CN108866518B - Method for preparing chemical nickel plating layer on surface of nickel ferrite ceramic material without sensitization and activation - Google Patents
Method for preparing chemical nickel plating layer on surface of nickel ferrite ceramic material without sensitization and activation Download PDFInfo
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- CN108866518B CN108866518B CN201810824193.0A CN201810824193A CN108866518B CN 108866518 B CN108866518 B CN 108866518B CN 201810824193 A CN201810824193 A CN 201810824193A CN 108866518 B CN108866518 B CN 108866518B
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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
- 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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
Abstract
A method for preparing a chemical nickel plating layer on the surface of a nickel ferrite ceramic material without sensitization and activation comprises the following steps: (1) preparation of Fe2O3、NiO、Ni、MnO2And V2O5The powder of (2) is added with organic binder for grinding after wet grinding and mixingGranulating and screening out the bonding material; after compression molding, sintering, crushing and screening to obtain ceramic particles; (2) mixing NiCl2、NaH2PO2Mixing trisodium citrate, sodium acetate and lactic acid, and adding ammonia water to obtain chemical nickel plating solution; (3) and heating the chemical nickel plating solution, immersing the ceramic particles, adding ammonia water, carrying out chemical nickel plating, filtering, washing and drying. The method prepares the composite ceramic by adding Ni powder in the high-temperature synthesis process, takes a large amount of uniformly distributed Ni as an active catalytic center, does not need the processes of coarsening, sensitization, activation and the like, simplifies the process flow, shortens the time and reduces the production cost.
Description
Technical Field
The invention belongs to the technical field of material surface modification, and particularly relates to a method for preparing a chemical nickel-plating layer on the surface of a nickel ferrite ceramic material without sensitization and activation.
Background
NiFe2O4The ceramic belongs to a cubic crystal ionic compound, Ni-O, Fe-O in a spinel structure is a strong ionic bond, the electrostatic strength of each bond is equal, the structure is firm, the thermal conductivity and the thermal expansibility are the same in all directions, the thermal expansion coefficient is small, and the ceramic has the advantages of high strength, high melting point, good chemical stability and gas sensitivity, high catalytic activity, soft magnetic property and the like, and is widely applied to the fields of structural ceramics, electrode materials, catalysts, gas sensors, magnetic fluids, microwave absorbing materials and the like.
NiFe2O4Ceramics belong to high-temperature semiconductor materials, have relatively poor electrical conductivity at room temperature and poor surface weldability, and severely restrict the application of the ceramics, so that the ceramics need to be subjected to surface metallization modification treatment. There are many methods for modifying the surface of ceramics by metallization, such as vacuum evaporationMagnetron sputtering, electroplating, chemical plating, and the like. The chemical nickel plating has the advantages of good uniformity, high hardness, corrosion resistance, conductivity, weldability and other comprehensive physical and chemical properties, and the plating is not limited by the shape of the matrix, the thickness of the plating layer is adjustable, the process is simple, the application range is wide, and the like, so the chemical nickel plating can be widely applied to the industries of electronics, valve manufacturing, machinery, petrochemical industry, automobiles, aerospace and the like. The ceramic itself has no catalytic activity for the chemical reduction of metals, and if no pretreatment is carried out, chemical plating on the surface of the ceramic is impossible, and activation treatment must be carried out before chemical plating. Conventional SnCl2-PdCl2The sensitization-activation process has complex treatment process, the price of palladium is expensive, the cost is high, and PdCl2Has strong toxicity and great pollution. Therefore, researchers have been studying new palladium-free activation processes, and the activation process using nickel as a catalyst has become a hot spot of current research. Literature "study of Process for chemical plating of Ni-P alloy on ceramic surface" (Lilibo, Lidongping, Zhang Shuhua, etc.) ceramic sheets were immersed in NiSO4·6H2O、NaH2PO2And C2H6In the activating solution consisting of O, the nickel salt is reduced to an active center by heat treatment at 280 ℃ for 12min, and a nickel coating which is completely, uniformly and compactly covered is obtained after chemical plating. In the literature, "investigation of palladium-free activated electroless nickel plating on glass surface" (Foundry, Liyi, Wangben, etc.) studies on Ni (Ac)2、NaH2PO2And CH3And (3) activating the mixed solution with OH as a component, wherein hydrazine hydrate is used as a reducing agent, the mixed solution is activated for 30min at the temperature of 165-170 ℃, and active nickel is prepared by a thermal reduction decomposition method and is used as an active center for subsequent chemical plating. The patent ' palladium-free activation chemical nickel plating process for the surface of the alumina ceramic ' (Zhangliang, Zhang Baoquan) ' soaks the coarsened alumina ceramic in a boron salt solution for 20-30 seconds, and soaks the alumina ceramic in a nickel colloid for 20-30 seconds after washing, so that a plurality of uniformly distributed surface active centers can be formed, and a flat, continuous and compact nickel plating layer is obtained on the surface of the alumina after chemical plating. Although the activation process using nickel as catalyst has been developed, it is required to be carried out in nickel salt solution or colloid, and oil removal is required before activation,Coarsening and the like, the process is relatively complex, and the problems of pollution and the like are easily caused.
