SU789451A1 - Method of producing coating on support - Google Patents

Description

METHOD OF OBTAINING COATINGS ON A SUBSTRATE

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one

The invention relates to methods for producing oxide and sulphide coatings on solid substrates that are widely used in optical instrumentation, in the chemical and glass industries, in construction business in the manufacture of sunscreens and decorative coatings.

A known method of producing oxide 10 coatings from an aqueous solution of metal acetates, according to which a solution of cobalt acetate is boiled at 100-105 ° C for 5-6 hours before and filtered, then applied to the substrate 1. 15

As is closer to the technical essence and the achieved result, the proposed method is to obtain an oxide coating on a substrate. Mainly from glass, by heating and applying a film-forming substance from a solution of metal acetylacetonate in an aprotic solvent 2.

However, these methods are quite complex, since they are based on the phenomenon of hydrolysis of metal acetates to form colloidal solutions, which are rather unstable in time and can be 30

coagulate under the influence of various factors (mechanical stress, temperature change, the presence of impurities). Filtration of such solutions is a long and laborious process, and the presence of acid formed during the film formation process significantly complicates the process and limits the range of materials on which these coatings can be applied.

The purpose of the invention is to simplify the process of obtaining coatings on a substrate.

This goal is achieved by the fact that in a process for producing coatings on a substrate, mainly glass, by heat treatment and film coating of a substance from a solution of a metal-containing compound in an organic solvent, the film-forming substance is applied from a solution containing additionally nitrogen, oxygen or sulfur containing an organic complexing agent, and metal oxide is used as the metal-containing compounds.

It is advisable to use monoethanolamine, diethanolamine, triethanolamine as a nitrogen-containing organic complexing agent.

ethylenediamine, dimethylglyoxime, 8-hydroxyquinoline, 2,2-dipyridyl, 1,10-phenanthroline, an oxygen-containing organic compound — acetylacetone, benzoyl acetone, acetoacetic ester, catechol, a sulfur-containing organic compound — dithizone, thiourea and its derivatives.

When this occurs, the complexation reaction between the metal oxide and the organic matter occurs. The complex that is formed as a result of the complexation reaction is converted into a solution using an organic solvent. At the same time, the necessary condition is met, the initial ligand (organic matter) and the resulting complex are soluble in the selected organic solvent. Among the organic solvents, both aprotic solvents, such as acetonitrile, benzonitrile, hexamethylphosphoric triamide, dimethyl sulphoxide / dimethylformamide, formamide propylene carbonate, and proton donor, such as fatty alcohols, are taken.

The process of preparing solutions depends on the rate of dissolution of the corresponding oxides. To intensify the process, it is recommended to heat the reaction mixtures. Under normal conditions, the reaction mixture cannot be heated above, the boiling point of the corresponding solvent. In addition, some solvents, for example, formamide, dimethyl sulfoxide, hexamethylphosphoric triamide, can partially decompose when heated to boiling, therefore the optimum temperature range is 5-130 ° C.

The amount of dissolved oxide increases with increasing concentration of organic matter. The optimum concentration of organic matter in this method is. ten%, .

For the preparation of solutions, it is desirable to take freshly prepared oxides. The dissolution of the oxides is carried out in a 250 mp reactor equipped with a stirrer and reflux condenser. 0.1 g of the corresponding metal oxide is added to a 10% solution of organic matter in an organic solvent. The mixture is heated with constant stirring until the oxide is completely dissolved.

Example. Cobalt ii3 sulphide ii3 solution of 0.1 g co-oxide was sprayed onto the glass substrate. Balta in 100 ml of 10% rayvor thiourea in formamide. The mixture is heated for 3 hours at 110 ° C, with constant stirring. The resulting solution has a purple color. The cobalt oxide concentration is 1 g / l. The substrate temperature during spraying is 200-240 ° C.

Example 2. 0.1 g of zinc oxide is dissolved in 100 ml of a 10% solution of acetylacetone in dimethylformamide at 110-120 seconds. Complete dissolution occurs after 2 hours. Concentration. solution of 1 g / l. This solution is sprayed onto a quartz substrate. The substrate temperature during spraying is 190-2.2 ° C. The result is a transparent coating of zinc oxide with a specific resistance of 40 com / o.

Example 3. In 100 ml of a 10% solution of ethylene diamine in ethyl alcohol, 0.1 g of nickel oxide is introduced. . The mixture was boiled for 8 hours. The resulting solution, having a blue color, was applied to a 2000 cm ssall substrate.

All prepared solutions are stable under normal conditions indefinitely. The introduction of electrolytes does not have a noticeable effect. During thermal decomposition, the resulting solutions can again release the dissolved oxide. Moreover, the solutions obtained using sulfur-containing compounds are isolated by spraying onto the substrate the corresponding sulfide.

Using a spraying device, the solutions obtained in this way are applied to heated substrates (glass, glass, silicon, aluminum, and other metals). At the same time, the formation of oxide and sulfide coatings was detected on the surface of the substrates using chemical and X-ray analyzes.

The use of the proposed method as compared with the known ones allows one to expand the range of oxide coatings obtained, as well as to obtain sulfide coatings. In addition, the resulting solutions have a much greater stability. The method is simple and versatile.

Claims (4)

1. A method of producing coatings on a substrate, mainly glass, by heat treatment and applying a film-forming substance from a solution of a metal-containing compound in an organic solvent, characterized in that, in order to simplify the process, the application of a film-forming substance is carried out from a solution containing additionally nitrogen -, - an oxygen- or sulfur-containing organic complexing agent; and a metal oxide is used as the metal-containing compound. 2. A method according to claim 1, characterized in that monoethanol, iH, diethanolamine, triethanolamine, i-ethylenediamine, dimethylglyoxime, 2,2-dipyridyl, 1,10-phenanthrolium, 8-hydroxyquinoline are used as the nitrogen-containing organic complex. 3. The method according to claim 1, with the tl and h ayusch and the fact that as the oxygen-containing organic complexing agent use acetylacetone, benoyloacetone, acetoacetic acid, pyrocatechin. 4. The method according to claim 1, which is based on the fact that dithizone, thiourea and its derivatives are used as the sulfur-containing organic complexing agent. information sources,. taken into account in the examination 1. Author's certificate of the USSR 161877, cl. From 03 to 17/10, 1963. 2. The patent of the USSR No. 608465, cl. From 03 to 17/00, 1972.