Method of producing high-porous coating on basis of double silicon and nickel oxides

FIELD: process engineering.

SUBSTANCE: invention relates to production of thin-film materials base on system of double oxides used fast developing areas of electronic lighting engineering, etc, as sensitive, decorative, filtering and distributing coatings, etc. Proposed method comprises preparing film forming solution and applying it on article surface. Fresh film forming solution is kept for 8-13 days at 6-8°C, drying is performed at 60°C for 30-40 min and nonlinear heating to 800-900°C in air and curing at 800-900°C for one hour and cooled in conditions of natural cooling down of muffle furnace at the following ratio of components in film forming solutions in wt %: tetraethoxysilane - 22.6-21.4; hydrochloric acid - 4.4-10-4-1.2-10-4, distilled water - 2.3-0; metal salt - NiCl2-6H2O 1.1- 8.4; ethanol - (98 wt %) making the rest.

EFFECT: simplified production of uniform coating with perfected properties.

2 ex, 1 dwg

 

The invention relates to the technology of thin-film materials based on systems of double oxides used in the rapidly developing fields of electronics and lighting industry, the production of materials of catalysts, as functionally sensitive, decorative, filter, and distributes radiation coatings.

A method of obtaining bactericidal oxide coating (Patent RF №2395548, C09D 5/14 publ. 27.07.2010), comprising preparing an acidic film-forming solution (ERP), application of a film on the surface of the solid inorganic material, drying the coated material, heat treatment at temperatures above the temperature of decomposition of metal salts, but below the melting temperature or softening of a solid inorganic material. The disadvantages of this method are the special selection of solvents to avoid runoff of the applied layer on the substrate, a thorough cleaning is used for the comminution of air or gas, the need to maintain a certain size and shape of the jet of sprayed solution, as well as sophisticated equipment. In addition, in the described method of producing films for improving the wettability of the surface of the coated material use organic additives, and as the binder components - metal oxides: Rennie, iron, titanium, lanthanum, which greatly complicates the composition of the synthesized materials and affects the properties of the obtained films. To achieve the desired pH of the film-forming solution in this way use of acid treatment of natural or synthetic oxides or carbonates of magnesium, calcium or zinc, which does not allow to precisely control the content of acid in the solution and technologically complicates the process.

A method of obtaining gas sensitive material of the film-forming solution (Patent RF №2310833, G01N 27/12, 20.11.2007,), comprising preparing a reaction solution using tetraethoxysilane and nitrate of silver, the coating film by centrifuging, drying the samples and heat treated at 370-750°C. the Disadvantages of this method are the absence of PORES of controlled amounts of water and acid involved in the processes of hydrolysis of tetraethoxysilane and significantly reduces the time of ripening solutions, as well as the absence of alcohol, promoting uniform distribution of components in the solution and the free diffusion of ions and molecules in the volume.

Known method of preparing the film-forming solutions used to obtain thin-film coatings (Hernandez-Torres J. Optical properties of sol-gel SiO2films containing nickel / J. Hernandez-Torres, Mendoza-Galvan // Thin Solid Films. - 2005. - V.472. - P.130-35.), selected as a prototype. The method includes preparing THEN for obtaining films of SiO2-NiO-based tetraethoxysilane, ethanol, water with a molar ratio of the components: tetraethoxysilane/alcohol/water=1/4/11 .7. The number setevogo of Nickel nitrate was varied to obtain films with the atomic ratio Si/Ni: 1.2; 3.1; 7.1. Films were obtained on glass and quartz substrates by the method of extrusion rate of 20 cm/min, All samples were dried in air at 180°C for 30 minutes. Subsequent heat treatment was carried out at 300 and 500°C for 30 minutes.

The disadvantages of this method are:

1. the absence in the film-forming solution of the acid, which is the catalyst for hydrolysis and condensation of tetraethoxysilane, which affects the time of maturation of the solutions and on the porosity of the films;

2. not focusing on the degree of ksusenosti ethanol, which is an important parameter influencing the rheological properties of solutions;

3. upon receipt of the films by the method of extrusion, it is difficult to obtain a uniform coating thickness, which is connected with the rheological characteristics of film-forming solutions - solutions with higher values of concentration and viscosity can be progressively enriched with dissolved substance in the zone of immersion, leading to the fact that the thickness of the coating is increased from top to bottom when removing the sample, and with features of fixing the substrate inclination angle of the coated surface to the fluid level should be equal to 90°.

