CN113584547B - Preparation method of micro-nano metal particle surface coating - Google Patents
Preparation method of micro-nano metal particle surface coating Download PDFInfo
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- CN113584547B CN113584547B CN202110915225.XA CN202110915225A CN113584547B CN 113584547 B CN113584547 B CN 113584547B CN 202110915225 A CN202110915225 A CN 202110915225A CN 113584547 B CN113584547 B CN 113584547B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/006—Nanoparticles
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
Abstract
A preparation method of a micro-nano metal particle surface coating belongs to the field of surface engineering. The method comprises the following steps: selecting and configuring an electroplating solution to be electroplated, selecting micro-nano metal particles to be electroplated, removing surface oxide films from the selected micro-nano metal particles, mixing the micro-nano metal particles with a weakly acidic electroplating solution, adding the electroplating solution into an electroplating bath, adding a magnetic rotor into the electroplating bath to stir the electroplating solution, uniformly dispersing the micro-nano metal particles into the electroplating solution, keeping stirring not stopped in the electroplating process, turning on a micro-pump power supply to stably circulate the electroplating solution in a micro-tube, turning on an electroplating power supply to perform electroplating, completing electroplating after a certain time, and centrifugally drying the electroplated plating solution to obtain the micro-nano metal particles with good coatings. The invention can be applied to the solder balls in the electronic packaging field such as flip chip bonding, ball grid array packaging and the like, and has the advantages of low resistance, strong signal transmission capability, strong electromigration resistance, strong creep resistance and the like.
Description
Technical Field
The invention belongs to the field of surface engineering, and particularly relates to a preparation method of a micro-nano metal particle surface coating.
Background
With the continuous development and innovation of electronic packaging technology, the density of Integrated Circuits (ICs) is higher and higher, and the IC integration density and performance are further improved due to the appearance of Flip Chip bonding (Flip Chip), Ball Grid Array (BGA) and other technologies. Most of the high-density electronic packaging technologies include a ball-mounting process, i.e., a solder ball for connecting, transmitting signals, etc. is mounted on a pad. These solder balls are the most prone locations to failure and therefore have stringent performance requirements. For example: the metal copper has the advantages of low resistance, strong signal transmission capability, strong electromigration resistance, strong creep resistance and the like, and the metal tungsten has good high-temperature service performance and is an ideal material as solder ball brazing filler metal. However, the solder ball has the problems of high melting point, difficult diffusion, easy oxidation and the like, so that the solder ball is difficult to realize reliable connection when being directly used as a connecting material, and needs to be subjected to surface treatment to form a reliable metal layer which is easy to realize connection with a bonding pad on the surface of the metal solder ball. The metal layer on the surface of the solder ball is prepared by an electroplating method, and the traditional sedimentation method electroplating can cause the metal ball to grow on the surface of the cathode and the coating is not uniform. Therefore, a novel micro-nano metal particle surface plating technology needs to be developed to adapt to the application of flip chip bonding, ball grid array packaging and other technologies, so as to promote the development of electronic packaging technology.
