CN111763931A - Preparation method of nickel-plated glass microspheres and product - Google Patents
Preparation method of nickel-plated glass microspheres and product Download PDFInfo
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- CN111763931A CN111763931A CN202010682990.7A CN202010682990A CN111763931A CN 111763931 A CN111763931 A CN 111763931A CN 202010682990 A CN202010682990 A CN 202010682990A CN 111763931 A CN111763931 A CN 111763931A
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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
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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
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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
- C23C18/18—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
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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
Abstract
The invention discloses a preparation method of nickel-plated glass microspheres, which is characterized by comprising the following steps: (1) adding the prepared glass microspheres into an ethanol solution of a silane coupling agent, stirring for 5-10 minutes, and filtering by using a filter screen; (2) drying at 60-80 ℃, adding into nickel acetate solution, stirring for 5-10 minutes to make nickel acetate adhere to the surface of the glass microsphere, and filtering with a filter screen again; (3) immersing the nickel acetate into an ethanol solution of sodium borohydride to reduce the nickel acetate, and quickly taking out after 30-60 seconds; (4) adding the solution into alkaline plating solution, stirring for 5-30 minutes to ensure that the plating layer is uniform to reach the set thickness, and then filtering; (5) drying at 80-90 ℃ to obtain the nickel-plated glass microspheres with uniform nickel plating on the surfaces. The invention also discloses the nickel-plated glass microsphere prepared by the method, wherein a layer of chemical nickel plating layer is uniformly, completely and continuously covered on the surface of the glass microsphere, and the plating layer is thicker, uniform and continuous and has good adhesive force.
Description
Technical Field
The invention relates to the technical field of chemical nickel-plating materials, in particular to a preparation method of nickel-plated glass microspheres and a product.
Background
The glass beads (containing hollow glass beads) have low density and stable chemical properties, and can replace pure metal powder with high density, poor dispersibility and easy sedimentation after plating metal on the surface of the glass beads, so that the glass beads are used for electromagnetic shielding materials or conductive and heat-conductive fillers, and the cost is reduced. But since ordinary glass is an amorphous stateSolid, the surface has no catalytic activity, and the conventional chemical plating process can not react on the surface spontaneously. Generally, a layer of active material is first coated on the surface of the glass to serve as a catalytic active center. PdCl is mostly adopted in the traditional process2-SnCl2The method uses palladium metal for activation, which is expensive and causes great environmental pollution, so that the method is especially important for finding a more economic and environment-friendly activation method.
The chemical nickel plating method disclosed in the Chinese patent application CN105731819A needs to be processed in a muffle furnace with high temperature of 170 ℃, and then the chemical plating process is 80-85 ℃; the chemical nickel plating method disclosed in CN104086086A requires treatment in a muffle furnace at a high temperature of 170 ℃ and activation with hydrofluoric acid at a concentration of 10-30 wt% in an ultrasonic field; the chemical nickel plating method disclosed in CN108220928A requires the use of hot sulfuric acid for sensitization, and the chemical plating process is performed at 80 ℃.
The prior art has the defects of complex activation process, high temperature, complex overall process steps, high material cost, difficult application to industrial production and the like; meanwhile, the nickel plating layer of the prepared nickel (hollow) plated glass beads is uneven, thin and small in adhesive force, and when the nickel plating layer is applied to heat conduction, electric conduction, electromagnetic shielding and other purposes, the performance of the nickel (hollow) plated glass beads is greatly limited, and the nickel (hollow) plated glass beads cannot meet the requirements frequently.
Disclosure of Invention
The invention aims to provide a preparation method of nickel-plated glass microspheres aiming at the defects in the prior art, the invention adopts a surface chemical nickel plating method, utilizes a coupling agent to enhance the adhesive capacity of a metal coating on the surfaces of the glass microspheres, then prepares a set amount of active nickel on the surfaces of the glass microspheres as an active center, prepares a nickel coating with good adhesive force, thicker and uniform coating after the glass microspheres are treated in an alkaline plating solution containing nickel sulfate, and has simple steps and easy industrialization.
