamine, n-Propylamine, diethylamine, triethylamine, butylamine, pentylamine, hexylamine, octylamine and dodecylamine and their salts; alkanolamine is, such as ethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine and 2-amino-2-methyl-1-propanol; hydroxides of Quaternary ammonium bases such as hydroxide of Tetramethylammonium, the hydroxide of tetraethylammonium, the hydroxide of tetrapropylammonium and tetrabutylammonium hydroxide, and their salts; salts of Quaternary ammonium bases, such as salt cetyltrimethylammonium, salt stearylamine, salt designed, salt dimethyldodecylamine, salt dimethyldiallylammonium; and the like. These connections main character can be used individually or in combination. Download connection main character is preferably 5-40 equivalent % of the total equivalent of the layered Titanic acid (1A). This gives the possibility to stratify the layered Titanic acid to titanium acid in the form of flocculent particles with an average thickness of 0.01 to 1.5 μm.

Preferably when adding the connection of the main character with stirring using a high shearing force. This results in Titanic acid in the form of flocculent particles that are comparable in size distribution of particles with a layered titanate as the original substance. Also prevent and fine grinding of the obtained titanium acid in the form of flocculent h is CI.

After exposure to the connection of the main character, if necessary, may be followed by treatment with acid to remove the remaining part of the connection of the main character so that Titanic acid in the form of flocculent particles contained 0.3 to 5 wt.% potassium in the form of potassium oxide (K2O).

Received by the specified method Titanic acid in the form of flocculent particles consists of from several tens to several hundreds of layers has an average major diameter of typically 1-100 μm, preferably 1-10 μm, and the average thickness of usually 0.01 to 1.5 μm, preferably 0.01 to 1 μm, and contains 0.3 to 5 wt.% potassium in the form of potassium oxide (K2O).

If the content of potassium in Titanic acid in the form of flocculent particles falls below 0.3 wt.%, may have difficulty maintaining its desired shape. In addition, when forming a thin film of resin containing Titanic acid in the form of flocculent particles, may be undesirable staining. If the potassium content exceeds 5 wt.%, formed in electrically conductive connection in the form of flocculent particles can be reduced conductivity, leading to the impossibility of obtaining the desired level of electrical conductivity.

The first and second conductive layers can be deposited on the Titanic acid in the form of flocculent particles according to the method described, for example, the Japanese laid patent application No. Hei 10-147891.

In an exemplary procedure according to this method Titanic acid in the form of flocculent particles are first dispersed in water. Supporting system is typically at pH 2-5 by adding an alkaline agent is added to it by the combination of tin and a compound of antimony to mix with it (the first stage). Then, maintaining the system at pH 2-5 by adding an alkaline agent, similarly to the first stage, it adds a connection tin for mixing with her (second stage). Removing solids from the mixture, followed by drying and heating results in electrically conductive composition in the form of flocculent particles of the present invention.

In the first stage, the concentration of Titanic acid in the form of flocculent particles in the water dispersion is not specifically defined and may be selected appropriately from the range, which enables smooth flow and easy the first stage of the reaction.

Preferably a compound of tin, used in the first stage, is a compound of tetravalent tin. Examples of these compounds include tin chloride, tin sulfate, nitrate, tin and the like. These tin compounds can be used individually or in combination. Compound of antimony is a compound of trivalent antimony, which may take many fo the we such as chloride, sulfate and nitrate. It is usually chloride (antimony trichloride) is easily accessible. These antimony compounds can be used individually or in combination. The number of compounds of tin and antimony compounds at this stage is not specifically defined and may be selected from a wide intervals, depending on the desired conductive characteristics and intended use. The total number of these compounds (in the form of their oxides, SnO2and Sb2O3) is usually at least 3 wt. parts, preferably 5-20 wt. parts, per 100 wt. parts of Titanic acid in the form of flocculent particles. In addition, the ratio of the number of tin compounds to the compound of antimony is not specifically defined and may be selected from a wide range depending on various conditions, for example, the desired conductive characteristics of the electrically conductive composition in the form of flocculent particles and its intended use. Compound of antimony is usually used in an amount of 0.1-50 wt. parts, preferably 1-30 wt. parts per 100 wt. parts of the compound of tin, in the form of their respective oxides. Compound of tin and a compound of antimony is preferably used in the form of an aqueous solution. The concentration of each compound in the aqueous solution is not specifically defined the s and may be acceptable manner selected from a wide interval, which ensures a smooth flow of the reaction. Preferably these compounds are used in a mixed form.

The alkaline agent may be selected from the known state of the art. Examples of alkaline agents are the hydroxides of alkali metals such as sodium hydroxide and potassium hydroxide; carbonates of alkali metals such as sodium carbonate and potassium carbonate; ammonium carbonate; aqueous ammonia; and the like. These alkaline agents may be used individually or in combination, if necessary. Preferably, the alkaline agent is used in the form of an aqueous solution. The amount of alkaline agent may be selected appropriately to maintain the system at pH 2-5.

The first stage can be carried out, for example, precapitalism aqueous solution containing a compound of tin and a compound of antimony, to aqueous dispersions of electrically conductive titanium acid in the form of flocculent particles under stirring and while maintaining the system usually at pH 1-5 by adding dropwise an aqueous solution of an alkaline agent. This reaction can be carried out at room temperature, but preferably at an elevated temperature of 50-80°C. the Reaction can be completed at the end of the addition. Preferably the reagents allowed to stand at paramasivan is about 0.5-5 hours after the addition. This reaction gives the tin hydroxide and the hydroxide antimony in the system. They settle on the surface of Titanic acid in the form of flocculent particles with the formation of the first deposited layer.

The second stage can be carried out in the same manner as the first stage, except that instead of tin acid and compounds of antimony is used as a compound of divalent tin. For example, the second stage can be carried out by addition of compounds of divalent tin to the water dispersion of electroconductive titanium acid in the form of flocculent particles containing on the surface of the first deposited layer obtained in the first stage, while stirring and maintaining the system, usually at pH 2-5 adding dropwise an aqueous solution of an alkaline agent.