Disclosure of Invention
Aiming at the defects of the prior nickel ferrite ceramic material surface treatment technology, the invention provides a method for preparing a chemical nickel plating layer without sensitization and activation on the surface of a nickel ferrite ceramic material, and NiFe is synthesized by high-temperature sintering2O4Ni-NiFe prepared by doping metal Ni powder in process2O4The composite ceramic takes uniformly distributed active Ni as a chemical plating catalytic center, does not need sensitization and activation pretreatment, and solves the problem that SnCl is adopted in the prior art2-PdCl2The high cost of the sensitization-activation process and the relative complexity and contamination problems of the nickel salt activation process, while in NiFe2O4And plating a continuous compact chemical nickel plating layer on the surface of the ceramic chip after the ceramic particles.
The method of the invention comprises the following steps:
1. preparation of Fe2O3Powder, NiO powder, Ni powder, MnO2Powder and V2O5The powder is used as a raw material, absolute ethyl alcohol is used as a wet grinding medium, all the raw materials are subjected to wet grinding and mixing for 2-4 hours by using a ball grinding tank, and then the absolute ethyl alcohol is dried to be removed, so that mixed powder is obtained; adding an organic binder into the mixed powder for grinding and granulating, wherein the organic binder accounts for 2-6% of the total mass of the mixed powder, and screening out a part with the particle size of less than or equal to 250 mu m after grinding and granulating to serve as a binding material; pressing and molding the bonding material under the condition of 100-200 MPa to prepare a green body; sintering the green body for 4-6 hours under the condition of protective atmosphere and at 1200-1300 ℃, and cooling to normal temperature along with the furnace to obtain a composite ceramic block material; crushing the composite ceramic block, and screening out a part with the particle size of 74-250 mu m as nickel ferrite ceramic particles;
2. nickel salt NiCl2•6H2O, reducing agent NaH2PO2•H2O, complexing agent trisodium citrate and buffering agent sodium acetate are respectively added with water to prepare NiCl2Solution, NaH2PO2The solution, the trisodium citrate solution and the sodium acetate solution are mixed and added with lactic acid, and then added with water and mixed evenly,finally, adding ammonia water to adjust the pH value to 9.0-9.5 to prepare a chemical nickel plating solution;
3. heating the chemical nickel plating solution to 65-75 ℃, then immersing the nickel ferrite ceramic particles into the chemical nickel plating solution, stirring the chemical nickel plating solution through a stirrer to uniformly disperse the nickel ferrite ceramic particles in the chemical nickel plating solution for chemical nickel plating, and adding ammonia water to control the pH value of the chemical nickel plating solution to be 8.5-9.5; and when the color of the chemical nickel plating solution is changed from green to clear, the chemical nickel plating is finished, all materials after the chemical nickel plating are filtered and separated, the obtained solid phase is washed by water until the filtrate is neutral, and then the solid phase is dried to remove moisture, so that a chemical nickel plating layer is prepared on the surface of the nickel ferrite ceramic particles.
Fe as described above2O3The grain diameter of the powder is less than or equal to 1 mu m, the grain diameter of the NiO powder is less than or equal to 10 mu m, the grain diameter of the Ni powder is less than or equal to 100 mu m, MnO2The particle diameter of the powder is less than or equal to 5 mu m, V2O5The particle size of the powder is less than or equal to 100 mu m.
