CN110042373B - Diamond containing metal-ceramic composite coating and preparation method thereof - Google Patents

Diamond containing metal-ceramic composite coating and preparation method thereof Download PDF

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CN110042373B
CN110042373B CN201910292846.XA CN201910292846A CN110042373B CN 110042373 B CN110042373 B CN 110042373B CN 201910292846 A CN201910292846 A CN 201910292846A CN 110042373 B CN110042373 B CN 110042373B
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solution
diamond
powder
metal
stirring
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CN110042373A (en
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文中流
王刚
贺冲
张福绪
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Guangdong xinjinggang Diamond Tools Co., Ltd
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Guangdong Xinjinggang Diamond Tools Co Ltd
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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
    • C23C18/1655—Process features
    • C23C18/1662—Use of incorporated material in the solution or dispersion, e.g. particles, whiskers, wires
    • 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
    • C23C18/1655—Process features
    • C23C18/1664—Process features with additional means during the plating process
    • C23C18/1669—Agitation, e.g. air introduction
    • 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
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
    • C23C18/1879—Use of metal, e.g. activation, sensitisation with noble metals
    • 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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  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Chemically Coating (AREA)

Abstract

The invention discloses a method for preparing a diamond containing a metal-ceramic composite coating, which comprises the following steps: respectively putting 60-200 parts of diamond powder and 3-6 parts of hexagonal-phase boron nitride two-dimensional nanosheet powder into a colloidal palladium activating solution to perform palladium activating treatment; adding diamond powder subjected to palladium activation treatment and hexagonal-phase boron nitride two-dimensional nanosheet powder into a chemical plating solution in unit volume, wherein the chemical plating solution contains nickel salt and hypophosphite; stirring the electroless plating solution added with the diamond powder and the hexagonal-phase boron nitride two-dimensional nanosheet powder; and after stirring, filtering the chemical plating to obtain filter residues, and washing and drying the filter residues to obtain the diamond containing the metal-ceramic composite plating layer. The invention also provides a diamond containing the metal-ceramic composite coating. The diamond coating provided by the invention has high hardness.

Description

Diamond containing metal-ceramic composite coating and preparation method thereof
Technical Field
The invention relates to the technical field of diamond grinding tools, in particular to a diamond containing a metal-ceramic composite coating and a preparation method thereof.
Background
In the diamond grinding tool, because the diamond is a compact covalent bond structure and has high surface energy, the diamond is difficult to form good infiltration with base materials such as resin, metal and the like, the diamond abrasive particles and the bonding agent are only mechanically bonded, the bonding strength is low, and the diamond is easy to fall off in the grinding process.
In order to improve the bonding strength between the bonding agent and the diamond abrasive, researchers in the industry have been dedicated to modifying the surface of diamond, and the most common method is to coat a thin film of metal such as nickel, copper, etc. on the surface of the diamond abrasive (also called as diamond surface metallization). In addition, diamond is a brittle material, and certain crystal defects, coating impurities and the like exist on the surface and inside of diamond abrasive grains due to production and processing. The defects are more in low-grade grinding materials, so that the impact strength is lower, and the grinding materials are easy to break in the grinding process to lose the grinding function. The abrasive particles are wrapped by relatively tough metal coatings and the like to make up for surface defects, so that the impact resistance of the abrasive particles can be improved to a certain extent, and the service life of the abrasive tool is prolonged, which is particularly important for the abrasive tool made of resin bonding agent. During high-temperature grinding, the coating can also isolate and protect the diamond, reduce the erosion of oxidation and chemical reaction and further prolong the service life of the grinding tool.
However, the hardness of the existing metal-coated diamond still needs to be improved, i.e. the hardness of the metal-coated diamond is lower.
The above is only for the purpose of assisting understanding of the technical aspects of the present invention, and does not represent an admission that the above is prior art.