The connection of the tin is a compound of divalent tin. Specific examples are tin chloride, tin sulfate, nitrate, tin and the like. These compounds of divalent tin can be used individually or in combination. The amount of compounds of divalent tin is not specifically defined and may be appropriately selected within a wide range depending on various conditions, for example, the intended use of the obtained conductive composition in the form of flocculent particles, the number is, I can pay tithing deposited layer and the proportions of tin hydroxide and hydroxide antimony, present in the deposited layer. The connection of divalent tin can usually be added in an amount of at least 3 wt. parts, preferably 5-20 wt. parts, per 100 wt. parts of Titanic acid in the form of flocculent particles as a core material (core). The connection of divalent tin is usually used in the form of an aqueous solution. The concentration of divalent tin in aqueous solution is not specifically defined and may be appropriately selected from the interval, ensuring a smooth flow of the reaction used in the reaction conditions.

Like the first stage, the second stage can also be carried out at room temperature, but preferably can be carried out at elevated temperatures of 50-80°C. the Reaction can be completed at the end of the addition. Preferably the reagents are allowed to stand with stirring for about 0.5 to 5 hours after the addition. The reaction leads to the formation of the system of the hydroxide of the divalent tin. He settles on top of the first deposited layer on the titanium acid in the form of flocculent particles.

To remove solids from the aqueous dispersion obtained after the second stage, can be used a means of division, known at the present level of technology, such as the filter is of centrifuging.

The solid is usually dried at a temperature of 50-200°C, preferably 90-120°C. Drying usually are for 1-30 hours, preferably 10-20 hours.

After drying, the solid is heated at a temperature of 200-1000°C, preferably 300-600°C. Heating usually last from 30 minutes to 5 hours, preferably 1-3 hours. By the specified heating part of Titanic acid as filler converted into titanium dioxide. Additionally hydroxide tin (II)hydroxide tin (IV) and hydroxide antimony converted into the corresponding oxides.

Obtained in this way electrically conductive composition in the form of flocculent particles of the present invention is a conductive material which contains titanium oxide in the form of flocculent particles as the substrate, the first layer containing tin oxide, which includes antimony, and deposited on the surface of titanium oxide in the form of flocculent particles, and a second layer containing tin oxide and deposited on the first layer. In the above example, obtain a tin oxide, existing both in the first and second layers contains a combination of tin oxide (II) and tin oxide (IV). This structure gives improved electrical conductivity properties of the material of the present invention. However, it is not intended to exclude cases where both the first and second layers soda is RATM or tin oxide (II), or only tin oxide (IV). The thickness of the first layer is not specifically defined, but can usually be 5-20 nm. The thickness of the second layer is usually equal to 5-20 nm.

Believe that the antimony in the first conductive layer of the electrically conductive composition in the form of flocculent particles of the present invention exists in the form of its oxide or solid solution with tin oxide.

Titanic acid in the form of flocculent particles may be subjected to any known surface treatment or surface coating to improve its dispersive ability of the pigment. If necessary, a dispersion of titanium acid in the form of flocculent particles may be added to the dispersion stabilizer.

Electrically conductive composition of this invention contains a binder and the above-mentioned electrically conductive composition in the form of flocculent particles. The proportion of mixing these components is not specifically defined and may be appropriately selected from a wide range depending on the type of binder used, the intended use of the obtained composition and other things. Given conductivity, mechanical strength, machinability, properties, formation of thin films obtained composition, the conductive composition in the form of flocculent particles are usually used in amounts of 5 to 200 wt. parts, preferably 10-50 wt. parts per 100 wt. the hour is her binder.

Binder is not specifically defined by type. Applicable binder materials known at the present level of technology, if only they can dispersing electrically conductive composition in the form of flocculent particles. Among them, preferred thermoplastic resins, thermosetting resins, inorganic fillers, metal-containing organic compounds and the like. These binders can be used individually or in combination, if necessary.

Specific examples of thermoplastic resins are polyethylene, polypropylene, polyisoprene, chlorinated polyethylene, polyvinyl chloride, polybutadiene, polystyrene, high impact polystyrene, a copolymer of Acrylonitrile and styrene (AS), acrylonitrilebutadienestyrene (ABS), a ternary copolymer of methyl methacrylate, butadiene and styrene (MBS)copolymer of methyl methacrylate, Acrylonitrile, butadiene and styrene (MABS), a ternary copolymer of Acrylonitrile, kilowog rubber and styrene (AAS), polyacrylate, polyesters (polyethylene terephthalate, polybutylene terephthalate, polyethylenterephthalat and the like), polycarbonate, simple Polyphenylene ether, modified simple Polyphenylene ether, aliphatic polyamide, aromatic nylon, polyster, a polyimide, a simple polyetherketoneketone, polysulfone, polyacrylate, simple polyetherketone, simple Polief reconocen, simple preferential, simple positiveresults, simple polyethersulfone, polybenzimidazole, polyamidoimide, simple polyetherimide, Polyacetal, liquid crystal polymer and the like. These thermoplastic resins may be used individually or in combination, if necessary.

Specific examples of thermosetting resins are polyurethanes, phenolic resins, melamine resins, urea resins, unsaturated complex polyester resin, diallylphthalate resin, silicone resin, epoxy resin (epoxy resin bisphenol a epoxy resin, bisphenol F, fenomenologia epoxy resin, resolvability epoxy resin, cycloaliphatic epoxy resin, epoxy resin of complex glycidyloxy esters, epoxy resins from glycidamide, heterocyclic epoxy resin, epoxy resin modified with urea, epoxy resins, brominated bisphenol a), and the like. These thermosetting resins may be used individually or in combination, if necessary.

Specific examples of inorganic fillers are insoluble infusible or plastic binder, obtained by curing one or more silicates, phosphates, borates and other inorganic curable substances, their predestin the Cove or hydrates, under the action of heat, light, electron beam or catalyst. These inorganic fillers can be used individually or in combination, if necessary.