Disclosure of Invention
The invention aims to solve the problem that a coating is difficult to form on the surface of the existing micro-nano metal particle, and provides a preparation method of the coating on the surface of the micro-nano metal particle, which utilizes electroplating to form the coating on the surface of the micro-nano metal particle by circulating a plating solution in a fluid system, thereby improving the utilization rate of the plating solution; the cathode is washed by controlling the flow rate of the plating solution, so that the phenomenon that metal particles grow on the cathode is avoided; by introducing multiple pairs of electrodes into the fluid system, the efficiency of electroplating is improved. Therefore, the process has the advantages of reliable micro-nano metal particle plating layer formation, high electroplating efficiency, high material utilization rate and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a micro-nano metal particle surface coating comprises the following specific steps:
the method comprises the following steps: selecting micro-nano metal particles to be electroplated, and removing an oxide film on the surfaces of the micro-nano metal particles;
step two: selecting and configuring a plating solution to be electroplated, and selecting and manufacturing an electroplated electrode;
step three: mixing the micro-nano metal particles obtained in the step one with the plating solution obtained in the step two;
step four: assembling an electroplating device, wherein the electroplating device specifically comprises an electroplating bath, a micro-flow tube, a micro-pump and a power supply; the micro flow pipe comprises a vertical section and a transition section; the vertical section is provided with a plurality of pairs of electrodes for electroplating and lead-out wires of the electrodes, the anode is tightly attached to the micro-flow tube in the vertical section of the micro-flow tube, and the included angle between the cathode facing the flow direction of the plating solution and the wall of the micro-flow tube is 10 degrees; a plurality of pairs of supporting structures are arranged on two sides of the top end of the electroplating bath and used for supporting the vertical section of the micro-flow tube; during assembly, at the inlet, the micro pump does not enter the liquid level, the micro pipe is led out from the micro pump and inserted into the liquid level, and plating solution is pumped; connecting an electrode power supply and an electrode, and a micro-pump power supply and a micro-pump by using a lead;
step five: adding the mixed solution of the micro-nano metal particles and the plating solution obtained in the third step into the plating tank obtained in the fourth step, and adjusting the micro-flow tube to enable the starting end of the micro-flow tube to be located 30mm below the liquid level of the plating solution and enable the tail end of the micro-flow tube not to enter the plating solution;
step six: adding a magnetic stirrer into the electroplating bath at a rotation speed of 1 × 103r/min, in the subsequent electroplating process, opening the magnetic stirring all the time;
step seven: turning on a micro-pump power supply to enable the mixed liquid of the micro-nano metal particles and the plating liquid to stably circulate in the micro-flow tube;
step eight: turning on an electroplating power supply, controlling the pressure applied by the micro pump, and controlling the flow rate of the plating solution in the micro tube to be 0.05-0.2 m/s to carry out electroplating, wherein the flowing direction of the plating solution is ensured to be the same as the direction in which the distance between the cathode and the anode is reduced in the electroplating process;
step nine: controlling the current density of electroplating to be 1-5A/dm2Electroplating for 5-20 min to obtain a complete high-quality coating, and completing electroplating;
step ten: turning off the electroplating power supply and magnetic stirring, lifting the micro-flow tube at the starting end position to exceed the liquid level of the plating solution, turning off the micro-pump power supply after the plating solution in the micro-flow tube completely flows into the electrolytic bath, and then turning off the electroplating power supply;
step eleven: and filtering or centrifuging the plating solution obtained in the step ten to obtain electroplated micro-nano metal particles.
Compared with the prior art, the invention has the beneficial effects that: the invention provides an electroplating method for introducing electrodes and circulating plating solution into a fluid system to form a plating layer on the surface of micro-nano metal particles, aiming at the problem that the micro-nano metal particle plating layer is difficult to form. Compared with the traditional sedimentation method, the technology has the advantages of avoiding the growth of micro-nano metal particles on the cathode, ensuring uniform plating, high electroplating efficiency, high material utilization rate and the like. The micro-nano metal particles with uniform and reliable plating layers formed by the technology can be used for welding balls in the electronic packaging field of flip chip bonding, ball grid array packaging and the like, and compared with common low-melting-point solid solution welding balls, the metal particle welding balls have the advantages of creep resistance, strong electromigration resistance, good high-temperature use performance, low resistance, high signal transmission efficiency and the like, the connection performance of pure metal and a welding pad is improved, and the integration density of an IC (integrated circuit) and the packaging reliability are greatly improved.
Drawings
FIG. 1 is a diagram of a structure of an electroplating bath with three pairs of support structures for micro flow tubes;
FIG. 2 is a view showing the structure of a micro flow tube;
FIG. 3 is a block diagram of the assembly of a plating bath, a micro-pump and a micro-fluidic tube;
FIG. 4 is a schematic view of a vertically oriented microchannel taken from FIG. 2;
FIG. 5 is a cross-sectional view of the microfluidic tube of FIG. 4 with a pair of electrodes and a lead-out wire diagram of the electrodes;
FIG. 6 is a diagram of a process of electroplating micro-nano metal particles in a micro-fluidic tube;
fig. 7 is a structural diagram of an overall device for electroplating micro-nano metal particles in a fluid device.