Disclosure of Invention
The invention mainly aims to provide a diamond containing a metal-ceramic composite coating and a preparation method thereof, and aims to solve the problem of low hardness of the diamond of a metal coating.
In order to achieve the object of the present invention, the present invention provides a method for preparing a diamond containing a metal-ceramic composite coating layer, the method comprising the steps of:
respectively putting 60-200 parts of diamond powder and 3-6 parts of hexagonal-phase boron nitride two-dimensional nanosheet powder into a colloidal palladium activating solution to perform palladium activating treatment;
adding the diamond powder subjected to palladium activation treatment and the hexagonal-phase boron nitride two-dimensional nanosheet powder into a chemical plating solution in unit volume, wherein the chemical plating solution contains nickel salt and hypophosphite;
stirring the electroless plating solution added with the diamond powder and the hexagonal-phase boron nitride two-dimensional nanosheet powder;
and after stirring, filtering the chemical plating to obtain filter residues, and washing and drying the filter residues to obtain the diamond containing the metal-ceramic composite plating layer.
In one embodiment, in the stirring process of the electroless plating, the stirring speed is 120r/min to 240r/min, the pH value of the electroless plating is 4.5 to 4.7, and the temperature of the electroless plating is 94 ℃ to 98 ℃.
In one embodiment, the stirring of the electroless plating is stopped when the stirring time is 13-17 min.
In one embodiment, the content of the nickel salt is 0.114 mol/L-0.304 mol/L, and the content of the hypophosphite is 0.484 mol/L-1.130 mol/L.
In one embodiment, the electroless plating solution further comprises a complexing agent, a stabilizer and a wetting agent, wherein the content of the complexing agent is 36-43 g/L, the content of the stabilizer is 16.5-23 mg/L, and the content of the wetting agent is 5-10 mg/L.
In one embodiment, the complexing agent comprises at least one of succinic acid, lactic acid, malic acid and glycine, the stabilizer is at least one of thiourea, potassium iodate and maleic acid, the hypophosphite is sodium hypophosphite monohydrate, and the nickel salt is nickel sulfate hexahydrate.
In an embodiment, before the step of performing palladium activation treatment on the diamond powder and the hexagonal phase boron nitride two-dimensional nanosheet powder, the preparation method further comprises the step of preparing the hexagonal phase boron nitride two-dimensional nanosheet powder, wherein the preparation method comprises the following steps:
weighing lithium tetraborate, sodium azide and magnesium as raw materials, and mixing to obtain a mixed material, wherein the molar ratio of the lithium tetraborate to the sodium azide to the magnesium is 1-1.5: 3-5: 4-7;
placing the mixed material in a high-temperature reaction kettle for sealing, and placing the sealed high-temperature reaction kettle into a muffle furnace for reaction to obtain an intermediate material;
soaking and stirring the washed intermediate material with hydrochloric acid, wherein the hydrochloric acid content in the hydrochloric acid solution is 17-19% in the soaking process of the intermediate material;
and after stirring, carrying out suction filtration, cleaning and drying on the intermediate material soaked in the hydrochloric acid to obtain hexagonal-phase boron nitride two-dimensional nanosheet powder.
In an embodiment, before the step of performing palladium activation treatment on the diamond powder and the hexagonal-phase boron nitride two-dimensional nanosheet powder, the method further includes the step of preparing a colloidal palladium activation solution, and the preparing of the colloidal palladium activation solution includes the following steps:
adding 65-70 g of tin chloride dihydrate and 6-8 g of sodium stannate heptahydrate into concentrated hydrochloric acid for dissolving to obtain a solution A, wherein the concentration of hydrochloric acid in the concentrated hydrochloric acid is 36-38%;
adding 0.9-1.1 g of palladium chloride and 2.5-2.6 g of tin chloride dihydrate into the concentrated hydrochloric acid for dissolving to obtain a solution B;
and adding the solution A into the solution B to obtain a mixed solution, and adding deionized water to 1L after heating the mixed solution in a water bath and stirring to obtain the colloidal palladium activating solution.