Specific examples of metal-containing organic compounds are organosilicon compounds technologicheskie compounds, phosphorus compounds, boron compounds and the like. These metal-containing organic compounds can be used individually or in combination, if necessary.

Among the above binder of thermoplastic resin and thermosetting resin are preferably applicable in this invention. Especially it is preferable to use a thermoplastic resin.

Electrically conductive composition of this invention may optionally contain one or more of the following components that will have no adverse impact on the desired properties of conductive material different from the electrically conductive composition in the form of flocculent particles of the present invention, the particles of which have a layered (or flaky, or scaly), fibrous, granular and globular form; inorganic fillers; pigments; organic solvents; antioxidants; antistatic agents; lubricants for the form; lubricants; stabilized the market of heat; antipyrene; agents against leakage; UV absorbers; light stabilizers; sutomiscica, absorbing light; inactivator metal; antioxidants; plasticizers; agents for improving the impact strength, and agents that improve compatibility.

Electrically conductive composition of this invention can be obtained by mixing and/or kneading a binder and electrically conductive composition in specific quantities, and possibly other additives in suitable quantities by methods known at the present level of technology. These components, respectively, in the form of powder, beads, flakes or granules may be mixed using an extruder, such as an extruder with a single screw or double screw, and/or kneaded using a kneading machine such as a mixer, a Banbury mixer, pressure, or the two-shaft mixer, obtaining at the same time, for example, electrically conductive material of the present invention. The composition may be molded into a film, sheet, or another arbitrary shape by a known processing method such as extrusion, injection, extrusion or casting. In addition, the composition can also be made in the form of adhesive, paint, ink or paste, depending on its intended use.

In addition to using as primers for electrostatic damage to the module the practical coating of plastic exterior parts, electroconductive composition of the present invention can find various applications that require electrical conductivity, by appropriate selection of the types of the binder serving as a matrix, and other components depending on the particular application.

Specific applications include building and coating composition for slot machines and electric and electronic devices such as displays, personal computers, word processors, CD players, MD players, DVD players, head stereophony, portable telephones, PHS (miniature cordless phones), PDA (portable digital devices, such as electronic organizers), transmitters, cameras, digital camera, camera, copier (device) for flat paper, printers, and Fax machines; structural details (e.g., belts, coils, supports the rotating parts, carrier tape, coil for Nessa tape and reel for magnetic tape) and packaging materials (e.g., bags, trays, cassettes and containers); working boards for use during transportation of the electronic parts and precision devices, for example, sheets, films, trays, carriers, wafer baskets and packaging for use in transporting IP (integrated circuits), LSI (large-scale integrated circuits and other semiconductor elements;connectors and anisotropic conductive films for flat-Packed IP does not contain lead chip carrier IP flexible printed panel and the like; conductive paste for the electrical connection of printed circuit boards, for the formation of fingerprints via holes and through holes; electrically conductive paste for inductors, capacitors and resonators, and other ceramic structures; anti-static film for use in LCD, electrochromic devices, electroluminescent devices, solar cells, films, light modulation and optical screens; adhesives for mounting semiconductor elements and light-emitting diodes; film, shielding the leakage magnetic waves, cover and paste for display devices such as CRT (cathode ray tube), LCD (liquid crystal display) and PDP (plasma display); end electrodes for electronic parts such as the electrodes of multilayer ceramic capacitors, multilayer inductors, piezoelectric conductors, resistors and PCB; electrodes and coating compositions for film elements, solar cells, secondary elements and other elements; the jigs for use in the manufacture of semiconductor devices and electronic components; separate drives for the device to produce the image; transmitting conductive tape for adhesion of E. ectronic contacts or electromagnetic screening; tablets digital input transducers in the flow resistance; converters volumetric pressure; flat cables; gaskets; materials of floors, walls and ceilings for clean rooms, sanitary facilities for food and in-hospital measurements; fuel tanks; low-power devices; pulleys; brushes for hair; hoses for organic solvent; coating compositions for welding joints; magnets tape; compounds or adhesives for protective lamination isolated power cables, DC cables and other cables; devices RTS channel (packet); conductive paper; electroconductive non-woven fibers, antistatic gloves; and the like. Electroconductive composition of the present invention is applicable also as a heat-conducting or heat dissipating structure, surface composition, paste, adhesive or layer. In addition, electrically conductive composition of this invention may be an intermediate in the preparation of fibers. Products obtained from these fibers can be used in the form of carpets, mats, layers or materials for interior decoration of vehicles, such as passenger cars, or furniture; conductive plating; filters; drying tape for use in obtaining goods of hygiene, such as diapers and sanitary napkins; with the schiehlen coarse fabric for paper-making machines; and similar.

An electrically conductive composition in the form of flocculent particles according to this invention can be formed with a certain thickness. Conductive composition exhibits excellent electrical conductivity properties, as it is derived from the source material with a specific particle size and the content of potassium oxide special treatment, which gives the substrate material conductivity. In the specific case, when it is loaded into the resin to obtain a primer composition, the primer composition may be applied on the plastic finishing detail to ensure the thickness of the primer layer is about 1-10 microns. In addition, the primer layer can be given a uniform surface resistivity at a level of approximately 104-108Ωsuitable for electrostatic coating. By itself, the electrically conductive composition in the form of flocculent particles of the present invention exhibits desirable characteristics that are not found in conventional conductive materials.

In addition, the conductive composition in the form of flocculent particles of the present invention has a high whiteness and the opacity as its basic material contains titanium acid. Conductive composition when it is embedded in the resin, can give a coating film that not only Prowse the conductive properties, but it also has wonderful high property opacity. Usually, if you want a clear shade, primer should be applied prior to electrostatic coating. In this case, very often the surface of the resin, which had to be covered, had a black color. Accordingly, the primer should be a primer layer, which may give the opacity of the specified black color. In this regard, this material having the properties of whiteness and opacity, which are attributed titanium acid is very useful. Using this primer is more preferable if it is white, because sharp color, such as red, blue or yellow, as well as pale color, such as beige, light blue or pink, can be applied electrostatically. This primer can also be used, if electrostatically applied deep color such as black or silver.