Detailed Description
The technical solution of the present invention is further described below with reference to the drawings and examples, but the present invention is not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention should be covered by the protection scope of the present invention.
The invention provides an electroplating method for forming a coating on the surface of micro-nano metal particles based on circulating plating solution in a fluid system. The invention can solve the problems that plating layers are difficult to form on the micro-nano metal particles and the plating layers are incomplete and the like, and improves the utilization rate of the plating solution by circulating the plating solution in the fluid system; the cathode is washed by controlling the flow rate of the plating solution, so that the phenomenon that metal particles grow on the cathode is avoided; by introducing multiple pairs of electrodes into the fluid system, the efficiency of electroplating is improved.
The invention is based on circulating plating solution in a fluid system, forms a plating layer on the surface of micro-nano metal particles, is used for processing the plating layer on the surface of a solder ball in the field of electronic packaging (such as flip chip bonding, ball grid array packaging and the like), can solve the problems that the plating layer is difficult to form on the micro-nano metal particles, the plating layer is incomplete and the like, and simultaneously expands the application field of the micro-nano metal particles, such as improving the weldability of the micro-nano metal particles so that the micro-nano metal particles can be applied to the bonding field of electronic packaging and the like.
The embodiment describes a method for forming a good coating on the surface of micro-nano metal particles by electroplating, and the micro-nano metal particles continuously wash a cathode at a specific speed by circulating a mixed solution of a plating solution and the micro-nano metal particles in a fluid system, so that the coating is formed on the surface of the micro-nano metal particles near the cathode.
The first embodiment is as follows: the embodiment describes a preparation method of a micro-nano metal particle surface coating, which comprises the following specific steps:
the method comprises the following steps: selecting micro-nano metal particles to be electroplated, and removing an oxide film on the surfaces of the micro-nano metal particles;
step two: selecting and configuring a plating solution to be electroplated, and selecting and manufacturing an electroplated electrode;
step three: mixing the micro-nano metal particles obtained in the step one with the plating solution obtained in the step two to prevent the micro-nano metal particles from being oxidized in the air;
step four: assembling an electroplating device, wherein the electroplating device specifically comprises an electroplating bath, a micro-flow tube, a micro-pump and a power supply; the microfluidic tube comprises a vertical section and a transition section, as shown in fig. 2; the vertical section is provided with a plurality of pairs of electrodes for electroplating and lead-out wires of the electrodes, and parameters such as the diameter of the micro-flow tube are selected according to specific electroplating; electroplating is carried out in the vertical direction, so that the accumulation of particles in the bent section in the electroplating process can be avoided as much as possible; in the vertical section of the micro-flow tube, the anode is tightly attached to the micro-flow tube, the included angle between the cathode facing the flow direction of the plating solution and the wall of the micro-flow tube is 10 degrees, the cathode and the anode are led out from the micro-flow tube by using a lead, and the screenshot of the front view surface is shown in figure 4; a plurality of pairs of supporting structures are arranged on two sides of the top end of the electroplating bath, as shown in figure 1, and are used for supporting the vertical section of the micro-flow tube; during assembly, at the inlet, the micro pump does not enter the liquid level, the micro pipe is led out from the micro pump and inserted into the liquid level, and plating solution is pumped, wherein the combined drawing is shown in figure 3; connecting an electrode power supply and an electrode, and a micro-pump power supply and a micro-pump by using a lead, wherein the structure diagram is shown in FIG. 7;
in the present invention, a micro pump is used to provide power for the flow of plating solution in the micro flow tube; the structure of the plating bath is shown in fig. 1, wherein two sides of the top of the plating bath are provided with support structures of the micro-flow tubes, the micro-pump and the micro-flow tubes are arranged on the plating bath, the starting end of each micro-flow tube is positioned 50mm below the support structure by adjusting the micro-flow tubes, the micro-pump is arranged above the starting end support structure, the tail end of each micro-flow tube and the support structure are kept horizontal, and the electrodes are positioned at the vertical positions of the micro-flow tubes. The combination diagram is shown in fig. 2.