The invention also provides the nickel-plated glass microsphere prepared by the method, and the nickel-plated glass microsphere has the advantages of thick, uniform and continuous plating layer, good adhesive force, excellent heat conduction, electric conduction, electromagnetic shielding, machining and other performances.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the nickel-plated glass microspheres is characterized by comprising the following steps of:
(1) adding the prepared glass microspheres into an ethanol solution containing a silane coupling agent, stirring for 5-10 minutes, and filtering by using a filter screen;
(2) drying at 60-80 ℃, adding into nickel acetate solution, stirring for 5-10 minutes to make nickel acetate adhere to the surface of the glass microsphere, and filtering with a filter screen again;
(3) immersing the glass microspheres into an ethanol solution containing sodium borohydride, reducing the nickel acetate, and quickly taking out the glass microspheres after 30-60 seconds to obtain the glass microspheres with 3-5 mu m active nickel layers attached to the surfaces;
(4) adding the nickel-base composite material into an alkaline plating solution containing nickel sulfate, sodium citrate and sodium hypophosphite, stirring for 5-30 minutes, enabling an active nickel layer to automatically initiate chemical nickel-plating reaction, enabling a plating layer to be uniform and reach;
(5) drying at 80-90 ℃ to obtain the nickel-plated glass microspheres with uniform nickel plating on the surfaces.
The glass microspheres are solid or hollow glass microspheres, and the diameter of the glass microspheres is 40-50 mu m.
The thickness of the nickel plating layer is set to be 20-25 mu m.
The silane coupling agent in the step (1) is KH 791; the content of the silane coupling agent in the ethanol solution is 10-50 g/L.
The concentration of the nickel acetate solution in the step (2) is 30-50g/L, wherein the ethanol is absolute ethanol with the purity of 95%.
The concentration of the ethanol solution of the sodium borohydride in the step (3) is 2-8g/L, wherein the ethanol has the purity of 95%.
In the alkaline plating solution in the step (4), the solutes are nickel sulfate, sodium citrate and sodium hypophosphite, the solvent is deionized water, the neutralizing alkali is ammonia water, the ph range is 9-10, and the temperature is 40-50 ℃.
The alkaline plating solution in the step (4) comprises the following components in percentage by mass: nickel sulfate: sodium citrate: sodium hypophosphite: the deionized water is alkaline plating solution, and the mass ratio of each component is as follows: nickel sulfate: sodium citrate: sodium hypophosphite: 25-50 parts of deionized water, 4-10 parts of deionized water, 16-30 parts of deionized water and 1000 parts of deionized water.
The filter screens in all the steps are 400-mesh nylon screens.
The nickel-plated glass microsphere prepared by the method is characterized in that a chemical nickel-plating layer is uniformly, completely and continuously covered on the surface of the glass microsphere, the hardness of the nickel-plating layer is 7-8H, the thickness of the nickel-plating layer is 20-25 mu m, and the adhesive force measured by a grid-scribing method is 2-3 grades.
The invention has the beneficial effects that:
(1) the method for plating the nickel glass microspheres comprises the steps of firstly treating the surfaces of the glass microspheres by using a silane coupling agent, then soaking the glass microspheres in an ethanol solution containing nickel acetate, and then reducing the glass microspheres by using a sodium borohydride solution to obtain the glass microspheres with active nickel layers attached to the surfaces; and finally, putting the glass microspheres into prepared alkaline plating solution containing nickel sulfate, and obtaining the nickel-plated glass microspheres with uniform nickel plating on the surface after the active nickel layer automatically initiates the subsequent nickel plating reaction. The method adopts surface chemical nickel plating, and has the advantages of concise activation process, lower temperature, concise overall process steps, low material cost and easy industrial production; meanwhile, the nickel plating layer of the prepared nickel (hollow) plated glass bead is complete and continuous, has uniform thickness, larger thickness and larger adhesive force, greatly improves the comprehensive performance, and has good heat conduction, electric conduction, electromagnetic shielding, machining and other properties.