This conductive composition containing a conductive composition in the form of flocculent particles of the present invention typically exhibits a surface conductivity of at a very narrow level of 10-2-1010Ω and shows good electrical conductivity properties. In particular, the composition of this invention containing a binder resin, exhibits a specific surface is e resistance, adjustable arbitrarily without affecting the film-forming properties. Therefore, the conductive composition is easily gives a thin film having a surface resistivity of approximately 104-108Ω and the average thickness of 1-10 microns.

Mainly conductive composition of the present invention provides a high dimensional accuracy in the low shrinkage in the form and provide high mechanical strength.

DESCRIPTION of PREFERRED EXAMPLES

This invention is specifically described below with reference to synthetic examples, examples and comparative examples.

(SYNTHESIS EXAMPLE 1)

27,64 g of potassium carbonate, 4,91 g of lithium carbonate, 69,23 g of titanium dioxide and 74,56 g of potassium chloride were grinded in a dry form and mixed to obtain the source material, which was then caliciviral at 1100°C for 4 hours. After calcination, the obtained sample was immersed in 10 kg of pure water, stirred for 20 hours, separated, washed with water and dried at 110°C. This led to the formation of white powder, which was identified as a layered titanate To0,80Li0,266Ti1,733O4with an average largest diameter of 44 μm and an average thickness of 3 μm.

65 g of the specified K0,80Li0,266Ti1,733O4was dispersively under stirring in 5 kg of 3.5%solenoidality for the exchange of ions and of Li ions with hydrogen ions or hydronium ions. Subsequent separation and washing with water was brought to obtain a layered Titanic acid. It was determined that the remaining number To2In the layered Titanic acid was 2.0 wt%. The percentage of ions exchanged It was 92% and the percentage of exchange of Li ions was 99% or higher. The percentage of ions exchanged For ions and Li, in combination, was 94%. The specified layered Titanic acid was dispersible in 5 kg of water. Then under stirring was added 250 g (11 equivalent %) 1 wt.%-aqueous solution of n-Propylamine. After stirring for about 30 minutes was added in 3.5%hydrochloric acid to establish a pH variance of 2.0. After stirring within one hour, the dispersion was separated by filtration with suction. The obtained wet cake was dispersible in water, washed with water and again separated. This process was repeated three times to achieve sufficient rinsing. The obtained product was dried at 110°15 hours and then was rasmalai mixer to obtain a Titanic acid in the form of flocculent particles. It was found that the powder contains 1.1 wt.% potassium in the form of potassium oxide (K2About), has an average major diameter of 30 μm and an average thickness of 0.3 μm.

(SYNTHESIS EXAMPLE 2)

27,64 g of potassium carbonate, 4,91 g of lithium carbonate, 69,23 g of titanium dioxide and 74,56 g of potassium chloride were grinded in a dry form and mixed to obtain recognize the aqueous material, which then caliciviral at 950°C for 4 hours. After calcination, the obtained sample was immersed in 10 kg of pure water, stirred for 20 hours, separated, washed with water and dried at 110°C. This led to the formation of white powder, which was identified as a layered titanate To0,80Li0,266Ti1,733O4with an average largest diameter of 9 μm and an average thickness of 1 μm.

13 g of the specified K0,80Li0,266Ti1,733O4was dispersively under stirring in 200 kg 1,75%hydrochloric acid for the exchange of ions and of Li ions with hydrogen ions or hydronium ions. Subsequent separation and washing with water was brought to obtain a layered Titanic acid. It was determined that the remaining number To2In the layered Titanic acid was 6.0%per annum. The percentage of ions exchanged It was 76% and the percentage of exchange of Li ions was 99% or higher. The percentage of ions exchanged For ions and Li, in combination, accounted for 82%. The specified layered Titanic acid was dispersible in 600 g of water. Then under stirring was added 250 g (22 equivalent %) of 0.6%aqueous solution of 3-methoxypropylamine. After stirring for about 1 hour was added 100 g of 3.5%hydrochloric acid. After stirring at 60°the dispersion was separated by filtration with suction. The obtained wet cake was dispersible in water, washed with water and again separated. This process was repeated three times to achieve sufficient rinsing. The obtained product was dried at 110°C for 15 hours and then was rasmalai mixer to obtain a powder of titanium acid in the form of flocculent particles. It was found that the powder contains 2.1% of the residual To a2Oh, has an average largest diameter of 6.2 μm and an average thickness of 0.04 μm.

(SYNTHESIS EXAMPLE 3)

27,64 g of potassium carbonate, 4,91 g of lithium carbonate and 69,23 g of titanium dioxide were grinded in a dry form and mixed to obtain the source material, which was then caliciviral at 850°C for 4 hours. The obtained layered titanate was identified as0,80Li0,266Ti1,733O4and after grinding had an average major diameter of 5 μm and an average thickness of 2 μm. 65 g of the specified K0,80Li0,266Ti1,733O4was dispersively under stirring in 5 kg of 3.5%hydrochloric acid and then filtered. The obtained product was washed in 5 kg of 2%hydrochloric acid on a Buechner funnel to obtain a layered Titanic acid, which contain hydrogen ions or hydronium ions instead of ions To ions and Li. Layered Titanic acid and then washed with water, and it was determined that the remaining number To2About it was 0.14%. The percentage of ions exchanged For ions and Li, in combination, accounted for 99.6 percent. The specified layered Titus is a new acid was dispersible in 5 kg of water, to which under stirring was added 250 g (11 equivalent %) 1%aqueous solution of n-Propylamine. After stirring for about 30 minutes was added in 3.5%hydrochloric acid to establish a pH variance of 2.0. After stirring for one hour, the dispersion was separated by filtration with suction. The obtained wet cake was dispersible in water, washed with water and again separated. This process was repeated three times to achieve sufficient rinsing. The obtained product was dried at 110°C for 15 hours and then was rasmalai mixer to obtain a powder of titanium acid in the form of flocculent particles. It was found that the powder consists of a set of very thin layers of titanium acid a thickness of 0.1 μm or less in the form of plates having a size greater than the thickness of the original particles. Their average large diameter and the average thickness was defined as 10 μm and 0.5 μm, respectively.

