CN113737171A - Preparation method of porous tantalum film - Google Patents
Preparation method of porous tantalum film Download PDFInfo
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- CN113737171A CN113737171A CN202111059233.5A CN202111059233A CN113737171A CN 113737171 A CN113737171 A CN 113737171A CN 202111059233 A CN202111059233 A CN 202111059233A CN 113737171 A CN113737171 A CN 113737171A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
- C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/087—Coating with metal alloys or metal elements only
Abstract
The invention discloses a preparation method of a porous tantalum film, which comprises the following steps: firstly, adding tantalum powder into a polyvinyl butyral solution to obtain tantalum powder slurry; polishing the tantalum substrate, and then cleaning with deionized water to obtain the cleaned tantalum substrate; thirdly, carrying out chemical polishing treatment on the cleaned tantalum substrate to obtain a polished tantalum substrate; fourthly, spraying the tantalum powder slurry on the surface of the polished tantalum substrate to obtain a tantalum film green body material; and fifthly, sintering the green tantalum film material in vacuum to obtain the porous tantalum film on the surface of the tantalum substrate. According to the invention, the tantalum powder slurry is sprayed on the surface of the tantalum substrate and then sintered, and the monodisperse porous tantalum film is obtained on the surface of the tantalum substrate by regulating the slurry concentration and the spraying pressure, so that the surface area of the tantalum substrate is effectively increased, the application of the tantalum substrate in different fields is promoted, and the application environment of tantalum metal is expanded.
Description
Technical Field
The invention belongs to the technical field of refractory metal porous membranes, and particularly relates to a preparation method of a porous tantalum membrane.
Background
The tantalum has the characteristics of high melting point, good corrosion resistance and the like, so that the tantalum has a very wide application field. In chemical, electronic, electrical and other industries, tantalum can replace many tasks that need to be undertaken by precious metal materials, resulting in significant reductions in material costs for the relevant industries. The capacitor equipment prepared by using the tantalum has very obvious advantages and is mainly applied to military equipment. Statistically, half of the world's tantalum metal production is used in tantalum capacitor production.
With the continuous progress of material science, tantalum is gradually applied to different fields, such as the field of bioimplants, hydrogen separation and purification and the like. In addition, with the continuous progress of powder preparation technology, spherical ultrafine tantalum powder with narrow particle size distribution can be obtained in the market at present, and a material foundation is laid for the preparation of the ultrathin porous tantalum film.
Therefore, a method for preparing a tantalum film with a high specific surface area and a porous structure is needed.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing a porous tantalum film, aiming at the defects of the prior art. According to the method, the tantalum powder slurry is sprayed on the surface of the tantalum substrate and then sintered, so that a monodisperse porous tantalum film is obtained on the surface of the tantalum substrate, the surface area of the tantalum substrate is effectively increased, the application of the tantalum substrate in different fields is promoted, and the application environment of tantalum metal is expanded.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for preparing a porous tantalum film, comprising the steps of:
step one, adding tantalum powder into a polyvinyl butyral solution to obtain tantalum powder slurry; the solid content of the tantalum powder slurry is 45-65%;
polishing the tantalum substrate, and then cleaning with deionized water to obtain the cleaned tantalum substrate;
step three, carrying out chemical polishing treatment on the cleaned tantalum substrate obtained in the step two to obtain a polished tantalum substrate;
step four, spraying the tantalum powder slurry obtained in the step one on the surface of the polished tantalum substrate obtained in the step three to obtain a tantalum film green body material;
and step five, performing vacuum sintering on the green body material of the tantalum film obtained in the step four to obtain the porous tantalum film on the surface of the tantalum substrate.
The invention can obtain even tantalum powder slurry by dispersing tantalum powder by polyvinyl butyral solution, the tantalum powder slurry has better stability and fluidity, is suitable for obtaining a tantalum film by adopting a spraying process, ensures that the obtained tantalum powder layer is formed by a single-layer tantalum powder layer by controlling the concentration of the slurry, obtains a bright and flat surface by polishing a tantalum substrate and removing oxide skin after chemical polishing, exposes more tantalum atoms, improves the sintering activity of the tantalum powder and the tantalum substrate to form good metallurgical bonding, realizes the single-layer distribution of the tantalum powder by spraying the tantalum powder slurry on the surface of the polished tantalum substrate and spraying a layer of tantalum powder slurry on the surface of the tantalum substrate, preliminarily obtains even green materials of the tantalum film, and realizes the vacuum sintering of the green materials of the tantalum film under the action of high temperature, and forming metallurgical bonding between the tantalum powder and a tantalum substrate of the substrate by diffusion, and generating particle bonding between the powders to form the metallurgical bonding, thereby obtaining a porous tantalum film distributed in a single layer on the surface of the tantalum substrate.