The present invention is to develop a simpler method of obtaining a uniform thickness of high-porous coating with the purpose of obtaining a developed surface, higher values of reflectance (90-110%) in the visible wavelength range and transmittance of near ultraviolet radiation (60-90%) with a simultaneous combination of low values of refractive index (1,35-1,43) and thickness (156-344 nm)that will allow you to use them as a redistributive radiation coatings.

The problem is solved in that a method of obtaining a highly porous coating includes preparation of film-forming solution and then applying it on the surface of the products by drying, annealing and cooling, but unlike the prototype of the freshly prepared film-forming solution was incubated for 8-13 days at a temperature of 6-8°C, drying is carried out at a temperature of 60°C for 30-40 minutes, with subsequent nonlinear heating to 800-900°C in an atmosphere of air in the first 15-20 minutes the heating rate and maximum is 22°C/min, in the next 17 minutes, the heating rate is maintained at a level of 18°C/min, then within 12 minutes, the heating rate is 12°C/min, the last 0-20 minutes of heating, the heating rate is maintained at 0.5°C/min - and exposure at 800-900°C for 1 hour, the gradual cooling natural cooling muffle furnace. To obtain a highly porous coating used film-forming solutions were prepared in the following ratio of components, wt.%:

the tetraethoxysilane 22,6-21,4;

hydrochloric acid 4,4·10-4to 1.2·10-4;

distilled water 2,3-0;

salt of the metal NiCl2·6H2O 1,1-8,4;

ethyl alcohol (98%) - the rest.

The presence of a large square section of the phase due to the formation of pores in the films can significantly change their properties by modification of the microstructure, and by various alloying elements and then fill in other formulations, which allows you to manage the target functional-sensitive properties, which are closely related with technological parameters of synthesis.

The processes of hydrolysis of tetraethoxysilane (TEOS), ectothermic. When creating favorable conditions for heat removal from the system can be controlled processes stitching siloxanes products of the hydrolysis of TEOS in the first minutes of ripening solutions, thereby predetermining the structure and properties of the synthesized films.

Add in THEN salt of d-metal leads to increased ionic strength of the solution that helps to change the solvate shell of reactive fragments and reduce e is ergie the reorganization of the environment, and, consequently, to the decrease in the activation energy of the ongoing processes. The hydrolysis rate of TEOS in such systems depends on the lability of aquacomplexes metals and their sustainability.

During the first days of ripening solution, active process of hydrolysis and condensation Angelov V. of tetraethoxysilane, which appear associated molecular unit of education with increasing size. On the second and third steps of the hydrolysis of TEOS in the film-forming solutions containing metal salts, is much faster, due to steric factor, symmetry violation molecules Angelov V. tetraeder and participation of complexes of metals in the process of substitution of ethoxy-groups in the group-HE.

As a result, a solution containing Nickel ions(II), after 10 minutes of ripening contains a high concentration of di - and trihydroxypropane of tetraethoxysilane, which contributes not only to increasing concentrations of the respective products of condensation and crosslinking of siloxane chains, leading to the early formation of the reticulated structure of the growing polymer to increase the viscosity of the solution and the concentration of free water.

Maturation of film-forming solutions at t is mperature 6-8°C increases the degree of hydrolysis of tetraethoxysilane, leading to the early formation of the reticulated structure of the growing polymer matrix. High speed heating the coatings in the first few minutes of annealing leads to the formation of pores due to boiling water, uniformly distributed in the film. Valence and deformation vibrations of links H-O-N recorded in the IR spectra of the films up to 300°C. a Gradual decrease in the rate of heat promotes deep processes of oxidation of hydroxy-clorides metals and processes of formation of oxides.

Keeping the film at a temperature of 800-900°C for one hour leads to the completion of the processes and increase the degree of crystallinity of samples. Uniform cooling contributes to the formation of a stable film structures.

The result is a porous coating (figure 1) are characterized by high values of reflectance (90-110%) in the visible wavelength range and transmittance of near ultraviolet radiation (60-90%) with a simultaneous combination of low values of refractive index (1,35-1,43) and thickness (156-344 nm). The porosity of the films is 22-40%, a pore size from 85 nm to 1.1 μm.

Example 1.