(SYNTHESIS EXAMPLE 4)

27,64 g of potassium carbonate, 4,91 g of lithium carbonate, 69,23 g of titanium dioxide and 74,56 g of potassium chloride were grinded in a dry form and mixed to obtain the source material. The source material was placed in a double crucible furnace with internal platinum container was heated up to 1200°and then was cooled to 600°With a speed of 4°/h before removing from the oven. After calciner is of the obtained sample was immersed in 10 kg of pure water, was stirred for 20 hours, separated, washed with water and dried at 110°C. This led to the formation of white powder, which was identified as a layered titanate To0,80Li0,266Ti1,733O4with an average largest diameter of 80 μm and an average thickness of 5 μm.

13 g of the specified K0,80Li0,266Ti1,733O4was dispersively with stirring 200 g of 1.75%hydrochloric acid for the exchange of ions and of Li ions with hydrogen ions or hydronium ions and thus gained the layered Titanic acid. After washing with water, the amount remaining To2In the layered Titanic acid was 6.0%per annum. The percentage of ions exchanged It was 76% and the percentage of exchange of Li ions was 99% or higher. The percentage of ions exchanged For ions and Li, in combination, accounted for 82%. The specified layered Titanic acid was dispersible in 600 g of water. Then under stirring was added 250 g (22 equivalent %) of 0.6%aqueous solution of 3-methoxypropylamine. After stirring for about one hour was added in 3.5%hydrochloric acid. After stirring at 60°the dispersion was separated by filtration with suction. The obtained wet cake was dispersible in water, washed with water and again separated. This process was repeated three times to achieve sufficient rinsing. The obtained product was dried at 110°With over 15 hours and then rezmelts the if mixer to obtain a powder of titanium acid in the form of flocculent particles. It was found that the powder contains 4.5% of residual K2Oh, has an average major diameter of 80 μm and an average thickness of 0.7 μm.

(SYNTHESIS EXAMPLE 5)

28,3 g of potassium carbonate, to 11.7 g of magnesium hydroxide, 64 g of titanium dioxide and 75 g of potassium chloride were grinded in a dry form and mixed to obtain the source material, which was then caliciviral at 1150°C for 10 hours. After calcination, the obtained sample was immersed in 10 kg of pure water, stirred for 20 hours, separated, washed with water and dried at 110°C. This led to the formation of a white powder with a mean major diameter of 5 μm and an average thickness of 1 μm.

65 g of the specified K0,80Mg0,40Ti1,60O4was dispersively under stirring in 5 kg of 3.5%hydrochloric acid to exchange ions and of Li ions with hydrogen ions or hydronium ions. This operation was repeated three times. Subsequent separation and washing with water was brought to obtain a layered Titanic acid. It was determined that the remaining number To2O and MgO in a layered Titanic acid was 0.5 and 1.0%,respectively. The percentage of ions exchanged It was 98%, and the percentage of ions exchanged Mg was 92%. The percentage of exchange of ions and Mg ions, in combination, accounted for 96%. The specified layered Titanic acid was dispersible in 5 kg of water. Then under stirring was added 500 g (23 equivalent %) 1%is one solution of n-Propylamine. After stirring for about 30 minutes was added in 3.5%hydrochloric acid to establish a pH variance of 2.0. After stirring for one hour, the dispersion was divided. The wet cake was dispersible in water, washed with water and again separated. This operation was repeated three times to achieve sufficient rinsing. The obtained product was dried at 110°C for 15 hours and then was rasmalai mixer to obtain a powder of titanium acid in the form of flocculent particles. It was found that the powder contains 0.5% residual K2Oh, has an average major diameter of 5 μm and an average thickness of 0.3 μm.

(SYNTHESIS EXAMPLE 6)

28,3 g of potassium carbonate, to 11.7 g of magnesium hydroxide, 64 g of titanium dioxide and 75 g of potassium chloride were grinded in a dry form and mixed to obtain the source material, which was then caliciviral at 1100°C for 3 hours. After calcination, the obtained sample was immersed in 10 kg of pure water, stirred for 20 hours, separated, washed with water and dried at 110°C. This led to the formation of a white powder with a mean major diameter of 23 μm and an average thickness of 3 μm.

65 g of the specified K0,80Mg0,40Ti1,60O4was dispersively under stirring in 5 kg of 3.5%hydrochloric acid to exchange ions and of Li ions with hydrogen ions or hydronium ions. Specified OPE what the situation was repeated three times. Subsequent separation and washing with water was brought to obtain a layered Titanic acid. It was determined that the remaining number To2O and MgO in a layered Titanic acid was 1.2 and 1.0%, respectively. The percentage of ions exchanged To was 95%, and the percentage of ions exchanged Mg was 92%. The percentage of exchange of ions and Mg ions, in combination, accounted for 93%. The specified layered Titanic acid was dispersible in 5 kg of water. Then under stirring was added 500 g (23 equivalent %) 1%aqueous solution of n-Propylamine. After stirring for about 30 minutes was added in 3.5%hydrochloric acid to establish a pH variance of 2.0. After stirring for one hour, the dispersion was divided. The wet cake was dispersible in water, washed with water and again separated. This operation was repeated three times to achieve sufficient rinsing. The obtained product was dried at 110°15 hours and then was rasmalai mixer to obtain a powder of titanium acid in the form of flocculent particles. It was found that the powder contains 1,0% residual To2Oh, has an average major diameter of 20 μm and an average thickness of 0.5 μm.