Step five: adding the mixed solution of the micro-nano metal particles and the plating solution obtained in the third step into the plating tank obtained in the fourth step, and adjusting the micro-flow tube to enable the starting end of the micro-flow tube to be located 30mm below the liquid level of the plating solution and the tail end of the micro-flow tube not to enter the plating solution;
step six: adding a polytetrafluoroethylene magnetic stirrer (C type: 10 multiplied by 60 mm)2) At a rotation speed of 1X 103r/min, in the subsequent electroplating process, magnetic stirring is opened all the time, so that the micro-nano metal particles are uniformly dispersed in the plating solution;
step seven: turning on a power supply of a micropump (model: ZL12(24) -RZ1030-4) to ensure that the mixed solution of the micro-nano metal particles and the plating solution stably circulates in the micro-flow tube;
step eight: turning on an electroplating power supply, controlling the pressure applied by the micro pump to ensure that the flow velocity of the plating solution in the micro tube is 0.05-0.2 m/s, and electroplating, wherein the flowing direction of the plating solution is ensured to be the same as the direction in which the distance between the cathode and the anode is reduced in the electroplating process, as shown in fig. 6; the flow rate is controlled to ensure that the micro-nano metal particles in the plating solution stay near the cathode for a short time to carry out electroplating, and the micro-nano metal particles are prevented from growing at the cathode by the scouring of the plating solution.
Step nine: controlling the current density of electroplating to be 1-5A/dm2Electroplating for 5-20 min to obtain a complete high-quality coating, and completing electroplating;
step ten: turning off the electroplating power supply and magnetic stirring, lifting the micro-flow tube at the starting end position to exceed the liquid level of the plating solution, turning off the micro-pump power supply after the plating solution in the micro-flow tube completely flows into the electrolytic bath, and then turning off the electroplating power supply;
step eleven: and filtering or centrifuging the plating solution obtained in the step ten to obtain electroplated micro-nano metal particles.
The second embodiment is as follows: in a specific embodiment of a method for preparing a micro-nano metal particle surface coating, in the step one, the micro-nano metal particles to be electroplated are spherical particles with a diameter of 50nm to 10 μm, and the micro-nano metal particles are made of copper and other micro-nano metal particles with good conductivity.
The third concrete implementation mode: in a specific embodiment, in a plating solution circulation process, the preparation method of the micro-nano metal particle surface plating layer needs to ensure that the plating solution is kept in a continuous state without bubbles in a micro-flow tube.
The fourth concrete implementation mode: in a step eight, the flow rate of the plating solution in the microflow pipe is 0.1m/s, and the flow rate enables the micro-nano metal particles to stay at the cathode for a short time to complete the electroplating in the electroplating process, and the micro-nano metal particles cannot grow on the surface of the cathode and enter the plating solution due to the washing of water flow.
The fifth concrete implementation mode: in the ninth step of the method for preparing a micro-nano metal particle surface coating, the electroplating current is 2 to 4A/dm2The electroplating time is 10-18 min.
The sixth specific implementation mode: the method for preparing the micro-nano metal particle surface coating in the embodiment one further comprises the following steps: drying the micro-nano metal particles in a reducing or inert atmosphere.
Example 1: performing electrochemical nickel plating on the surfaces of the micro-nano copper particles:
the method comprises the following steps: and (4) preparing a nickel plating solution. Adding 1L of deionized water into a preparation tank with the volume of 2L, heating to 50 ℃, sequentially adding 120g of nickel sulfate, 8g of sodium chloride, 60g of sodium sulfate, 30g of magnesium sulfate and 140g of sodium citrate, and stirring until the nickel sulfate, the sodium chloride, the sodium sulfate, the magnesium sulfate and the sodium citrate are completely dissolved; adding 20g of boric acid into another container, adding a proper amount of water, heating to 80 ℃, stirring until the boric acid is completely dissolved, and adding the boric acid into a preparation tank; adding 0.1g of sodium dodecyl sulfate and a proper amount of warm water into another container, stirring until the sodium dodecyl sulfate and the warm water are completely dissolved, and adding the mixture into a preparation tank; and (3) adjusting the pH of the plating solution to 5.5 by using sodium hydroxide with the mass fraction of 3% and sodium sulfate with the mass fraction of 3% to complete the preparation.