(2) The invention mainly improves the pretreatment process in the chemical nickel plating process including the pretreatment (including activation, sensitization and the like) and the chemical plating process, and adopts nickel acetate and sodium borohydride to generate active nickel to replace the common complex activation process, so that the temperature is relatively low and the energy consumption is less in the nickel plating process; the active nickel layer is obtained by adopting a reduction method and then the chemical nickel plating process is initiated by the active nickel layer, so that the activation temperature is lower, the whole steps are simpler, and the control and the industrialization are easy.
(3) The invention introduces silane coupling agent to carry out surface pretreatment on the glass microsphere, on one hand, the invention can improve the fast adhesion of each liquid component on the surface of the glass microsphere and shorten the process treatment time, and on the other hand, the invention can increase the adsorption capacity of the surface of the glass microsphere to the metal nickel coating so as to lead the glass microsphere to reach the required thickness.
(4) The nickel-plated glass microsphere material provided by the invention has the diameter of 40-50 mu m, and the nickel-plated layer on the surface of the nickel-plated glass microsphere material has uniform and continuous thickness, uniform shape, good appearance consistency, thickness of 20-25 mu m, hardness of 7-8H, adhesive force of 2-3 grades, good heat conduction, electric conduction and electromagnetic shielding performances and low weight density; the material can be widely applied to the fields of anti-interference, corrosion resistance, wear resistance, high heat conduction, high electric conduction, high electromagnetic loss and the like, and has a wide application prospect.
The present invention will be described in further detail with reference to specific embodiments.
Detailed Description
The invention provides a preparation method of nickel-plated glass microspheres, which comprises the following steps:
(1) adding the prepared glass microspheres into an ethanol solution containing a silane coupling agent, stirring for 5-10 minutes, and filtering by using a filter screen;
(2) drying at 60-80 ℃, adding into nickel acetate solution, stirring for 5-10 minutes to make nickel acetate adhere to the surface of the glass microsphere, and filtering with a filter screen again;
(3) immersing the glass microspheres into an ethanol solution containing sodium borohydride, reducing the nickel acetate, and quickly taking out the glass microspheres after 30-60 seconds to obtain the glass microspheres with 3-5 mu m active nickel layers attached to the surfaces;
(4) adding the nickel-base composite material into an alkaline plating solution containing nickel sulfate, sodium citrate and sodium hypophosphite, stirring for 5-30 minutes, enabling an active nickel layer to automatically initiate chemical nickel-plating reaction, enabling a plating layer to be uniform and reach;
(5) drying at 80-90 ℃ to obtain the nickel-plated glass microspheres with uniform nickel plating on the surfaces.
The glass microspheres are solid or hollow glass microspheres, and the diameter of the glass microspheres is 40-50 mu m.
The thickness of the nickel plating layer is set to be 20-25 mu m.
The silane coupling agent in the step (1) is KH 791; the content of the silane coupling agent in the ethanol solution is 10-50 g/L.
The concentration of the nickel acetate solution in the step (2) is 30-50g/L, wherein the ethanol is absolute ethanol with the purity of 95%.
The concentration of the ethanol solution of the sodium borohydride in the step (3) is 2-8g/L, wherein the ethanol has the purity of 95%.
In the alkaline plating solution in the step (4), the solutes are nickel sulfate, sodium citrate and sodium hypophosphite, the solvent is deionized water, the neutralizing alkali is ammonia water, the ph range is 9-10, and the temperature is 40-50 ℃.
The alkaline plating solution in the step (4) comprises the following components in percentage by mass: nickel sulfate: sodium citrate: sodium hypophosphite: the deionized water is alkaline plating solution, and the mass ratio of each component is as follows: nickel sulfate: sodium citrate: sodium hypophosphite: 25-50 parts of deionized water, 4-10 parts of deionized water, 16-30 parts of deionized water and 1000 parts of deionized water.
The filter screens in all the steps are 400-mesh nylon screens.
