CN109365802B - Preparation method of core-shell structure metal ceramic composite powder - Google Patents
Preparation method of core-shell structure metal ceramic composite powder Download PDFInfo
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- CN109365802B CN109365802B CN201811346903.XA CN201811346903A CN109365802B CN 109365802 B CN109365802 B CN 109365802B CN 201811346903 A CN201811346903 A CN 201811346903A CN 109365802 B CN109365802 B CN 109365802B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4417—Methods specially adapted for coating powder
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
Abstract
The invention discloses a preparation method of core-shell structure metal ceramic composite powder, which comprises the following steps: 1) carrying out catalytic activation treatment on ceramic powder particles: placing ceramic powder particles in a reactor, heating reaction raw materials, introducing carrier gas carrying reaction raw material vapor into the reactor, and introducing hydrogen to carry out reduction reaction so as to deposit catalytic metal on the surfaces of the ceramic powder particles; 2) placing the ceramic powder particles obtained in the step 1) in a reactor in a water bath, adding a metal salt raw material and a reducing agent, and plating a metal coating layer through an autocatalytic reaction to obtain the metal ceramic composite powder. The invention omits the coarsening, sensitization and activation processes in the traditional chemical plating metal process, does not need to use expensive palladium chloride catalyst, avoids the introduction of impurity palladium, realizes metal plating at lower temperature, has controllable content of the coated metal, has simple integral coating process and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a preparation method of core-shell structure metal ceramic composite powder.
Background
The hard alloy is a composite material which is generally prepared by taking refractory metal hard compounds WC, TiC and the like with high hardness and high elastic modulus as main phases and taking metals Fe, Co and Ni as binder phases through a powder metallurgy process. It has the characteristics of high strength, high hardness, wear resistance, high temperature resistance, corrosion resistance, high elastic modulus, chemical stability and the like of ceramics, and also has better toughness and plasticity. Therefore, the hard alloy is widely applied to the aspects of modern tools, high-temperature resistant materials, wear-resistant materials, corrosion-resistant materials and the like, is one of indispensable materials of a plurality of high and new technologies and modern industries, and is known as 'industrial teeth'.
Because the technical process is simple, the ball milling method (CN103789565B) is widely applied to preparing the hard alloy composite powder. The method is to ball mill the ceramic powder of WC, TiC and the like and metal iron, cobalt or nickel for a long time to mix the ceramic powder and the metal powder. However, the composite powder prepared by the method has the following problems: 1) a large amount of impurities can be introduced in the long-time ball milling process, so that the performance of the formed product is influenced; 2) although the ball milling is carried out for a long time, the density difference between the metal and the ceramic powder easily causes the uneven distribution of the metal in the ceramic matrix, and the segregation is easily caused in the subsequent forming process to influence the performance of the hard alloy.
The hard alloy composite powder is used as a basic unit of hard alloy, wherein the dispersion uniformity of the ceramic powder and the metal powder is an important influence factor of the performance of the hard alloy. In order to solve this problem, a method of depositing a metal layer on the surface of the ceramic particles is generally used to improve the dispersibility of the two phases and enhance the interfacial bonding force between the two phases. Chemical plating (CN1245353C, CN105364081A, CN101403110B, CN106623908A) is an advanced method for preparing composite powder, and a suitable reducing agent is selected to make metal ions in a solution undergo an oxidation-reduction reaction, so that a metal coating is selectively reduced and precipitated on the surface with catalytic activity. However, since the surface of the ceramic powder has no catalytic activity, the ceramic powder needs to be subjected to complex pretreatment processes such as coarsening, activation and sensitization to attach a small amount of palladium on the surface of the ceramic, the process is complex, and each step needs to be washed with water, so that a large amount of water resource waste and pollution are caused. The activation process needs to use expensive palladium chloride, which increases the cost, and a small amount of metal palladium impurities are inevitably introduced into the powder.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a method for preparing a core-shell structure metal-clad ceramic composite powder, in which a powder raw material of a metal-ceramic composite material is used as an entry point. The metal-coated ceramic composite powder synthesized by the method has the advantages of uniform metal distribution on the surface of the powder, controllable content, strong binding force between the coating layer and the ceramic matrix, low impurity content and the like.