The preparation method of the porous tantalum film is characterized in that in the step one, the tantalum powder is spherical tantalum powder, and D90 of the spherical tantalum powder is not more than 5.6 microns. The method ensures that the prepared tantalum film has a porous structure by controlling the shape of the tantalum powder, wherein D90 is used for representing that the cumulative particle size distribution is 90%, and the particle size of the spherical tantalum powder is ensured to be at a smaller level by controlling the D90 of the spherical tantalum powder to be not more than 5.6 microns, so that the prepared porous tantalum film has the ultrathin characteristic.
The preparation method of the porous tantalum film is characterized in that in the step one, the solvent of the polyvinyl butyral solution is absolute ethyl alcohol, and the mass content of the polyvinyl butyral in the polyvinyl butyral solution is 1% -3%. The invention ensures that the polyvinyl butyral is uniformly dispersed in the absolute ethanol by preparing the polyvinyl butyral and the absolute ethanol into the solution, thereby uniformly dispersing the tantalum powder in the polyvinyl butyral solution, and preventing the polyvinyl butyral from influencing the subsequent reaction while promoting the uniform dispersion of the tantalum powder by controlling the content of the polyvinyl butyral in the polyvinyl butyral solution to be at a lower level
The preparation method of the porous tantalum film is characterized in that in the second step, the polishing treatment is sequentially performed by using 280#, 600#, 1000# sand paper, and the tantalum substrate is a tantalum sheet. According to the method, the rough-to-fine sand paper is used for polishing, so that a bright and flat surface is obtained while oxide skin is removed, more tantalum atoms are exposed, the sintering activity of tantalum powder and a tantalum matrix is improved, the quality of the prepared porous tantalum film is ensured, and the tantalum sheet is used as the tantalum matrix and has the advantage of easiness in treatment.
The preparation method of the porous tantalum film is characterized in that the chemical polishing treatment process in the step three is as follows: soaking the tantalum substrate in a hydrofluoric acid solution containing 1-3% of ammonium sulfate by mass for 20-40 min, taking out, immediately washing the tantalum substrate with deionized water, and drying the tantalum substrate with nitrogen to obtain a polished tantalum substrate; the hydrofluoric acid solution is an aqueous solution containing hydrofluoric acid with the mass fraction of 40%. According to the method, the hydrofluoric acid solution containing ammonium sulfate is adopted to effectively remove the oxide film on the surface of the tantalum substrate, a smooth surface can be obtained, and the oxide film is properly removed by controlling the soaking time, the ammonium sulfate content and the hydrofluoric acid content.
The preparation method of the porous tantalum film is characterized in that the spraying pressure in the spraying in the fourth step is 0.45 MPa-0.60 MPa. The invention controls the spraying pressure and regulates the spraying speed of the slurry to obtain uniform tantalum film green materials, thereby realizing the single-layer distribution of tantalum powder.
The preparation method of the porous tantalum film is characterized in that the sintering process in the fifth step is as follows: in a high-temperature vacuum furnace, the vacuum degree is 3.0 multiplied by 10-3Pa～9.0×10-2Heating to 1500-1700 ℃ under Pa, and then preserving heat for 1-2 h. The invention prevents the tantalum powder and the tantalum matrix from being oxidized by controlling the vacuum degree during sintering, avoids the defects of sintering failure caused by too low vacuum degree and poor economic benefit caused by too high vacuum degree, and ensures that the tantalum powder and the tantalum powder as well as the tantalum powder and the tantalum matrix of the matrix are mixed by controlling the sintering temperature and timeThe porous tantalum film with good bonding degree is obtained by forming metallurgical bonding through sufficient substance diffusion.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the tantalum powder slurry is sprayed and sintered on the surface of the tantalum substrate, so that a monodisperse porous tantalum film is obtained on the surface of the tantalum substrate, the surface area of the tantalum substrate is effectively increased, and the application of the tantalum substrate in different fields can be promoted.
2. According to the invention, uniform tantalum film green materials are obtained by controlling the slurry concentration and the spraying pressure, and the single-layer distribution of tantalum powder is realized.
3. According to the invention, the tantalum powder is dispersed by the polyvinyl butyral solution, so that uniform tantalum powder slurry can be obtained, and the method is suitable for obtaining a tantalum film by adopting a spraying process; by polishing the tantalum substrate firstly and then chemically polishing, the oxide skin is removed, and simultaneously, a bright and smooth surface is obtained, so that the sintering activity of the tantalum powder and the tantalum substrate is improved, and the tantalum powder and the tantalum substrate form good metallurgical bonding.