For each of the layered titanate in synthetic examples 1-6 formula composition, medium, large diameter and the average thickness shown in table 1. In addition, table 1 shows the average large diameter, Rudnaya thickness and the content of potassium, in the form of potassium oxide (K2O), for each Titanic acid in the form of flocculent particles.

Table 1
Synthetic example
231456
Layered titanateFormula compositionK0,80Li0,266Ti1,733O4K0,80Mg0,40Ti1,60O4
Medium large diameter (µm)954480523
The average thickness (μm)123513
Titanic acid in the form of flocculent particlesMedium large diameter (µm)6,2103080520
The average thickness (μm)0,040,50,30,70,30,5
The potassium content (%)2,13,61,14,5,5 1

(EXAMPLES 1-6)

Titanic acid in the form of flocculent particles in each of synthetic examples 1-6, weighing 250 g, were dispersible in 2500 ml of water. The dispersion was stirred with a stirrer for 10 minutes, maintaining at 70°to form a suspension. 130 g (23 wt.% per Sn) aqueous solution of tin tetrachloride and 12.8 g of antimony trichloride were dissolved in 66.6 g of 12 wt.%-Noah hydrochloric acid to obtain a mixed solution. Specified mixed solution was added dropwise to the suspension for about 1 hour. At the same time separately added dropwise 15 wt.%-aqueous sodium hydroxide solution to maintain throughout the reaction the pH of the solution in the range of 1-4. After the first stage reaction, the addition, the reaction solution was stirred for 30 minutes, while not changing the temperature and pH.

Then was added dropwise for about one hour a mixed solution containing 130 g (23 wt.% per Sn) aqueous solution douglasthe tin and 100 g of 12 wt.%-Noah hydrochloric acid. At the same time separately added dropwise 15 wt.%-aqueous solution of sodium hydroxide to maintain the pH of a reaction solution in the range of 1-4 similar to the first stage. After adding dropwise to the 2nd stage of the reaction the resulting solution was stirred for 30 minutes at the same value of the rate is ature and pH and then left to cool to room temperature. Thereafter, the reaction product was filtered, washed with water, obezvozhivani and dried. The dried product was subjected to heat treatment in air, i.e. in an oxidizing atmosphere at a temperature and for a time specified in table 2, to obtain a conductive composition in the form of flocculent particles of the present invention.

Medium large diameters, the average thickness and the content of potassium in the form of potassium oxide (K2O) for electrically conductive compositions in examples 1-6 are identical to the values obtained for the respective starting materials, i.e. samples of Titanic acid in the form of flocculent particles in synthetic examples 1 to 6.

The pH during the addition of tin tetrachloride and antimony trichloride, the pH value adding douglasthe tin, the temperature of the heat treatment and the time period for each of examples 1-6 are shown in table 2.

Table 2
PRPRApp.1PRPRPR
the pH during the addition of tin tetrachloride and antimony trichloride3,12,81,62,0the 3.81,2
pH when adding dujarier the tin 4,83,52,83,0the 3.82,1
The temperature of heat treatment (°)375425400450475500
The time of heat treatment (h)2,00,51,01,52,01,0

Data (transmission electron microscopy) confirm that these conductive compositions in the form of flocculent particles are electrically conductive materials, each of which contains a first conductive layer containing tin oxide and antimony oxide, and the second conductive layer containing tin oxide on the front surface of the titanium oxide as the filler material. The average thickness of the first conductive layer was 10 nm, and the average thickness of the second conductive layer was 8 nm. It was found that the first conductive layer contains 21,0 wt. parts of antimony oxide antimony per 100 wt. parts of tin oxide.

(COMPARATIVE EXAMPLE 1)

Followed the procedure of example 1 except that to obtain granulated electrically conductive composition instead of Titanic acid in the form of flocculent particles obtained in synthetic example 1, using the ovale granular titanium oxide (product name: JR, product Teika Co., Ltd., the average particle diameter of 0.27 μm).

(COMPARATIVE EXAMPLE 2)

The predecessor of the product obtained in synthetic example 1, that is, the layered Titanic acid was removed before its relocation to a more thin layers by the action of amine, dried and illnerova at 500°C for 1 hour to obtain a titanium oxide in the form of flocculent particles (average major diameter of 30 μm, an average thickness of 2 μm and a potassium content of 1.9 wt.% (in the form of potassium oxide(K2O))). Followed the procedure of example 1, except that to obtain a conductive composition in the form of flocculent particles instead of Titanic acid in the form of flocculent particles obtained in example of synthesis 1 were obtained using the described method, the titanium oxide in the form of flocculent particles.

(COMPARATIVE EXAMPLE 3)

Followed the procedure of example 1, except that the fibrous electrically conductive composition instead of Titanic acid in the form of flocculent particles obtained in example of synthesis 1, used fiber titanium oxide (product name: FTL-200, product of Ishihara Sangio Co., Ltd., the average fiber diameter of 0.2 μm and an average fiber length of 3 μm).

(COMPARATIVE EXAMPLE 4)

27,64 g of potassium carbonate, 4,91 g of lithium carbonate, 69,23 g of titanium dioxide and 74,56 g of potassium chloride were grinded in a dry form and mixed for receiving the Oia source material, which then caliciviral at 1100°C for 4 hours. After calcination, the obtained sample was immersed in 10 kg of pure water, stirred for 20 hours, separated, washed with water and dried at 110°C. This led to the formation of white powder, which was identified as a layered titanate To0,80Li0,266Ti1,733O4with an average largest diameter of 44 μm and an average thickness of 3 μm.