Step two: selecting nano copper particles with the diameter of 1 mu m as micro-nano metal particles to be electroplated.
Step three: and removing the oxide on the surface of the copper particles selected in the second step by using dilute hydrochloric acid.
Step four: and (4) adding the copper particles obtained in the third step into the plating solution obtained in the first step.
Step five: selecting nickel plates with the mass fraction of sulfur of 0.01-0.015% as an anode and a cathode for electroplating.
Step six: a plurality of pairs of electrodes for electroplating and lead-out wires of the electrodes are arranged in the vertical direction of a micro-flow tube (a silicone tube with the inner diameter of 6mm and the outer diameter of 8 mm) shown in figure 2, the section of the front view surface is shown in figure 4, the anode is tightly attached to the micro-flow tube, the included angle between the flow direction of the cathode facing the plating solution and the wall of the micro-flow tube is 10 degrees, and the area ratio of the projection surface of the cathode on the anode to the anode is 1: 1.
Step seven: the microfluidic tube shown in fig. 2 was combined with the plating tank and the micropump (ZL12(12) -RZ1030) shown in fig. 1, and as shown in fig. 3, the starting end of the microfluidic tube was extended to a position 50mm below the supporting structure, the end of the microfluidic tube was kept flat with the supporting structure, and the micropump was mounted at the starting end of the microfluidic tube.
Step eight: the structure diagram of the electrode power supply and the electrode, the micro-pump power supply and the micro-pump are connected by using a lead as shown in fig. 7.
Step nine: and D, adding the mixed solution of the micro-nano metal particles and the plating solution obtained in the step four into a plating bath of the device shown in the figure 7, so that the liquid level is located at a distance of 30mm beyond the starting end of the micro-flow tube, and the tail end of the micro-flow tube does not enter the plating solution.
Step ten: adding a polytetrafluoroethylene magnetic stirrer (C type: 10 multiplied by 60 mm)2) At a rotation speed of 1X 103r/min, uniformly dispersing the micro-nano metal particles in the plating solution, and opening the magnetic stirring all the time in the subsequent electroplating process.
Step eleven: and (3) turning on a power supply of the micropump to ensure that the mixed solution of the micro-nano metal particles and the plating solution stably circulates in the microflow tube.
Step twelve: turning on the electroplating power supply, the cathode current density is 3A/dm2Controlling the applied pressure of the micro pump to make the flow rate of the plating solution be 0.1m/s, and electroplating at 40 deg.C while ensuring the relationship between the flow direction of the plating solution and the cathode in the electroplating process as shown in FIG. 6;
step thirteen: the system was allowed to work under the above conditions for 10min to complete the electroplating.
Fourteen steps: turning off the electroplating power supply and magnetic stirring, lifting the microflow pipe at the starting end position to exceed the liquid level of the plating solution, and turning off the power supply of the micropump after the plating solution in the microflow pipe flows into the electrolytic bath;
step fifteen: and C, filtering or centrifuging the plating solution obtained in the step thirteen to obtain electroplated micro-nano metal particles.
Sixthly, the steps are as follows: drying the electroplated micro-nano copper particles obtained in the step fifteen in a nitrogen atmosphere;
seventeen steps: and (4) storing the dried micro-nano copper particles obtained in the sixteenth step in a reducing atmosphere.