In the step 1, the mass fraction of Ni in the nickel ferrite ceramic particles is 4-10%, and MnO is added2The mass fraction of (A) is 1-3% and V2O5The mass fraction of the alloy is 0.5-1.5%, and the balance is NiFe2O4Preparing raw materials according to the mass fraction of the nickel ferrite ceramic particles, wherein Fe2O3The powder and NiO powder are fully reacted to generate NiFe in the sintering process2O4。
The organic binder is a polyvinyl alcohol solution, wherein the mass fraction of polyvinyl alcohol is 2-8%.
In the step 1, the protective atmosphere is argon atmosphere, and the oxygen partial pressure under the protective atmosphere is 10-50 Pa.
In the step 2, NiCl in the chemical nickel plating solution2The concentration of the mixed solution is 28-36 g/L, NaH2PO2The concentration is 28-36 g/L, the concentration of lactic acid is 15-25 mL/L, the concentration of trisodium citrate is 20-30 g/L, and the concentration of sodium acetate is 10-20 g/L.
The mass concentration of the ammonia water is 10-15%.
In the step 3, 20-40 g of nickel ferrite ceramic particles are placed in 1L of chemical nickel plating solution.
In the step 3, the thickness of the chemical nickel plating layer on the surface of the nickel ferrite ceramic particles is 8-12 μm, and the nickel content of the chemical nickel plating layer is more than or equal to 90% by mass percent.
Compared with the prior art, the invention has the following characteristics and positive effects:
(1) synthesis of NiFe by high-temperature solid-phase reaction2O4In the ceramic process, a large amount of Ni-NiFe with uniformly distributed Ni particles is prepared by doping metal Ni powder2O4The Ni particles have high activity, can be used as a catalytic center of chemical nickel plating, promote the normal operation of the chemical plating process, avoid the process procedures of oil removal, coarsening, sensitization, activation and the like before the conventional chemical nickel plating, simplify the process flow, reduce the production cost and reduce the pollution of waste liquid to the environment;
（2）Ni-NiFe2O4nickel particles embedded in NiFe in composite ceramic2O4In ceramics, the bonding is tight, and the traditional activation process is that Pt or Ni is attached to NiFe2O4The ceramic surface has poor binding force, and the nickel catalytic center and the nickel coating have the same components, which is beneficial to the tight combination of the nickel coating and the nickel catalytic center, so compared with the traditional activation process, the nickel coating and the NiFe2O4The bonding strength between the ceramics is higher, and the bonding is tighter.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is an electron microscope micrograph of nickel ferrite ceramic particles having a surface with a chemical nickel plating layer according to example 1 of the present invention;
FIG. 3 is an electron microscope micrograph of nickel ferrite ceramic particles having a surface with a chemical nickel plating layer according to example 2 of the present invention;
FIG. 4 is an electron microscope micrograph of nickel ferrite ceramic particles having a surface with a chemical nickel plating layer according to example 3 of the present invention.
Detailed Description
The following describes preferred embodiments of the present invention in detail with reference to the examples.
Fe used in the examples of the present invention2O3Powder, NiO powder, Ni powder, MnO2Powder and V2O5The powders were all commercially available.
NiCl adopted in the embodiment of the invention2•6H2O、NaH2PO2•H2O, trisodium citrate, sodium acetate and lactic acid are commercially available analytical pure reagents.
The ammonia water adopted in the embodiment of the invention is prepared by diluting a commercially available analytical pure reagent (with the mass concentration of 25-28%), and the mass concentration is 10-15%.
The polyvinyl alcohol used in the examples of the present invention was a commercially available analytical reagent.
The device used for observing the microscopic morphology in the embodiment of the invention is an Ultra Plus type field emission scanning electron microscope.
In the embodiment of the invention, the mixed powder and the solid phase are dried by adopting a vacuum drying oven under the following drying conditions: the temperature is 80 plus or minus 2 ℃, and the vacuum degree is less than or equal to 67 Pa.
In the embodiment of the invention, a mortar is used for grinding and granulating.
In the embodiment of the invention, the dosage of the absolute ethyl alcohol during wet grinding is based on the immersion of all raw materials.
In the embodiment of the invention, the chemical nickel plating solution is heated by adopting a constant-temperature water bath kettle.
The water used in the examples of the present invention is deionized water.