In order to achieve the purpose, the specific technical scheme of the invention is as follows:
the invention provides a preparation method of core-shell structure metal ceramic composite powder, which comprises the following steps: 1) carrying out catalytic activation treatment on ceramic powder particles: placing ceramic powder particles in a reactor, heating reaction raw materials, introducing carrier gas carrying reaction raw material vapor into the reactor, and introducing hydrogen to carry out reduction reaction so as to deposit catalytic metal on the surfaces of the ceramic powder particles;
2) placing the ceramic powder particles obtained in the step 1) into a reactor in a water bath, adding a metal salt raw material and a reducing agent, and plating a metal coating layer through an autocatalytic reaction to obtain the metal ceramic composite powder.
Preferably, the ceramic powder particles in step 1) include one or more of tungsten carbide, titanium carbide, chromium carbide, niobium carbide, tantalum carbide, vanadium carbide, titanium nitride and silicon nitride, and the particle size range of the ceramic powder particles is 0.1-1000 μm.
Preferably, the catalytic activation treatment on the particle surface in the step 1) is to deposit a low-content catalytic metal on the particle surface, wherein the catalytic metal comprises one or more of iron, cobalt and nickel, and the mass fraction of the catalytic metal deposit is 0.001-1%.
Preferably, the reaction raw materials in step 1) include one or more of a reaction raw material for depositing iron, a reaction raw material for depositing cobalt, and a reaction raw material for depositing nickel, wherein the reaction raw material for depositing iron is one or more of ferric trifluoride, ferric dichloride, ferric trichloride, ferric dibromide, ferric diiodide, and ferrocene, the reaction raw material for depositing cobalt is one or more of cobalt fluoride, cobalt chloride, cobalt bromide, cobalt iodide, and cobaltocene, and the reaction raw material for depositing nickel is one or more of nickel fluoride, nickel chloride, nickel bromide, nickel iodide, and nickelocene.
Preferably, the particle surface catalytic activation treatment in step 1) employs a chemical vapor deposition technique.
Preferably, the carrier gas in the step 1) comprises one or more of argon, nitrogen, helium and neon, the temperature of the heating reaction raw material is 150-700 ℃, the hydrogen reduction temperature is 450-900 ℃, and the reaction time is 1-10 min.
Preferably, the metal salt raw material in step 2) includes one or more of iron salt, cobalt salt and nickel salt, and the reducing agent includes one or more of sodium hypophosphite, sodium borohydride and hydrazine hydrate.
Preferably, the iron salt comprises one or more of ferrous sulfate, ferrous nitrate and ferrous chloride, the cobalt salt comprises one or more of cobalt sulfate, cobalt nitrate, cobalt oxalate and cobalt chloride, and the nickel salt comprises one or more of nickel sulfate, nickel nitrate and nickel chloride.
Preferably, the water bath heating temperature in the step 2) is 50-100 ℃, the pH value is 8-12, and the reaction time is 5-120 min.
The invention provides a core-shell structure metal ceramic composite powder prepared by a preparation method, wherein metal in the metal ceramic composite powder comprises one or more of iron, cobalt and nickel, and the mass fraction of the metal coating is 1-50%.
The invention discloses a preparation method of core-shell structure metal ceramic composite powder, belonging to the technical field of powder metallurgy. The invention utilizes chemical vapor deposition to deposit a small amount of metallic iron, cobalt or nickel on the surface of the ceramic powder, and utilizes the catalytic activity of the metallic iron, cobalt or nickel to self-catalytically plate a large amount of metallic iron, cobalt or nickel. The method does not need coarsening, sensitizing and activating processes in the traditional chemical plating process of the ceramic powder, has simple process, and particularly does not need expensive catalyst palladium chloride. In addition, the autocatalytic metal plating process is carried out at a lower temperature, so that the energy consumption is reduced, and the production cost can be greatly reduced. The composite powder has the advantages of pure product, strong binding force between the coating layer and the ceramic matrix, uniform and compact coating, controllable content, simple process and the like, and is suitable for large-scale industrial production. The composite powder obtained by the method is easy to alloy in the subsequent powder metallurgy process, and is not easy to segregate in the using process.