The nickel-plated glass microsphere prepared by the method uniformly, completely and continuously covers a layer of chemical nickel-plating layer on the surface of the glass microsphere, the hardness of the nickel-plating layer is 7-8H, the thickness of the nickel-plating layer is 20-25 mu m, and the adhesive force measured by a grid-scribing method is 2-3 grades.
Specific example 1:
the preparation method of the nickel-plated glass microsphere provided by the embodiment of the invention adopts a surface chemical nickel plating process, and comprises the following steps:
(1) adding the solid glass microspheres into 50ml of 95% ethanol solution containing 2gKH791, stirring for 10 minutes, and filtering by using a 400-mesh nylon net;
(2) drying at 80 ℃, adding the dried mixture into 40g/L nickel acetate solution, stirring for 10 minutes, and filtering by using a 400-mesh nylon net again;
(3) immersing the glass microspheres into a 95% ethanol solution of 10g/L sodium borohydride to reduce the nickel acetate, and quickly taking out the glass microspheres after 40-60 seconds to obtain the glass microspheres with 3-5 mu m active nickel layers attached to the surfaces;
(4) adding the glass microspheres with the surface adhered with the active nickel layer of 3-5 mu m into alkaline plating solution containing 30g/L nickel sulfate, 5g/L sodium citrate and 20g/L sodium hypophosphite and having a ph of 9-10, stirring for 30 minutes at 45 ℃, filtering, automatically initiating chemical nickel plating reaction by the active nickel layer, enabling the plating layer to be uniform to reach a set thickness, and then filtering;
(5) and finally, drying at 80 ℃ to obtain the glass microspheres with nickel plated surfaces.
The nickel-plated glass microsphere prepared by the method is solid glass microsphere with the diameter of 40-50 mu m, the surface of the glass microsphere is uniformly, completely and continuously covered with a chemical nickel-plating layer, the hardness of the nickel-plating layer is 7-8H, the thickness of the nickel-plating layer is 20-25 mu m, and the adhesion force measured by a grid cutting method is 2-3 grades.
Specific example 2
This example provides a method for preparing nickel-plated glass microspheres and an article, which is substantially the same as example 1, except that the method comprises the following steps:
adding glass microspheres into 50ml of 95% ethanol solution containing 2g of KH791, stirring for 10 minutes, filtering with a 400-mesh nylon net, drying at 80 ℃, adding into 60g/L of nickel acetate solution, stirring for 10 minutes, filtering again with the 400-mesh nylon net, immersing into 10g/L of 95% ethanol solution of sodium borohydride, quickly taking out the glass microspheres after 1 minute, adding into an alkaline plating solution containing 25g/L of nickel sulfate, 4g/L of sodium citrate and 16g/L of sodium hypophosphite and having a ph of 9-10, stirring for 30 minutes at 45 ℃, filtering, and drying at 80 ℃ to obtain the glass microspheres with nickel plated surfaces.
Specific example 3
This example provides a method for preparing nickel-plated glass microspheres and articles, which are substantially the same as examples 1 and 2, except that the method comprises the following steps:
adding glass microspheres into 50ml of 95% ethanol solution containing 3gKH791, stirring for 10 minutes, filtering by using a 400-mesh nylon net, drying at 80 ℃, adding into 60g/L of nickel acetate solution, stirring for 10 minutes, filtering again by using the 400-mesh nylon net, immersing into 10g/L of 95% ethanol solution of sodium borohydride, quickly taking out the glass microspheres after 1 minute, adding into an alkaline plating solution containing 50g/L of nickel sulfate, 10g/L of sodium citrate and 30g/L of sodium hypophosphite and having a ph of 9-10, stirring for 30 minutes at 45 ℃, filtering, and drying at 80 ℃ to obtain the nickel-plated glass microspheres with uniform, continuous and firm surface coatings.