In one embodiment, the step of adding the solution a to the solution B comprises:
and adding the solution A into the solution B when the solution B is stirred for 11-13 min, wherein when the concentrated hydrochloric acid starts to be added with solid, the concentrated hydrochloric acid is stirred, and the solid is at least one of the palladium chloride and the tin chloride dihydrate.
In order to achieve the above object, the present invention also provides a diamond containing a metal-ceramic composite coating layer, which is prepared by the above method for preparing a diamond containing a metal-ceramic composite coating layer.
The embodiment of the invention provides a diamond containing a metal-ceramic composite coating and a preparation method thereof, which comprises the steps of respectively putting 60-200 parts of diamond powder and 3-6 parts of hexagonal phase boron nitride two-dimensional nanosheet powder into a colloidal palladium activating solution, performing palladium activation treatment, adding the diamond powder subjected to palladium activation treatment and hexagonal phase boron nitride two-dimensional nanosheet powder into the chemical plating solution with unit volume, stirring, after stirring is finished, filtering the chemical plating to obtain filter residue, washing and drying the filter residue to obtain the diamond containing the metal-ceramic composite plating layer, the hardness of the Ni-P-HBN coating of the diamond can reach 1100 HV-1300 HV, and exceeds the hardness of metal coatings such as an electroplated chromium coating, a Ni-P coating and the like, and the hardness of the coating of the diamond prepared by the method is higher.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
First, a brief overview of the method of producing the roof tile provided by the embodiments of the present invention is provided.
The production method of the roof decorative tile provided by the embodiment of the invention comprises the following steps:
1. weighing 60-200 parts of diamond powder and 3-6 parts of hexagonal phase boron nitride two-dimensional nanosheet powder, wherein the granularity of the diamond powder is 60-400 meshes;
2. respectively adding the weighed diamond powder and hexagonal-phase boron nitride two-dimensional nanosheet powder into a colloidal palladium activating solution, wherein the colloidal palladium activating solution is immersed in the diamond powder and the hexagonal-phase boron nitride two-dimensional nanosheet powder, the temperature of the colloidal palladium activating solution is maintained between 18 ℃ and 30 ℃ in the immersion process, the colloidal palladium activating solution is slowly stirred, the colloidal palladium solution is filtered to obtain filter residues when the stirring time is 3min to 10min, the two filter residues are washed with water and then added into 10% diluted hydrochloric acid to be slowly stirred for dispergation, the dispergation process lasts for 30s to 60s, the temperature of the diluted hydrochloric acid is maintained between 40 ℃ and 45 ℃, and diamond containing mass palladium and hexagonal-phase boron nitride two-dimensional nanosheets are obtained after dispergation is finished;
3. measuring chemical plating solution with unit volume, wherein the unit volume is L when the part is g, the unit volume is 1000L when the part is 1000g, the chemical plating solution contains nickel salt and hypophosphite, the content of the nickel salt is 0.114-0.304 mol/L, the content of the hypophosphite is 0.484-1.130 mol/L, the chemical plating solution also contains 36-43 g/L of complexing agent, 16.5-23 mg/L of stabilizing agent and 5-10 mg/L of wetting agent, the complexing agent comprises at least one of succinic acid, lactic acid, malic acid and glycine, the stabilizing agent is at least one of thiourea, potassium iodate and maleic acid, the hypophosphite is sodium hypophosphite monohydrate, and the nickel salt is nickel sulfate hexahydrate; the nickel salt can also be nickel halide, and the hypophosphite can be sodium hypophosphite, potassium hypophosphite and the like;
4. adding diamond powder subjected to palladium activation treatment and hexagonal-phase boron nitride two-dimensional nanosheet powder into chemical plating solution in unit volume, stirring, wherein in the stirring process, the temperature of the chemical plating solution is maintained at 94-98 ℃, the stirring speed is 120-240 r/min, the pH value of the chemical plating solution is maintained at 4.5-4.7, and when the stirring time is 13-17 min, stopping stirring the chemical plating solution;
5. and filtering, washing and drying the chemical plating solution which is stopped stirring to obtain the diamond containing the metal-ceramic composite plating layer, wherein the plating layer is Ni-P-HBN.