The nickel content of the electroless nickel plating layer in the embodiment of the invention is obtained by EDS analysis.
In the embodiment of the invention, a YES-2000 digital display type pressure tester is adopted for compression molding.
In the embodiment of the invention, the stirring speed is 300-500 rpm when the chemical nickel plating solution is stirred.
Example 1
Preparation of Fe2O3Powder, NiO powder, Ni powder, MnO2Powder and V2O5Powder as raw material, Fe2O3The grain diameter of the powder is less than or equal to 1 mu m, the grain diameter of the NiO powder is less than or equal to 10 mu m, the grain diameter of the Ni powder is less than or equal to 100 mu m, MnO2The particle diameter of the powder is less than or equal to 5 mu m, V2O5Powder particleThe diameter is less than or equal to 100 mu m;
adopting absolute ethyl alcohol as a wet grinding medium, carrying out wet grinding and mixing on all the raw materials for 2 hours by using a ball grinding tank, and then drying to remove the absolute ethyl alcohol to obtain mixed powder; adding an organic binder into the mixed powder for grinding and granulating, wherein the organic binder accounts for 2% of the total mass of the mixed powder, and screening out a part with the particle size of less than or equal to 250 mu m after grinding and granulating to serve as a binding material; pressing and molding the bonding material under the condition of 150MPa to prepare a green body; sintering the green body for 5 hours under the condition of protective atmosphere and 1250 ℃, and cooling to normal temperature along with the furnace to obtain a composite ceramic block material; crushing the composite ceramic block, and screening out a part with the particle size of 74-250 mu m as nickel ferrite ceramic particles;
the mass fraction of Ni in the nickel ferrite ceramic particles is 4 percent, and MnO is2Is 3% and V2O5The mass fraction of the alloy is 0.5 percent, and the rest is NiFe2O4Preparing raw materials according to the mass fraction of the nickel ferrite ceramic particles, wherein Fe2O3The powder and NiO powder are fully reacted to generate NiFe in the sintering process2O4；
The organic binder is polyvinyl alcohol solution, wherein the mass fraction of polyvinyl alcohol is 8%;
the protective atmosphere is argon atmosphere, and the oxygen partial pressure under the protective atmosphere condition is 10 Pa;
nickel salt NiCl2•6H2O, reducing agent NaH2PO2•H2O, complexing agent trisodium citrate and buffering agent sodium acetate are respectively added with water to prepare NiCl2Solution, NaH2PO2Mixing the solution, a trisodium citrate solution and a sodium acetate solution, adding lactic acid, adding water, uniformly mixing, and finally adding ammonia water to adjust the pH value to 9.0 to prepare a chemical nickel plating solution;
NiCl in chemical nickel plating solution2Concentration 28g/L, NaH2PO2The concentration is 36g/L, the concentration of lactic acid is 15 mL/L, the concentration of trisodium citrate is 30g/L, and the concentration of sodium acetate is 10 g/L;
heating the chemical nickel plating solution to 70 ℃, then immersing the nickel ferrite ceramic particles into the chemical nickel plating solution, and placing 20g of nickel ferrite ceramic particles in every 1L of the chemical nickel plating solution; stirring the chemical nickel plating solution by a stirrer to uniformly disperse nickel ferrite ceramic particles in the chemical nickel plating solution for chemical nickel plating, and adding ammonia water to control the pH value of the chemical nickel plating solution to be 8.5; when the color of the chemical nickel plating solution is changed from green to clear, the chemical nickel plating is finished, all materials after the chemical nickel plating are filtered and separated, the obtained solid phase is washed by water until the filtrate is neutral, then the solid phase is dried to remove moisture, and a chemical nickel plating layer is prepared on the surface of the nickel ferrite ceramic particles; the flow is shown in figure 1;
the average thickness of a chemical nickel plating layer on the surface of the nickel ferrite ceramic particles is 12 mu m, and the chemical nickel plating layer comprises 93 percent of nickel by mass; the microscopic morphology of the electron microscope is shown in FIG. 2, and it can be seen from the figure that a large amount of Ni particles are attached to the surface of the particles.