Example 2:
performing electrochemical gold plating on the surfaces of the micro-nano nickel particles:
the method comprises the following steps: and (4) preparing a gold plating solution. Adding 0.9L of deionized water into a preparation tank with the volume of 2L, sequentially adding 40g of sodium sulfite, 16g of sodium thiosulfate and 4g of gold sodium sulfite, and stirring until the sodium sulfite, the sodium thiosulfate and the gold sodium sulfite are completely dissolved; adding 10g of boric acid into another container, adding a proper amount of water, heating to 80 ℃, stirring until the boric acid is completely dissolved, and adding the boric acid into a preparation tank; adding 1g of polyethyleneimine and a proper amount of warm water into another container, stirring until the polyethyleneimine is completely dissolved, and adding the mixture into a preparation tank; and regulating the pH value of the plating solution to 6 by using 3% sulfuric acid by mass fraction, and finally adding deionized water until the volume of the solution is 1L to finish the preparation.
Step two: selecting nano nickel particles with the diameter of 1 mu m as micro-nano metal particles to be electroplated.
Step three: and removing the oxide on the surface of the nickel particles selected in the second step by using dilute sulfuric acid.
Step four: and (4) adding the nickel particles obtained in the third step into the plating solution obtained in the first step.
Step five: selecting a nickel plate with gold-plated surface as a cathode for electroplating, and selecting metal titanium as an anode for electroplating.
Step six: a plurality of pairs of electrodes for electroplating and lead-out wires of the electrodes are arranged in the vertical direction of a micro-flow tube (a silicone tube with the inner diameter of 6mm and the outer diameter of 8 mm) shown in figure 2, the section of the front view surface is shown in figure 4, the anode is tightly attached to the micro-flow tube, the included angle between the flow direction of the cathode facing the plating solution and the wall of the micro-flow tube is 10 degrees, and the area ratio of the projection surface of the cathode on the anode to the anode is 1: 1.
Step seven: the microfluidic tube shown in fig. 2 was combined with the plating tank and the micropump (ZL12(12) -RZ1030) shown in fig. 1, and as shown in fig. 3, the starting end of the microfluidic tube was extended to a position 50mm below the supporting structure, the end of the microfluidic tube was kept flat with the supporting structure, and the micropump was mounted at the starting end of the microfluidic tube.
Step eight: the structure of the micro pump power supply and the micro pump is shown in fig. 7.
Step nine: and D, adding the mixed solution of the micro-nano metal particles and the plating solution obtained in the step four into a plating bath of the device shown in the figure 7, so that the liquid level is located at a distance of 30mm beyond the starting end of the micro-flow tube, and the tail end of the micro-flow tube does not enter the plating solution.
Step ten: adding a polytetrafluoroethylene magnetic stirrer (C type: 10X 60mm2) into the electroplating bath at the rotating speed of 1X 103r/min to make the micro-nano metal particlesThe particles are uniformly dispersed in the plating solution, and the magnetic stirring is opened all the time in the subsequent electroplating process.
Step eleven: and (3) turning on a power supply of the micropump to ensure that the mixed solution of the micro-nano metal particles and the plating solution stably circulates in the microflow tube.
Step twelve: turning on the electroplating power supply, the cathode current density is 1.5A/dm2Electroplating is carried out by controlling the applied pressure of the micro pump to ensure that the flow rate of the plating solution is 0.1m/s, the electroplating temperature is 40 ℃, and the relation between the flow direction of the plating solution and the cathode is ensured in the electroplating process as shown in figure 6;
step thirteen: the system was allowed to work under the above conditions for 10min to complete the electroplating.
Fourteen steps: turning off the electroplating power supply and magnetic stirring, lifting the microflow pipe at the starting end position to exceed the liquid level of the plating solution, and turning off the power supply of the micropump after the plating solution in the microflow pipe flows into the electrolytic bath;
step fifteen: and filtering or centrifuging the plating solution obtained in the step thirteen to obtain electroplated micro-nano metal particles.
Sixthly, the steps are as follows: drying the electroplated micro-nano nickel particles obtained in the step fifteen in a nitrogen atmosphere;
seventeen steps: and (4) storing the dried micro-nano nickel particles obtained in the sixteenth step in a reducing atmosphere.