65 g of the specified K0,80Li0,266Ti1,733O4was dispersively under stirring in 5 kg of 3.5%hydrochloric acid to exchange ions and of Li ions with hydrogen ions or hydronium ions. Subsequent separation and washing with water was brought to obtain a layered Titanic acid. It was determined that the remaining number To2In the layered Titanic acid was 2.0%. The percentage of ions exchanged It was 92% and the percentage of exchange of Li ions was 99% or higher. The percentage of ions exchanged For ions and Li, in combination, accounted for 94%. The specified layered Titanic acid was dispersible in 5 kg of water. Then under stirring was added 250 g (11 equivalent %) 1%aqueous solution of n-Propylamine. After stirring for about 30 minutes was added in 3.5%hydrochloric acid to bring the pH of the dispersion to 2.0. After stirring for one hour, the dispersion was separated by filtration with suction. The obtained wet cake variance is Aravali in 1H. hydrochloric acid, was heated to 70°and then stirred. The product was dispersible in water, washed with water and again separated. This operation was repeated three times to achieve sufficient rinsing. The obtained product was dried at 110°C for 15 hours and then was rasmalai mixer to obtain a Titanic acid in the form of flocculent particles. It was found that the powder contains 0.2 wt.% potassium in the form of potassium oxide (K2About), has an average major diameter of 0.8 μm and an average thickness of 0.2 μm.

The specific volume resistance ( Ω·cm), medium large diameter (μm) and the average thickness (μm) for electrically conductive compositions obtained in the above examples 1-6 and comparative examples 1-4, and the surface resistance ( Ω) for the respective electrically conductive compositions was determined in accordance with the following methods. The results are shown in table 3.

(1) Specific volume resistance ( Ω·cm)

0.5 g of each sample powder was placed in politically tubular container (outer diameter 28 mm, inner diameter 10 mm and length 30 mm). Two copper rod, each of which had a diameter identical to the size of the inner diameter of the tubular container, and served electrode were inserted into the tubular container from opposite ends for placement on the style of powder between them. Copper rods moved in relation to each other for crushing of sample powder under a pressure of 100 kg/cm2. Measured values of current and voltage between the electrodes (copper bars). The value of resistance R ( Ω) was calculated from measurements. In addition, it was calculated specific volume resistance ρ ( Ω·cm), based on the thickness of the sample during measurement and the electrode area in accordance with the following equation:

the specific volume resistance ρ = resistance Ω × [the area of the electrode (cm2)/thickness of sample (cm)].

(2) Medium large diameter (μm) and the average thickness (μm)

Medium large diameter determined by a laser device to measure the distribution of diffraction particle size. The average thickness of the sample was determined using either electronic scanning microscope (SEM) with an increase of 1000-10000, or transmission electron microscope (TEM) with increasing 10000-1000000 with successive reading scales for actual values.

Conductive polymer compositions of the present invention and comparative polymer compositions were obtained according to the following procedure. Each of the conductive structures in the form of flocculent particles obtained in examples 1 to 6 were added to the acrylic binder (product name: Acrose FS Super Clear, the content of the solid matter 40%, the product of Dai Nippon Toryo Co., Ltd.) in the amount of 30 wt.% in the calculation of the solid material and then mixed under stirring, thus obtaining conductive composition.

Used the above procedure, except that instead of the electrically conductive compositions of examples 1-6 to obtain comparative compositions used conductive compositions of comparative examples 1-4.

Each of the above electrically conductive compositions of the present invention and comparative conductive compositions was applied on a PET film with a thickness of 50 μm to ensure it dry film thickness of 5 μm and then dried. The value of surface resistance ( Ω) the obtained coated film was measured using a measuring device (product name: Hiresta IP, for high-impedance 104-1012Ωand the product name: Lowresta GP, for a low resistance 10-5-107Ωboth produced by Mitsubishi Chem. Corp.). The results are shown in table 3.

In addition, the conductive polymer compositions of the present invention and comparative polymer compositions were obtained according to the following procedure. Each of the conductive structures in the form of flocculent particles of examples 1-6 were introduced in the 6,6-nylon (product name Zytel, a product of Du Pont) in an amount of 30 wt.% and then was mixed to obtain t is bleak conductive composition of the present invention.

Used the above procedure, except that instead of the electrically conductive compositions of examples 1-6 to obtain tablets of comparative compositions used conductive compositions of comparative examples 1-4.

Using the above tablets conductive compositions of the present invention and comparative conductive compositions, size (Mf) of each of the molded product 24 hours after molding and size (Mw) of the mold was measured according to the method DIN 16901 and then calculate the shrinkage factor (%) according to the following equation. The results are shown in table 3.

The shrinkage during molding (%) = (Mw - Mf)/Mw × 100.

From the point of view of anisotropy during molding, each value shown in the table were obtained by dividing the difference between the values measured in the flow direction during molding of the polymer and in the transverse direction, at 2.

Table 3
PRPRApp.1PRPRPR
The shape of the particlesCerealCerealCerealCerealCerealCereal
Medium large diameter (µm) 6,2103080520
The average thickness (μm)0,040,50,30,70,30,5
The specific volume resistance ( Ω·cm)8×1021×1028×1019×1017×1016×101
Surface resistance ( Ω)7×1068×1065×1066×1069×1067×106
The shrinkage during molding0,20,20,20,20,20,2

Compare. example 1Compare. example 2Compare. example 3Compare. example 4
The shape of the particlesGranulesCerealCerealCereal
Medium large diameter (µm)0,330300,8
The average thickness (μm)03 20,30,2
The specific volume resistance ( Ω·cm)1 × 1022 × 1022 × 1025 × 103
Surface resistance ( Ω)More than 10126 × 1092 × 1010More than 1013
The shrinkage during molding0,20,21,00,2

From table 3 it is clear that polymer composition containing each of the electrically conductive compositions in the form of flocculent particles of the present invention, even if it is formed in a very thin film, such as measuring 5 μm, exhibits good surface resistance. In contrast, it is clear that the film thickness of 5 μm formed from the electrically conductive compositions of comparative examples 1-4, shows a very low value of the surface resistance, which indicates the difficulty of forming thin film.

1. An electrically conductive composition in the form of flocculent particles, characterized in that it contains titanium oxide with an average value of the large diameter of 1-100 μm and an average thickness of 0.01 to 1.5 μm and a content of 0.3 to 5 wt.% potassium in the form of potassium oxide (K2About),the first conductive layer, including tin oxide containing antimony, and deposited on the surface of titanium oxide, and the second conductive layer comprising tin oxide and deposited on the first conductive layer.