4. According to the invention, the tantalum powder and the tantalum matrix are prevented from being oxidized by controlling the vacuum degree during sintering, and the sufficient substance diffusion between the tantalum powder and between the tantalum powder and the tantalum matrix is ensured by controlling the sintering temperature and time, so that metallurgical bonding is formed, and the porous tantalum film with good bonding degree is obtained.
5. The method has the advantages of simple process, environmental friendliness, low cost, suitability for large-scale production, capability of preparing the porous tantalum film with porous structure on the surface and single-layer dispersion of spherical tantalum powder, application in the fields of capacitor devices, hydrogen energy key materials and the like, and high use value.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is an SEM photograph of a porous tantalum film prepared in example 1 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, adding tantalum powder into a polyvinyl butyral solution to obtain tantalum powder slurry; the solid content of the tantalum powder slurry is 45%; the tantalum powder is spherical tantalum powder with the particle size of 1-6 mu m, and the D90 of the spherical tantalum powder is 5.5 mu m; the solvent of the polyvinyl butyral solution is absolute ethyl alcohol, and the mass content of the polyvinyl butyral in the polyvinyl butyral solution is 1%;
polishing the tantalum substrate, and then cleaning with deionized water to obtain the cleaned tantalum substrate; the sanding treatment is sequentially performed by using 280#, 600#, 1000# sand paper; the size of the tantalum substrate is 20mm multiplied by 0.1mm (diameter multiplied by thickness);
step three, carrying out chemical polishing treatment on the cleaned tantalum substrate obtained in the step two to obtain a polished tantalum substrate; the chemical polishing treatment process comprises the following steps: soaking the tantalum substrate in a hydrofluoric acid solution containing 1% of ammonium sulfate by mass for 20min, taking out, immediately washing with deionized water, and blow-drying with nitrogen to obtain a polished tantalum substrate; the hydrofluoric acid solution is an aqueous solution containing 40 mass percent of hydrofluoric acid
Step four, spraying the tantalum powder slurry obtained in the step one on the surface of the polished tantalum substrate obtained in the step three to obtain a tantalum film green body material; the spraying pressure in the spraying is as follows: 0.45 MPa;
step five, performing vacuum sintering on the green body material of the tantalum film obtained in the step four to obtain a porous tantalum film on the surface of the tantalum substrate; the sintering process comprises the following steps: in a high-temperature vacuum furnace, the vacuum degree is 3.0 multiplied by 10-3Heating to 1700 ℃ under Pa, and then preserving heat for 1 h.
Fig. 1 is an SEM image of the porous tantalum film prepared in this example, and it can be seen from fig. 1 that the porous tantalum film having a single layer tantalum powder distribution is obtained on the tantalum substrate, and the porous tantalum film has a porous structure uniformly distributed thereon.
Example 2
The embodiment comprises the following steps:
step one, adding tantalum powder into a polyvinyl butyral solution to obtain tantalum powder slurry; the solid content of the tantalum powder slurry is 65%; the tantalum powder is spherical tantalum powder with the particle size of 1-6 mu m, and the D90 of the spherical tantalum powder is 5.4 mu m; the solvent of the polyvinyl butyral solution is absolute ethyl alcohol, and the mass content of the polyvinyl butyral in the polyvinyl butyral solution is 3%;
polishing the tantalum substrate, and then cleaning with deionized water to obtain the cleaned tantalum substrate; the sanding treatment is sequentially performed by using 280#, 600#, 1000# sand paper; the size of the tantalum substrate is 20mm multiplied by 0.1mm (diameter multiplied by thickness);
step three, carrying out chemical polishing treatment on the cleaned tantalum substrate obtained in the step two to obtain a polished tantalum substrate; the chemical polishing treatment process comprises the following steps: soaking the tantalum substrate in a hydrofluoric acid solution containing 3% of ammonium sulfate by mass for 30min, taking out, immediately washing with deionized water, and blow-drying with nitrogen to obtain a polished tantalum substrate; the hydrofluoric acid solution is an aqueous solution containing 40 mass percent of hydrofluoric acid
Step four, spraying the tantalum powder slurry obtained in the step one on the surface of the polished tantalum substrate obtained in the step three to obtain a tantalum film green body material; the spraying pressure in the spraying is as follows: 0.60 MPa;
step five, performing vacuum sintering on the green body material of the tantalum film obtained in the step four to obtain a porous tantalum film on the surface of the tantalum substrate; the sintering process comprises the following steps: in a high-temperature vacuum furnace, the vacuum degree is 9.0 multiplied by 10-2Heating to 1500 ℃ under Pa, and then preserving heat for 2 h.