Claims (6)
1. A preparation method of a micro-nano metal particle surface coating is characterized by comprising the following steps: the method comprises the following specific steps:
the method comprises the following steps: selecting micro-nano metal particles to be electroplated, and removing an oxide film on the surfaces of the micro-nano metal particles;
step two: selecting and configuring a plating solution to be electroplated, and selecting and manufacturing an electroplated electrode;
step three: mixing the micro-nano metal particles obtained in the step one with the plating solution obtained in the step two;
step four: assembling an electroplating device, wherein the electroplating device specifically comprises an electroplating bath, a micro-flow tube, a micro-pump and a power supply; the micro flow pipe comprises a vertical section and a transition section; the vertical section is provided with a plurality of pairs of electrodes for electroplating and lead-out wires of the electrodes, the anode is tightly attached to the micro-flow tube in the vertical section of the micro-flow tube, and the included angle between the cathode facing the flow direction of the plating solution and the wall of the micro-flow tube is 10 degrees; a plurality of pairs of supporting structures are arranged on two sides of the top end of the electroplating bath and used for supporting the vertical section of the micro-flow pipe; during assembly, at the inlet, the micro pump does not enter the liquid level, the micro pipe is led out from the micro pump and inserted into the liquid level, and plating solution is pumped; connecting an electrode power supply and an electrode, and a micro-pump power supply and a micro-pump by using a lead;
step five: adding the mixed solution of the micro-nano metal particles and the plating solution obtained in the third step into the plating tank obtained in the fourth step, and adjusting the micro-flow tube to enable the starting end of the micro-flow tube to be located 30mm below the liquid level of the plating solution and the tail end of the micro-flow tube not to enter the plating solution;
step six: adding a magnetic stirrer into the electroplating bath at a rotation speed of 1 × 103r/min, in the subsequent electroplating process, opening the magnetic stirring all the time;
step seven: turning on a micro-pump power supply to ensure that the mixed liquid of the micro-nano metal particles and the plating solution stably circulates in the micro-flow tube;
step eight: turning on an electroplating power supply, controlling the pressure applied by the micro pump, and controlling the flow rate of the plating solution in the micro tube to be 0.05-0.2 m/s to carry out electroplating, wherein the flowing direction of the plating solution is ensured to be the same as the direction in which the distance between the cathode and the anode is reduced in the electroplating process;
step nine: controlling the current density of electroplating to be 1-5A/dm2Electroplating for 5-20 min to obtain a complete high-quality coating, and completing electroplating;
step ten: turning off the electroplating power supply and magnetic stirring, lifting the micro-flow tube at the starting end position to exceed the liquid level of the plating solution, turning off the micro-pump power supply after the plating solution in the micro-flow tube completely flows into the electrolytic bath, and then turning off the electroplating power supply;
step eleven: and filtering or centrifuging the plating solution obtained in the step ten to obtain electroplated micro-nano metal particles.
2. The method for preparing a micro-nano metal particle surface coating according to claim 1, wherein the method comprises the following steps: in the first step, the micro-nano metal particles to be electroplated are spherical particles with the diameter of 50 nm-10 mu m.
3. The method for preparing the micro-nano metal particle surface coating according to claim 1, characterized in that: in the circulation process of the plating solution, the plating solution is required to be kept in a bubble-free and continuous state in the micro flow tube.
4. The method for preparing the micro-nano metal particle surface coating according to claim 1, characterized in that: in the eighth step, the flow rate of the plating solution in the micro-flow tube is 0.1 m/s.
5. The method for preparing a micro-nano metal particle surface coating according to claim 1, wherein the method comprises the following steps: in the ninth step, the electroplating current is 2-4A/dm2The electroplating time is 10-18 min.
6. The method for preparing the micro-nano metal particle surface coating according to claim 1, characterized in that: the method further comprises the step of twelve: and drying the micro-nano metal particles in a reducing or inert atmosphere.
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| US5911865A (en) * | 1997-02-07 | 1999-06-15 | Yih; Pay | Method for electroplating of micron particulates with metal coatings |
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