According to the invention, a large number of palladium particles are deposited on the surfaces of diamond powder and hexagonal phase boron nitride two-dimensional nanosheet powder by adopting a colloidal palladium activation-sensitization technology, then codeposition of the hexagonal phase boron nitride (HBN) two-dimensional nanosheet powder and a nickel-phosphorus alloy on the surface of the diamond powder is realized by adopting a chemical plating technology, and finally the Ni-P-HBN metal-ceramic composite coating tightly combined with the diamond powder is prepared, wherein the hardness of the Ni-P-HBN can reach 1100 HV-1300 HV, and exceeds the hardness of metal coatings such as electroplated chromium, Ni-P and the like, meanwhile, as the coating of the diamond prepared by the invention contains a non-metal material, compared with the diamond of a metal coating, the heat conduction performance is poorer, and in the high-temperature grinding process, the Ni-P-HBN can better isolate high temperature to protect the diamond, and reduce the oxidation of the diamond and the erosion of chemical reaction, the service life of the grinding tool prepared by the diamond is prolonged.
In addition, the invention adopts an environment-friendly chemical plating solution formula, has simple and safe operation and high plating efficiency, and can complete plating within 15 min.
In one embodiment, hexagonal phase boron nitride two-dimensional nanoplate powder is purchased directly; in this embodiment, a method for preparing hexagonal phase boron nitride two-dimensional nanosheet powder is provided, where the method for preparing hexagonal phase boron nitride two-dimensional nanosheet powder includes the following steps:
A. weighing lithium tetraborate (Li)2B4O7) Sodium azide (NaN)3) The metal magnesium powder (Mg) is used as a raw material, and the molar ratio of lithium tetraborate to sodium azide to the metal magnesium powder is (1-1.5): (3-5): (4-7), mixing and stirring lithium tetraborate, sodium azide and metal magnesium powder to obtain a mixed material with various uniformly distributed raw materials;
B. placing the mixed materials in a high-temperature reaction kettle, sealing the high-temperature reaction kettle in which the mixed materials are placed, then placing the sealed high-temperature reaction kettle in a muffle furnace for reaction, controlling the muffle furnace to heat up to 500-600 ℃ at the heating rate of 8-12 ℃/min, keeping the temperature of the muffle furnace for 16-24 h, taking out the high-temperature reaction kettle, and obtaining an intermediate material after natural cooling;
C. sequentially washing the intermediate material by adopting absolute ethyl alcohol and deionized water, then putting the washed intermediate material into a hydrochloric acid solution for soaking, and stirring in the soaking process, wherein the hydrochloric acid content in the hydrochloric acid solution is kept between 17 and 19 percent;
D. and when the stirring time is 4-6 hours, stopping stirring, performing suction filtration on the hydrochloric acid solution to obtain a suction filtration product, cleaning the suction filtration product with absolute ethyl alcohol for 3-4 times, then placing the cleaned suction filtration product in a vacuum drying oven for drying, wherein the drying condition is 75-85 ℃, the drying time is 8-10 hours, and obtaining the hexagonal-phase boron nitride two-dimensional nanosheet powder after the drying is finished.
In this example, the production cost of diamond containing a metal-ceramic composite coating can be reduced by self-producing hexagonal phase boron nitride two-dimensional nano particles.