The invention provides a preparation method of nickel-plated glass microspheres, which belongs to the field of chemical nickel plating, and mainly adopts nickel acetate and sodium borohydride to generate active nickel to replace a common complex activation process, so that the reaction temperature is reduced, the process equipment is simplified, and the power consumption is reduced. Firstly, treating the glass microspheres by using a silane coupling agent to increase the adsorption capacity of the surfaces of the glass microspheres on various solute components and metal coatings; then dipping the glass microspheres in an ethanol solution containing nickel acetate, and reducing the dipped glass microspheres by using a sodium borohydride solution to obtain the glass microspheres with active nickel attached to the surfaces; and finally, putting the glass microspheres into prepared alkaline plating solution containing nickel sulfate, and reacting to obtain the nickel-plated glass microspheres with nickel plated on the surfaces. The method has the advantages of simple and easily-controlled steps and low cost, and can prepare the nickel coating with uniform and continuous thickness, good adhesive force and moderate hardness on the surface of the glass microsphere.
In the above examples of the present invention, the specific experimental procedures or conditions are not specified, and the procedures or conditions of the conventional experimental procedures described in the literature in the art can be performed. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The invention is not limited to the above embodiments, and other similar methods and products of nickel-plated glass microspheres obtained by the same or similar methods are adopted, and specific values, different material components for further improving the coating and functionalization, and the like are specifically selected from the value ranges of the components described in the embodiments of the invention, and are within the protection scope of the invention, and the embodiments of the invention are not listed.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements and the like that are made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the nickel-plated glass microspheres is characterized by comprising the following steps of:
(1) adding the prepared glass microspheres into an ethanol solution of a silane coupling agent, stirring for 5-10 minutes, and filtering by using a filter screen;
(2) drying at 60-80 ℃, adding into nickel acetate solution, stirring for 5-10 minutes to make nickel acetate adhere to the surface of the glass microsphere, and filtering with a filter screen again;
(3) immersing the glass microspheres into an ethanol solution of sodium borohydride to reduce nickel acetate, and quickly taking out the glass microspheres after 30-60 seconds to obtain the glass microspheres with the surface attached with an active nickel layer of 3-5 microns;
(4) adding the nickel-base composite oxide into an alkaline plating solution of nickel sulfate, sodium citrate and sodium hypophosphite, stirring for 5-30 minutes, automatically initiating a chemical nickel plating reaction by an active nickel layer, enabling the plating layer to be uniform to reach a set thickness, and then filtering;
(5) drying at 80-90 ℃ to obtain the nickel-plated glass microspheres with uniform nickel plating on the surfaces.
2. The method of claim 1, wherein the glass microspheres are solid or hollow glass microspheres having a diameter of 40 to 50 μm.
3. The method of claim 1, wherein the plating layer has a thickness of 20 to 25 μm.
4. The method according to claim 1, wherein the silane coupling agent in the step (1) is KH 791; the content of the silane coupling agent in the ethanol solution is 10-50 g/L.
5. The method according to claim 1, wherein the concentration of the nickel acetate solution in the step (2) is 30-50g/L, and the ethanol is 95% pure absolute ethanol.
6. The method according to claim 1, wherein the ethanol solution of sodium borohydride in the step (3) has a concentration of 2 to 8g/L, and the ethanol has a purity of 95%.
7. The method according to claim 1, wherein the alkaline plating solution in step (4) comprises the solutes of nickel sulfate, sodium citrate and sodium hypophosphite, the solvent is deionized water, the alkali for neutralization is ammonia water, the ph range is 9-10, and the temperature is 40-50 ℃.
8. The preparation method according to claim 7, wherein the alkaline plating solution in the step (4) comprises the following components in parts by mass: nickel sulfate: sodium citrate: sodium hypophosphite: 25-50 parts of deionized water, 4-10 parts of deionized water, 16-30 parts of deionized water and 1000 parts of deionized water.
9. The method according to claim 1, wherein the sieve used in each step is a 400 mesh nylon sieve.
10. A nickel-plated glass microsphere prepared by the method of any one of claims 1 to 9, wherein the surface of the glass microsphere is uniformly, completely and continuously covered with an electroless nickel plating layer, the nickel plating layer has a hardness of 7-8H and a thickness of 20-25 μm, and the adhesion measured by a cross-cut method is 2-3 grades.
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