Compared with the prior art, the invention has the advantages that:
(1) a chemical vapor deposition technology is adopted to pre-deposit a small amount of metal iron, cobalt or nickel on the surface of the ceramic powder particles, and the coarsening, sensitization and activation processes in the traditional chemical plating process of the ceramic powder are replaced, so that the process is simplified, and the time is saved;
(2) the catalytic activity of the metal iron, cobalt or nickel is utilized to selectively reduce and separate out metal on the surface of the ceramic powder, so that the use of palladium chloride is omitted, the introduction of impurity palladium is avoided, and the production cost is greatly reduced;
(3) the metal coating layer deposited in situ on the surface of the ceramic powder particles has high coating integrity and strong interface bonding capability with the ceramic powder particles;
(4) controllable coating and multi-metal mixed coating of the metal coating layer are realized, and the thickness and the content of the metal coating layer in the ceramic powder can be adjusted by adjusting parameters such as autocatalytic plating temperature, pH, metal salt concentration and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a field emission scan of a cobalt-coated tungsten carbide composite powder according to example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a field emission microscope of a nickel-coated titanium carbide composite powder according to example 2 of the present invention;
FIG. 3 is a SEM image of the Fe-Ni coated SiC composite powder of example 3 of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. Unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features. The description is only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
The invention is further illustrated by the following examples:
example 1
Cobalt chloride is used as a chemical vapor deposition cobalt source, nitrogen is used as a carrier gas, the cobalt chloride is heated to 650 ℃, hydrogen is used as a reducing gas, the temperature is 750 ℃, a small amount of cobalt is deposited on tungsten carbide powder with the particle size of 50 mu m, the deposition time is 1min, and the mass fraction of the cobalt in the obtained cobalt-coated tungsten carbide composite powder is 0.01%. Putting the powder into an autocatalytic cobalt plating stirring reactor, heating the powder to 50 ℃ in a water bath, controlling the pH value to be 8, taking cobalt sulfate as a cobalt salt and hydrazine hydrate as a reducing agent, and reacting for 60min to obtain the cobalt-coated tungsten carbide composite powder, wherein the mass fraction of the metal cobalt coating amount is 30%.
The field emission scanning electron microscope image of the cobalt-coated tungsten carbide composite powder is shown in fig. 1, and it can be seen from fig. 1 that metallic cobalt is completely deposited on the surface of the tungsten carbide particles.
Example 2
Nickel chloride is used as a chemical vapor deposition nickel source, argon is used as a carrier gas, the nickel chloride is heated to 680 ℃, hydrogen is used as a reducing gas, the temperature is 720 ℃, a small amount of nickel is deposited on the titanium carbide powder with the particle size of 100 mu m, the deposition time is 5min, and the mass fraction of nickel in the obtained nickel-coated titanium carbide composite powder is 0.1%. Putting the powder into an autocatalytic nickel plating stirring reactor, heating the powder to 70 ℃ in a water bath, controlling the pH value to be 12, taking nickel chloride as nickel salt and sodium hypophosphite as a reducing agent, and reacting for 120min to obtain the nickel-coated titanium carbide composite powder, wherein the mass fraction of the metal nickel coating is 50%.
The field emission scanning electron microscope image of the nickel-coated titanium carbide composite powder is shown in fig. 2, and it can be seen from fig. 2 that metallic nickel is completely deposited on the surface of the titanium carbide particles.
Example 3
Ferrocene is used as an iron source for chemical vapor deposition, neon is used as a carrier gas, the ferrocene is heated to 150 ℃, hydrogen is used as a reducing gas, the temperature is 900 ℃, a small amount of iron is deposited on silicon carbide powder with the particle size of 500 mu m, the deposition time is 10min, and the mass fraction of the iron in the obtained iron-coated silicon carbide composite powder is 1%. Putting the powder into an autocatalytic iron-nickel plating stirring reactor, heating the powder to 90 ℃ in a water bath, controlling the pH value to be 10, taking ferrous sulfate as an iron salt, nickel sulfate as a nickel salt and sodium borohydride as a reducing agent, and reacting for 60min to obtain iron-nickel coated silicon carbide composite powder, wherein the mass fraction of the metal coating amount is 10%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of core-shell structure metal ceramic composite powder comprises the following steps:
1) carrying out catalytic activation treatment on ceramic powder particles: placing ceramic powder particles in a reactor, heating reaction raw materials, introducing carrier gas carrying reaction raw material vapor into the reactor, and introducing hydrogen to carry out reduction reaction so as to deposit catalytic metal on the surfaces of the ceramic powder particles;
the mass fraction of the catalytic metal deposition is 0.001-1%;
2) placing the ceramic powder particles obtained in the step 1) in a reactor in a water bath, adding a metal salt raw material and a reducing agent, and plating a metal coating layer through an autocatalytic reaction to obtain metal ceramic composite powder;
the water bath heating temperature in the step 2) is 50-100 ℃, and the pH value is 8-12.