Example 2
The method is the same as example 1, except that:
(1) the mass fraction of Ni in the nickel ferrite ceramic particles is 10 percent, and MnO is2Is 1% and V2O5The mass fraction of (A) is 1.5%; wet milling and mixing for 3 hours in a ball milling tank;
(2) the organic binder accounts for 6 percent of the total mass of the mixed powder; compression molding pressure is 100 MPa; sintering the green body for 6 hours under the condition of protective atmosphere and 1200 ℃; the mass fraction of the polyvinyl alcohol is 2 percent; the oxygen partial pressure under the protective atmosphere condition is 50 Pa;
(3) NiCl in chemical nickel plating solution2Concentration 36g/L, NaH2PO2The concentration is 28g/L, the concentration of lactic acid is 25 mL/L, the concentration of trisodium citrate is 20g/L, and the concentration of sodium acetate is 20 g/L; adjusting the pH value to 9.3 by ammonia water;
(4) heating the chemical nickel plating solution to 65 ℃, then immersing nickel ferrite ceramic particles into the chemical nickel plating solution, and placing 30g of nickel ferrite ceramic particles in every 1L of the chemical nickel plating solution; stirring the chemical nickel plating solution by a stirrer to uniformly disperse nickel ferrite ceramic particles in the chemical nickel plating solution for chemical nickel plating, and adding ammonia water to control the pH value of the chemical nickel plating solution to be 9.0;
(5) the average thickness of a chemical nickel plating layer on the surface of the nickel ferrite ceramic particles is 10 mu m, and the chemical nickel plating layer comprises 92% of nickel by mass percent; the microscopic morphology of the electron microscope is shown in FIG. 3, and it can be seen from the figure that a small amount of fold structures are formed on the particle surface.
Example 3
The method is the same as example 1, except that:
(1) the mass fraction of Ni in the nickel ferrite ceramic particles is 8 percent, and MnO is2Is 2% and V2O5The mass fraction of (A) is 1.0%; wet milling and mixing for 4 hours in a ball milling tank;
(2) the organic binder accounts for 4 percent of the total mass of the mixed powder; compression molding pressure is 200 MPa; sintering the green body for 4 hours under the conditions of protective atmosphere and 1300 ℃; the mass fraction of the polyvinyl alcohol is 5 percent; the oxygen partial pressure under the protective atmosphere condition is 30 Pa;
(3) NiCl in chemical nickel plating solution2Concentration 32g/L, NaH2PO2The concentration is 33g/L, the lactic acid concentration is 20 mL/L, the trisodium citrate concentration is 25g/L, and the sodium acetate concentration is 15 g/L; adjusting the pH value to 9.5 by ammonia water;
(4) heating the chemical nickel plating solution to 75 ℃, then immersing the nickel ferrite ceramic particles into the chemical nickel plating solution, and placing 40g of nickel ferrite ceramic particles in every 1L of the chemical nickel plating solution; stirring the chemical nickel plating solution by a stirrer to uniformly disperse nickel ferrite ceramic particles in the chemical nickel plating solution for chemical nickel plating, and controlling the pH value of the chemical nickel plating solution to be 9.5 by adding ammonia water;
(5) the average thickness of a chemical nickel plating layer on the surface of the nickel ferrite ceramic particles is 8 mu m, and the chemical nickel plating layer comprises 91 percent of nickel by mass;
(6) the microscopic morphology of the electron microscope is shown in FIG. 4, and it can be seen that the particle surface is smooth.