Further, the colloidal palladium activation solution has time-efficiency, and therefore, the colloidal palladium activation solution needs to be prepared immediately, and in this embodiment, the colloidal palladium solution is prepared as follows:
Figure GDA0002967426450000061
firstly, 100mL of concentrated hydrochloric acid is taken, and 65g to 70g of SnCl is weighed2·2H2Adding O into 100mL concentrated hydrochloric acid, continuously stirring until the O is completely dissolved, and adding 6 g-7 g of Na2SnO3·7H2After O, uniformly stirring to obtain solution A;
then, 0.9g to 1.1g of PdCl2Adding 200mL concentrated hydrochloric acid, stirring until the concentrated hydrochloric acid is completely dissolved, and then adding 2.5-2.6 g SnCl into the mixture at the temperature of 30 +/-5 ℃ under the condition of continuous stirring2·2H2O, obtaining liquid B;
PdCl was added to 200mL of concentrated hydrochloric acid2Starting to time to obtain stirring time (when solid is added into the hydrochloric acid solution, the hydrochloric acid solution is stirred), and slowly adding the solution B into the solution B when the stirring time reaches 11-13 min to obtain a colloidal palladium solution;
and (3) placing the colloidal palladium solution in a water bath environment, heating and stirring, keeping the water bath temperature at 40-50 ℃, and adding deionized water to 1L after stirring for 2.5-3.5 h to obtain the colloidal palladium activating solution.
It should be noted that the purity of the above raw materials is analytically pure, the material of the reactor used in the step of chemically plating the diamond and the hexagonal phase boron nitride two-dimensional nanosheet is high molecular weight polyethylene, the stirring paddle is polytetrafluoroethylene, and the pH of the solution is adjusted by using 10% dilute hydrochloric acid and 10% NaOH solution.
Example 1
The method comprises the following steps: preparation of hexagonal phase boron nitride two-dimensional nanosheet
33.80g of lithium tetraborate (Li)2B4O7) 39.00g of sodium azide (NaN)3) Ball-milling and uniformly mixing 19.20g of 400-mesh metal magnesium powder (Mg), placing the mixture into a 500mL stainless steel high-temperature reaction kettle, sealing the stainless steel high-temperature reaction kettle, placing the sealed stainless steel high-temperature reaction kettle into a muffle furnace, heating the mixture to 500 ℃ at the speed of 10 ℃/min, preserving the heat for 18 hours, and naturally cooling the mixture to room temperature after the reaction is finished;
taking out the product (intermediate material) in the cooled high-temperature reaction kettle, washing the intermediate material for 4 times by absolute ethyl alcohol and deionized water in sequence, and then washing the intermediate material by using a washing machine 1:1, soaking in a hydrochloric acid solution (the hydrochloric acid content in the hydrochloric acid solution is 17 percent in a ratio of 1: 1) and stirring for 4 hours, monitoring the hydrochloric acid content in the soaking period, and supplementing the hydrochloric acid solution in time to keep the hydrochloric acid content in the hydrochloric acid solution at 17 to 19 percent;
and after stirring, carrying out suction filtration to obtain a suction filtration product, washing the suction filtration product for 3 times by using absolute ethyl alcohol, and drying the cleaned suction filtration product in a vacuum drying oven at 80 ℃ for 10 hours to obtain a white powdery hexagonal phase boron nitride (HBN) two-dimensional nanosheet.
Step two: activation treatment of powder surface colloid palladium
70g of SnCl2·2H2O is added into 100mL concentrated hydrochloric acid, stirring is continuously carried out until the O is completely dissolved, and 7g of Na is added2SnO3·7H2After O, uniformly stirring to obtain solution A;
1g of PdCl2Adding into 200mL concentrated hydrochloric acid, stirring to dissolve completely, adding 2.54g SnCl at 30 + -5 deg.C under stirring2·2H2And O, obtaining a liquid B. SnCl is added from the B liquid2·2H2And (3) starting timing, stirring the solution B for 12min, immediately and slowly pouring the solution A into the solution B, heating the prepared colloidal palladium solution in a water bath at the temperature of 45 +/-5 ℃, stirring for 3h, and then adding deionized water to 1L to obtain the colloidal palladium activation solution.