To prepare 100 ml of a film-forming solution must be connected to 1.9 ml of distilled water (2.3 wt.%), 0.06 ml of hydrochloric acid with a concentration of 2 mol/l (4,4·10 -4wt.%), 0,89 g of salt NiCl2·6H2O (1.1 wt.%) and to bring to a volume of 80 ml of ethyl alcohol (98%). The resulting homogeneous solution was cooled to 6-8°C. At the final stage of cooking, THEN pour in the prepared solution pre-cooled to 6-8°C tetraethoxysilane volume of 20 ml (22.6 wt.%). After ripening solution for 8 days at a temperature of 6-8°C THEN applied on a silicon or quartz substrate by centrifuging and subjected to a stepwise heat treatment: at 60°C for 30-40 minutes, followed by non-linear heating up to 800°C in an atmosphere of air in the first 15 minutes of heating rate and maximum is 22°C/min, in the next 17 minutes, the heating rate is maintained at a level of 18°C/min, then within 12 minutes, the heating rate is 12°C/min, the last 40 minutes of heating, the heating rate is maintained at the 0.5°C/min and holding at 800°C for 1 hour, the gradual cooling natural cooling muffle furnace. The resulting thin-film coating composition 5 wt.% NiO, 95 wt.% SiO2the thickness of 156 nm and a refractive index of 1.43. The porosity of the film 22%, a pore size from 185 nm to 1 μm.

Example 2.

To prepare 100 ml of a film-forming solution it is necessary to connect 0.06 ml of hydrochloric acid with a concentration of 2 mol/l (1.2 x 10-4mass%), 7,28 g of salt NiCl2·6H2O (8.4 wt.%) and to bring to a volume of 80 ml of ethyl alcohol (98%). The resulting homogeneous solution was cooled to 6-8°C. At the final stage of cooking, THEN pour in the prepared solution pre-cooled to 6-8°C tetraethoxysilane volume of 20 ml (21.4 wt.%). After ripening solution for 13 days at a temperature of 6-8°C THEN applied on a silicon or quartz substrate by centrifuging and subjected to a stepwise heat treatment: at 60°C for 30-40 minutes, followed by non-linear heating up to 900°C in an atmosphere of air in the first 20 minutes the heating rate and maximum is 22°C/min, in the next 17 minutes, the heating rate is maintained at a level of 18°C/min, then within 12 minutes, the heating rate is 12°C/min, the last 20 minutes of heating, the heating rate is maintained at the 0.5°C/min and holding at 900°C for 1 hour, the gradual cooling natural cooling muffle furnace. The resulting thin-film coating composition 30 wt.% NiO, 70 wt.% SiO2the thickness of 344 nm and a refractive index of 1.35. The porosity of the film is 40%, the pore size of from 85 nm to 1.1 μm.

Unlike the prototype, the described method is the control of processes of hydrolysis and condensation of tetraethoxysilane in the film-forming solution by introducing neo the required amount of acid and distilled water, that allows you to expand the time domain fitness-forming solutions for the deposition of uniform coatings. Appropriate synthesis conditions allow you to control the surface morphology. In addition, the films are applied in a simple way.

The coatings obtained using the described method, are characterized by highly developed porous structure, high values of reflectance in the visible range of the spectrum and transmittance of near-ultraviolet radiation with a combination of low values of refractive index and thickness, which opens up the possibility of using films in the production of materials of catalysts, as functionally sensitive, decorative, filter, and distributes radiation coatings. Figure 1 shows micrographs of the films of SiO2-With NiO NiO content 30 wt.%.

The method of obtaining highly porous coating comprising preparing a film-forming solution and then applying it on the surface of the products, drying, annealing and cooling, characterized in that the freshly prepared film-forming solution was incubated for 8-13 days at a temperature of 6-8°C, drying is carried out at a temperature of 60°C for 30-40 min, with subsequent nonlinear heating to 800-900°C in an atmosphere of air in the first 15-20 min speed is of AREVA and maximum is 22°C/min, in the following 17 min heating rate is maintained at a level of 18°C/min, then for 12 min heating rate is 12°C/min, 40-20 last min heating rate is maintained at 0.5°C/min and holding at 800-900°C for 1 h, the gradual cooling natural cooling muffle furnace at the following ratio of components in the film-forming solution, wt.%:

the tetraethoxysilane22,6-21,4
hydrochloric acidof 4.4·10-4to 1.2·10-4
distilled water2,3-0
salt of the metal NiCl2·6H2O1,1-8,4
ethyl alcohol (98%)rest



 

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