Claims (8)
1. A method for preparing a chemical nickel plating layer on the surface of a nickel ferrite ceramic material without sensitization and activation is characterized by comprising the following steps:
(1) preparation of Fe2O3Powder, NiO powder, Ni powder, MnO2Powder and V2O5The powder is prepared from anhydrous ethanolAs a wet grinding medium, wet grinding and mixing all the raw materials for 2-4 hours by using a ball milling tank, and then drying to remove absolute ethyl alcohol to obtain mixed powder; adding an organic binder into the mixed powder for grinding and granulating, wherein the organic binder accounts for 2-6% of the total mass of the mixed powder, and screening out a part with the particle size of less than or equal to 250 mu m after grinding and granulating to serve as a binding material; pressing and molding the bonding material under the condition of 100-200 MPa to prepare a green body; sintering the green body for 4-6 hours under the condition of protective atmosphere and at 1200-1300 ℃, and cooling to normal temperature along with the furnace to obtain a composite ceramic block material; crushing the composite ceramic block, and screening out a part with the particle size of 74-250 mu m as nickel ferrite ceramic particles;
(2) nickel salt NiCl2•6H2O, reducing agent NaH2PO2•H2O, complexing agent trisodium citrate and buffering agent sodium acetate are respectively added with water to prepare NiCl2Solution, NaH2PO2Mixing the solution, a trisodium citrate solution and a sodium acetate solution, adding lactic acid, adding water, uniformly mixing, and finally adding ammonia water to adjust the pH value to 9.0-9.5 to prepare a chemical nickel plating solution;
(3) heating the chemical nickel plating solution to 65-75 ℃, then immersing the nickel ferrite ceramic particles into the chemical nickel plating solution, stirring the chemical nickel plating solution through a stirrer to uniformly disperse the nickel ferrite ceramic particles in the chemical nickel plating solution for chemical nickel plating, and adding ammonia water to control the pH value of the chemical nickel plating solution to be 8.5-9.5; and when the color of the chemical nickel plating solution is changed from green to clear, the chemical nickel plating is finished, all materials after the chemical nickel plating are filtered and separated, the obtained solid phase is washed by water until the filtrate is neutral, and then the solid phase is dried to remove moisture, so that a chemical nickel plating layer is prepared on the surface of the nickel ferrite ceramic particles.
2. The method for preparing the electroless nickel plating layer on the surface of the nickel ferrite ceramic material without sensitization and activation according to claim 1, characterized in that the Fe2O3The grain diameter of the powder is less than or equal to 1 mu m, the grain diameter of the NiO powder is less than or equal to 10 mu m, the grain diameter of the Ni powder is less than or equal to 100 mu m, MnO2The particle diameter of the powder is less than or equal to 5 mu m, V2O5The particle size of the powder is less than or equal to 100 mu m.
3. The method for preparing the chemical nickel plating layer on the surface of the nickel ferrite ceramic material without sensitization and activation according to claim 1, wherein the mass fraction of Ni in the nickel ferrite ceramic particles is 4-10%, and MnO is added2The mass fraction of (A) is 1-3% and V2O5The mass fraction of the alloy is 0.5-1.5%, and the balance is NiFe2O4Preparing raw materials according to the mass fraction of the nickel ferrite ceramic particles, wherein Fe2O3The powder and NiO powder are fully reacted to generate NiFe in the sintering process2O4。
4. The method for preparing the electroless nickel plating layer on the surface of the nickel ferrite ceramic material without sensitization and activation according to claim 1, wherein the organic binder is a polyvinyl alcohol solution, and the mass fraction of polyvinyl alcohol is 2-8%.
5. The method for preparing the chemical nickel plating layer on the surface of the nickel ferrite ceramic material without sensitization and activation according to claim 1, wherein the protective atmosphere is argon atmosphere, and the oxygen partial pressure under the protective atmosphere is 10-50 Pa.
6. The method for preparing the chemical nickel plating layer on the surface of the nickel ferrite ceramic material without sensitization and activation according to claim 1, characterized in that NiCl is contained in the chemical nickel plating solution2The concentration of the mixed solution is 28-36 g/L, NaH2PO2The concentration is 28-36 g/L, the concentration of lactic acid is 15-25 mL/L, the concentration of trisodium citrate is 20-30 g/L, and the concentration of sodium acetate is 10-20 g/L.
7. The method for preparing the chemical nickel plating layer on the surface of the nickel ferrite ceramic material without sensitization and activation according to claim 1, wherein 20-40 g of nickel ferrite ceramic particles are placed in 1L of chemical nickel plating solution in the step (3).
8. The method for preparing the chemical nickel plating layer on the surface of the nickel ferrite ceramic material without sensitization and activation according to claim 1, wherein in the step (3), the thickness of the chemical nickel plating layer on the surface of the nickel ferrite ceramic particles is 8-12 μm, and the nickel content of the chemical nickel plating layer is more than or equal to 90% by mass percent.
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Application publication date: 20181123 Assignee: SUNSTONE DEVELOPMENT Co.,Ltd. Assignor: Northeastern University Contract record no.: X2021210000060 Denomination of invention: Method for preparing electroless nickel plating layer without sensitization and activation on the surface of nickel ferrite ceramic material Granted publication date: 20200331 License type: Exclusive License Record date: 20211202 |
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