Step three: activation of diamond powder and hexagonal-phase boron nitride two-dimensional nanosheet powder
Adding 60g of 120-mesh diamond powder and 3g of hexagonal-phase boron nitride two-dimensional nanosheet into a colloidal palladium activating solution at 30 ℃, slowly stirring, filtering the powder after 5min, washing with water, immersing into a 10% dilute hydrochloric acid solution at 40 ℃, slowly stirring for 60s for dispergation, and filtering to complete activation.
Step four: electroless plating
Placing the diamond powder and the hexagonal-phase boron nitride two-dimensional nanosheet which are subjected to dispergation in chemical plating solution for chemical plating, wherein the chemical plating solution comprises the following formula: 45g/L of nickel sulfate hexahydrate, 80g/L of sodium hypophosphite monohydrate, 12g/L of succinic acid, 12g/L of lactic acid, 8g/L of malic acid, 5g/L of glycine, 0.5mg/L of thiourea, 10mg/L of potassium iodate, 5mg/L of maleic acid and 2g/L of polyethylene glycol. In the plating process, the temperature of the plating solution is adjusted to 95 ℃, the pH value is 4.5-4.7, the stirring speed is 180r/min, and the reaction time is 15 min; and filtering, washing and drying after the plating to obtain the diamond powder with the Ni-P-HBN metal-ceramic composite plating layer plated on the surface, wherein the hardness of the plating layer reaches 1100Hv +/-40 Hv.
Example 2
The method comprises the following steps: preparation of hexagonal phase boron nitride two-dimensional nanosheet
119.40g of lithium tetraborate (Li)2B4O7) 325.00g of sodium azide (NaN)3) And 170.10g of 400-mesh metal magnesium powder (Mg) are uniformly mixed by ball milling, then the mixture is placed in a 500mL stainless steel high-temperature reaction kettle, the sealed mixture is placed in a muffle furnace, the temperature is raised to 600 ℃ at the speed of 10 ℃/min, the temperature is kept for 18 hours, and after the reaction is finished, the mixture is naturally cooled to room temperature.
Taking out the product (intermediate material) in the cooled high-temperature reaction kettle, washing the intermediate material for 4 times by absolute ethyl alcohol and deionized water in sequence, and then washing the intermediate material by using a washing machine 1:1, soaking in a hydrochloric acid solution (the hydrochloric acid content in the hydrochloric acid solution is 17 percent in a ratio of 1: 1) and stirring for 4 hours, monitoring the hydrochloric acid content in the soaking period, and supplementing the hydrochloric acid solution in time to keep the hydrochloric acid content in the hydrochloric acid solution at 17 to 19 percent;
and after stirring, carrying out suction filtration to obtain a suction filtration product, washing the suction filtration product for 3 times by using absolute ethyl alcohol, and drying the cleaned product in a vacuum drying oven at 80 ℃ for 10 hours to obtain a white powdery hexagonal phase boron nitride (HBN) two-dimensional nanosheet.
Step two: activation treatment of powder surface colloid palladium
70g of SnCl2·2H2O is added into 100mL concentrated hydrochloric acid, stirring is continuously carried out until the O is completely dissolved, and 7g of Na is added2SnO37H2O, and uniformly stirring to obtain solution A;
1g of PdCl2Adding into 200mL concentrated hydrochloric acid, stirring to dissolve completely, adding 2.54g SnCl at 30 + -5 deg.C under stirring2·2H2And O, obtaining a liquid B. SnCl is added from the B liquid2·2H2And (3) starting timing, stirring the solution B for 12min, immediately and slowly pouring the solution A into the solution B, heating the prepared colloidal palladium solution in a water bath at the temperature of 45 +/-5 ℃, stirring for 3h, and then adding deionized water to 1L to obtain the colloidal palladium activation solution.