2. An electrically conductive composition in the form of flocculent particles according to claim 1, in which the first conductive layer contains 0.1 to 50 parts by weight of antimonic component in the form of antimony oxide (Sb2About3) per 100 parts by weight of a tin component in the form of tin oxide (SnO2).

3. An electrically conductive composition in the form of flocculent particles according to claim 1 or 2, characterized in that it can be obtained by the action of the connection of the main character, has the effect of causing swelling of the intermediate layers, the layered Titanic acid to delamination when this layered Titanic acid with the formation of flakes of titanium acid, introducing the compound of tetravalent tin for education specified first conductive layer on the titanium acid in the form of flocculent particles, the introduction of compounds of divalent tin for education specified second conductive layer on the first conductive layer and heat treatment of this combination.

4. Conductive composition containing a binder and an electrically conductive composition in the form of flocculent particles according to any one of claims 1 to 3.

5. Electroconductive composition according to claim 4, the tives such as those it contains 100 wt. parts binder and 5-50 parts by weight of the conductive composition in the form of flocculent particles according to any one of claims 1 to 3.

6. Electroconductive composition according to claim 4 or 5, in which the specified binder may be one or more types selected from thermoplastic resins, thermosetting resins, inorganic fillers, and metal-containing organic compounds.



 

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4 cl, 1 dwg, 1 tbl, 2 ex

FIELD: electrical engineering; electricity-conductive compound in the form of flocculent particles.

SUBSTANCE: proposed compound has titanium oxide with mean large diameter of 1 to 100 μm and mean thickness of 0.01 to 1.5 μm, potassium in amount of 0.03 to 5 mass percent in the form of potassium oxide (K2O), as well as first electricity-conductive layer which is formed on surface and has in its composition tin oxide and antimony, and second electricity-conductive layer which is formed on first electricity-conductive layer and has in its composition tin oxide. Proposed electricity-conductive composition in the form of flocculent particles is capable of imparting good electricity-conductive properties even when formed in layer of 1 to 10 μm in thickness.

EFFECT: improved properties of electricity-conductive composition.

6 cl 3 tbl, 6 ex

FIELD: weapons and ammunition.

SUBSTANCE: method includes formation of phosphate layer used as ground, application of a polymer layer by means of the case treatment in an aqueous solution of a polymer composition and thermal treatment of the polymer coating. After the phosphate layer formation it is passivated in the aqueous solution of a passivating-stabilising additive with concentration of 10-15 g per litre of a working solution. The polymer layer is applied by means of the case treatment in the aqueous solution of a mix that contains 180-220 g of the polymer composition CKN-26 and 7-10 g of the passivating-stabilising additive with concentrations per litre of the working solution with provision of the pH values index for the whole working solution equal to 8.5-9.5. A mixture of the following solutions, wt %, is used as a passivating-stabilising additive: 1.8-2% solution of 2-mercaptobenzothiazole, dissolved in 12-15% aqueous solution of potassium carbonate or sodium carbonate - 90-93.5, 15% aqueous solution of the mixture of sodium hexametaphosphate and trisodium phosphate dihydrate salts taken at the ratio of 1:(1-2) - 6.5-10.

EFFECT: increased corrosion resistance of steel cartridge cases with polymer coating as a result of high stability of formed polymer coating.

6 cl, 1 ex

FIELD: machine building.

SUBSTANCE: proposed system (1) comprises first main side (2) to be located on boundary with structural part to be protected (30) and second main side (3) to be located on boundary with high-temperature ambient medium (4). System (1) has sections (5, 6) with different heat expansion factors. System first section (5) adjoining structural part to be protected (30) has first thermal expansion factor complying with that of structural part (30). At least, one second section (6) of system (1) has second, lower thermal expansion factor. System (1) is made up of joint between first ceramic heat insulation layer (8) facing aforesaid structural part, and second ceramic layer (9) facing high-temperature ambient medium (4). Note here that first and second protective layers (8, 9) are jointed together by plasma evaporation. System (1) consists of one of the following combinations of materials: 7YSZ/La2Hf2O7; 7YSZ/BaZrO3; 7YSZ/LaYbO3, where first value stands for material of first heat insulation layer (8), while second value designates material of second layer (9). Note also that 7YSZ is zirconium oxide stabilised by 7 wt % of yttrium oxide.

EFFECT: higher durability for gas turbine operation loads.

5 cl, 2 dwg

FIELD: machine-building industry.

SUBSTANCE: tool is cleaned and degreased and then treated with a solution of high-molecular fluoride containing compositions with temperature being maintained when tool is rotated at 12000 rev/min and/or treated ultrasonically at frequency not bringing the solution to cavitations. The nano-structured hardening coating TiCr-TiCrN-TiN is then applied from separated plasma.

EFFECT: increased wear resistance and effectiveness of cutting tool operation due to improved coating adhesion with tool surface and reduced number of micro and macro- defects at cutting edges.

6 tbl

FIELD: metallurgy.

SUBSTANCE: when processing especially hard materials, such as tempered instrumental steel, with hardness of more than 50, preferably 55 HRC, a blank is used with a wear-resistant multi-layer coating. The coating includes at least the first bearing layer from a material with the following composition: (TiaAl1-a)N1-x-yCxOy, in which 0.4<a<0.6, and 0<x and y<0.3, or (AlbCr1-b)N1-x-yCxOy, in which 0.5<b<0.7, and 0<x and y<0.3, and the second nanocrystalline layer of a material with the following composition: (Al1-c-d-eCrcSidMe)N1-x-yCxOy, where M stands for at least one element from transition metals of groups 4, 5, 6 of the periodical system, apart from chrome, and 0.2<c<0.35, 0<d<0.20, 0<e<0.04.

EFFECT: improved process characteristics of materials, mechanical processing of which is difficult.

24 cl, 7 tbl, 8 ex

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