Example 3
The embodiment comprises the following steps:
step one, adding tantalum powder into a polyvinyl butyral solution to obtain tantalum powder slurry; the solid content of the tantalum powder slurry is 50%; the tantalum powder is spherical tantalum powder with the particle size of 1-6 mu m, and the D90 of the spherical tantalum powder is 5.1 mu m; the solvent of the polyvinyl butyral solution is absolute ethyl alcohol, and the mass content of the polyvinyl butyral in the polyvinyl butyral solution is 2%;
polishing the tantalum substrate, and then cleaning with deionized water to obtain the cleaned tantalum substrate; the sanding treatment is sequentially performed by using 280#, 600#, 1000# sand paper; the size of the tantalum substrate is 20mm multiplied by 0.1mm (diameter multiplied by thickness);
step three, carrying out chemical polishing treatment on the cleaned tantalum substrate obtained in the step two to obtain a polished tantalum substrate; the chemical polishing treatment process comprises the following steps: soaking the tantalum substrate in a hydrofluoric acid solution containing 2% of ammonium sulfate by mass for 40min, taking out, immediately washing with deionized water, and blow-drying with nitrogen to obtain a polished tantalum substrate; the hydrofluoric acid solution is an aqueous solution containing 40 mass percent of hydrofluoric acid
Step four, spraying the tantalum powder slurry obtained in the step one on the surface of the polished tantalum substrate obtained in the step three to obtain a tantalum film green body material; the spraying pressure in the spraying is as follows: 0.55 MPa;
step five, performing vacuum sintering on the green body material of the tantalum film obtained in the step four to obtain a porous tantalum film on the surface of the tantalum substrate; the sintering process comprises the following steps: in a high-temperature vacuum furnace, the vacuum degree is 1.0 multiplied by 10-2Pa, heating to 1600 ℃ and then preserving the heat for 1.5 h.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (7)
1. A method for preparing a porous tantalum film, comprising the steps of:
step one, adding tantalum powder into a polyvinyl butyral solution to obtain tantalum powder slurry; the solid content of the tantalum powder slurry is 45-65%;
polishing the tantalum substrate, and then cleaning with deionized water to obtain the cleaned tantalum substrate;
step three, carrying out chemical polishing treatment on the cleaned tantalum substrate obtained in the step two to obtain a polished tantalum substrate;
step four, spraying the tantalum powder slurry obtained in the step one on the surface of the polished tantalum substrate obtained in the step three to obtain a tantalum film green body material;
and step five, performing vacuum sintering on the green body material of the tantalum film obtained in the step four to obtain the porous tantalum film on the surface of the tantalum substrate.
2. The method for preparing a porous tantalum film according to claim 1, wherein in the first step, the tantalum powder is spherical tantalum powder, and D90 of the spherical tantalum powder is not more than 5.6 μm.
3. The method for preparing a porous tantalum film according to claim 1, wherein the solvent of the polyvinyl butyral solution in the first step is absolute ethyl alcohol, and the mass content of the polyvinyl butyral in the polyvinyl butyral solution is 1% -3%.
4. The method for preparing a porous tantalum film according to claim 1, wherein in the second step, the sanding treatment is sequentially performed by using 280#, 600#, 1000# sandpaper, and the tantalum substrate is a tantalum sheet.
5. The method for preparing a porous tantalum film according to claim 1, wherein the chemical polishing treatment in the third step is as follows: soaking the tantalum substrate in a hydrofluoric acid solution containing 1-3% of ammonium sulfate by mass for 20-40 min, taking out, immediately washing the tantalum substrate with deionized water, and drying the tantalum substrate with nitrogen to obtain a polished tantalum substrate; the hydrofluoric acid solution is an aqueous solution containing hydrofluoric acid with the mass fraction of 40%.
6. The method for preparing a porous tantalum film according to claim 1, wherein the spraying pressure in the spraying in the fourth step is 0.45MPa to 0.60 MPa.
7. The method for preparing a porous tantalum film according to claim 1, wherein the sintering process in the fifth step is as follows: in a high-temperature vacuum furnace, the degree of vacuumIs 3.0X 10-3Pa～9.0×10-2Heating to 1500-1700 ℃ under Pa, and then preserving heat for 1-2 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114797496A (en) * | 2022-05-20 | 2022-07-29 | 西北有色金属研究院 | Palladium-tantalum composite membrane and preparation method thereof |
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