Step three: activation of diamond powder and hexagonal-phase boron nitride two-dimensional nanosheet powder
Adding 180g of 240-mesh diamond powder and 6g of hexagonal-phase boron nitride two-dimensional nanosheets into a colloidal palladium activating solution at 30 ℃, slowly stirring, filtering the powder after 5min, washing with water, immersing into a 10% dilute hydrochloric acid solution at 40 ℃, slowly stirring for 60s for dispergation, and filtering to complete activation.
Step four: electroless plating
Placing the diamond powder and the hexagonal-phase boron nitride two-dimensional nanosheet which are subjected to dispergation in chemical plating solution for chemical plating, wherein the chemical plating solution comprises the following formula: 60g/L of nickel sulfate hexahydrate, 120g/L of sodium hypophosphite monohydrate, 15g/L of succinic acid, 14g/L of lactic acid, 8g/L of malic acid, 6g/L of glycine, 1mg/L of thiourea, 10mg/L of potassium iodate, 10mg/L of maleic acid and 3.5g/L of polyethylene glycol. In the plating process, the temperature of the plating solution is adjusted to 95 ℃, the pH value is 4.5-4.7, the stirring speed is 240r/min, and the reaction time is 15 min. And filtering, washing and drying after the plating to obtain the diamond powder with the Ni-P-HBN metal-ceramic composite plating layer plated on the surface, wherein the hardness of the plating layer reaches 1300Hv +/-60 Hv.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or system that comprises the element.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalents and equivalent flow changes made by using the contents of the present specification, or applied directly or indirectly to other related technical fields are also included in the scope of the present invention.

Claims (10)

1. A method for preparing diamond containing a metal-ceramic composite coating is characterized by comprising the following steps:
respectively putting 60-200 parts of diamond powder and 3-6 parts of hexagonal-phase boron nitride two-dimensional nanosheet powder into a colloidal palladium activating solution to perform palladium activating treatment;
adding the diamond powder subjected to palladium activation treatment and the hexagonal-phase boron nitride two-dimensional nanosheet powder into a chemical plating solution in unit volume, wherein the chemical plating solution contains nickel salt and hypophosphite;
stirring the electroless plating solution added with the diamond powder and the hexagonal-phase boron nitride two-dimensional nanosheet powder;
and after stirring, filtering the chemical plating solution to obtain filter residues, and washing and drying the filter residues to obtain the diamond containing the metal-ceramic composite coating.
2. A method for preparing a diamond containing a metal-ceramic composite coating according to claim 1, wherein the stirring speed of the electroless plating solution is 120r/min to 240r/min during the stirring process, the pH of the electroless plating solution is 4.5 to 4.7, and the temperature of the electroless plating solution is 94 to 98 ℃.
3. A method for producing diamond containing a metal-ceramic composite coating layer according to claim 1, wherein stirring of the electroless plating solution is stopped when the stirring time is 13 to 17 min.
4. The method for preparing diamond containing metal-ceramic composite coating according to claim 1, wherein the content of the nickel salt is 0.114mol/L to 0.304mol/L, and the content of the hypophosphite is 0.484mol/L to 1.130 mol/L.
5. A method for preparing a diamond containing metal-ceramic composite coating according to claim 4, wherein the electroless plating solution further comprises a complexing agent, a stabilizer and a wetting agent, wherein the content of the complexing agent is 36 g/L-43 g/L, the content of the stabilizer is 16.5 mg/L-23 mg/L, and the content of the wetting agent is 5 mg/L-10 mg/L.
6. The method of claim 5, wherein the complexing agent comprises at least one of succinic acid, lactic acid, malic acid, and glycine, the stabilizer is at least one of thiourea, potassium iodate, and maleic acid, the hypophosphite is sodium hypophosphite monohydrate, and the nickel salt is nickel sulfate hexahydrate.