2. The preparation method of the core-shell structure metal ceramic composite powder according to claim 1, wherein ceramic powder particles in the step 1) comprise one or more of tungsten carbide, titanium carbide, chromium carbide, niobium carbide, tantalum carbide, vanadium carbide, titanium nitride and silicon nitride, and the particle size range of the ceramic powder particles is 0.1-1000 μm.
3. The preparation method of the core-shell structure cermet composite powder according to claim 1, wherein the catalytic activation treatment of the particle surface in step 1) is deposition of low content of catalytic metal on the particle surface, wherein the catalytic metal comprises one or more of iron, cobalt and nickel.
4. The method for preparing the core-shell structured metal ceramic composite powder according to claim 1, wherein the reaction raw material in step 1) comprises one or more of a reaction raw material for depositing iron, a reaction raw material for depositing cobalt and a reaction raw material for depositing nickel, wherein the reaction raw material for depositing iron comprises one or more of ferric trifluoride, ferric dichloride, ferric trichloride, ferric dibromide, ferric diiodide and ferrocene, the reaction raw material for depositing cobalt comprises one or more of cobalt fluoride, cobalt chloride, cobalt bromide, cobalt iodide and cobaltocene, and the reaction raw material for depositing nickel comprises one or more of nickel fluoride, nickel chloride, nickel bromide, nickel iodide and nickocene.
5. The preparation method of the core-shell structure cermet composite powder according to any of claims 1-4, characterized in that the particle surface catalytic activation treatment in step 1) employs chemical vapor deposition technology.
6. The preparation method of the core-shell structure metal ceramic composite powder according to any one of claims 1 to 4, wherein the carrier gas in the step 1) comprises one or more of argon, nitrogen, helium and neon, the temperature of the heating reaction raw material is 150-700 ℃, the hydrogen reduction temperature is 450-900 ℃, and the reaction time is 1-10 min.
7. The method for preparing the core-shell structured cermet composite powder according to claim 1, wherein the metal salt raw material in step 2) includes one or more of iron salt, cobalt salt and nickel salt, and the reducing agent includes one or more of sodium hypophosphite, sodium borohydride and hydrazine hydrate.
8. The preparation method of the core-shell structure cermet composite powder according to claim 7, wherein the iron salt comprises one or more of ferrous sulfate, ferrous nitrate and ferrous chloride, the cobalt salt comprises one or more of cobalt sulfate, cobalt nitrate, cobalt oxalate and cobalt chloride, and the nickel salt comprises one or more of nickel sulfate, nickel nitrate and nickel chloride.
9. The preparation method of the core-shell structure metal ceramic composite powder according to claim 1, wherein the reaction time in the step 2) is 5-120 min.
10. The core-shell structure metal ceramic composite powder prepared by the preparation method of any one of claims 1 to 9 is characterized in that metal in the metal ceramic composite powder comprises one or more of iron, cobalt and nickel, and the mass fraction of metal coating is 1-50%.
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| CN109852952B (en) * | 2019-02-28 | 2021-03-30 | 浙江英洛华磁业有限公司 | Hydrazine hydrate chemical nickel plating solution, preparation method thereof and nickel plating method |
| CN111424267B (en) * | 2020-04-24 | 2021-10-01 | 昆明理工大学 | Method for preparing nickel-coated bismuth sulfur chloride |
| CN112570711A (en) * | 2020-11-26 | 2021-03-30 | 中铭富驰（苏州）纳米高新材料有限公司 | Preparation method of nickel-coated titanium carbide composite powder |
| CN112548096A (en) * | 2020-12-14 | 2021-03-26 | 中北大学 | Cobalt-coated ceramic composite powder and preparation method and application thereof |
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| US5076841A (en) * | 1990-05-31 | 1991-12-31 | Shipley Company Inc. | Coating composition |
| CN1572903A (en) * | 2003-06-24 | 2005-02-02 | 罗姆和哈斯电子材料有限责任公司 | Catalyst composition and deposition method |
| CN101054663A (en) * | 2007-05-29 | 2007-10-17 | 南京工业大学 | Activating process for nonmetal basal body chemical plating |
| CN101210316A (en) * | 2007-12-25 | 2008-07-02 | 大连理工大学 | Heat treatment method for preparing carbon coating nano composite particles by using gas carbon source |
| CN104178752A (en) * | 2013-05-23 | 2014-12-03 | 中国科学院大连化学物理研究所 | Activation method used before chemical plating of palladium or palladium alloy film |
| CN108705077A (en) * | 2018-05-25 | 2018-10-26 | 中国科学院过程工程研究所 | A kind of preparation method of nucleocapsid iron coating ceramic composite granule |
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