7. The method for preparing diamond containing a metal-ceramic composite coating according to any one of claims 1 to 6, further comprising, before the step of subjecting the diamond powder and the hexagonal phase boron nitride two-dimensional nanoplate powder to palladium activation treatment, the preparation of hexagonal phase boron nitride two-dimensional nanoplate powder comprising the steps of:
weighing lithium tetraborate, sodium azide and magnesium as raw materials, and mixing to obtain a mixed material, wherein the molar ratio of the lithium tetraborate to the sodium azide to the magnesium is 1-1.5: 3-5: 4-7;
placing the mixed material in a high-temperature reaction kettle for sealing, and placing the sealed high-temperature reaction kettle into a muffle furnace for reaction to obtain an intermediate material;
soaking and stirring the washed intermediate material with hydrochloric acid, wherein the hydrochloric acid content in the hydrochloric acid solution is 17-19% in the soaking process of the intermediate material;
and after stirring, carrying out suction filtration, cleaning and drying on the intermediate material soaked in the hydrochloric acid to obtain hexagonal-phase boron nitride two-dimensional nanosheet powder.
8. The method for preparing diamond containing a metal-ceramic composite coating according to any one of claims 1 to 6, further comprising, before the step of subjecting the diamond powder and the hexagonal-phase boron nitride two-dimensional nanoplate powder to palladium activation treatment, the preparation of a colloidal palladium activation solution, the preparation of the colloidal palladium activation solution comprising the steps of:
adding 65-70 g of tin chloride dihydrate and 6-8 g of sodium stannate heptahydrate into concentrated hydrochloric acid for dissolving to obtain a solution A, wherein the concentration of hydrochloric acid in the concentrated hydrochloric acid is 36-38%;
adding 0.9-1.1 g of palladium chloride and 2.5-2.6 g of tin chloride dihydrate into the concentrated hydrochloric acid for dissolving to obtain a solution B;
and adding the solution A into the solution B to obtain a mixed solution, and adding deionized water to 1L after heating the mixed solution in a water bath and stirring to obtain the colloidal palladium activating solution.
9. A method of producing diamond containing a metal-ceramic composite coating according to claim 8, wherein the step of adding the solution a to the solution B comprises:
and adding the solution A into the solution B when the solution B is stirred for 11-13 min, wherein when the concentrated hydrochloric acid starts to be added with solid, the concentrated hydrochloric acid is stirred, and the solid is at least one of the palladium chloride and the tin chloride dihydrate.
10. A diamond containing a metal-ceramic composite coating layer, characterized in that the diamond containing a metal-ceramic composite coating layer is prepared by the method for preparing a diamond containing a metal-ceramic composite coating layer according to any one of claims 1 to 9.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105058248A (en) * 2015-08-04 2015-11-18 蓬莱市超硬复合材料有限公司 Compound metal and ceramic bonding agent diamond grinding wheel
CN107974141A (en) * 2017-12-14 2018-05-01 云浮华云创新设计有限公司 A kind of nano-material modified fluorocarbon resin class stone material water-repellent paint and preparation method thereof
CN108823553A (en) * 2018-07-25 2018-11-16 芜湖昌菱金刚石工具有限公司 A kind of preparation method of diamond surface Electroless Ni-P Plating
CN108914096A (en) * 2018-07-25 2018-11-30 芜湖昌菱金刚石工具有限公司 A kind of preparation method of diamond surface cladding Ni-W-P metallization coating

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105058248A (en) * 2015-08-04 2015-11-18 蓬莱市超硬复合材料有限公司 Compound metal and ceramic bonding agent diamond grinding wheel
CN107974141A (en) * 2017-12-14 2018-05-01 云浮华云创新设计有限公司 A kind of nano-material modified fluorocarbon resin class stone material water-repellent paint and preparation method thereof
CN108823553A (en) * 2018-07-25 2018-11-16 芜湖昌菱金刚石工具有限公司 A kind of preparation method of diamond surface Electroless Ni-P Plating
CN108914096A (en) * 2018-07-25 2018-11-30 芜湖昌菱金刚石工具有限公司 A kind of preparation method of diamond surface cladding Ni-W-P metallization coating

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