CN106978614B - Preparation method of clean graphite silver-plated electric contact material - Google Patents
Preparation method of clean graphite silver-plated electric contact material Download PDFInfo
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- CN106978614B CN106978614B CN201610032856.6A CN201610032856A CN106978614B CN 106978614 B CN106978614 B CN 106978614B CN 201610032856 A CN201610032856 A CN 201610032856A CN 106978614 B CN106978614 B CN 106978614B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 26
- 239000010439 graphite Substances 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 19
- 238000007747 plating Methods 0.000 claims abstract description 56
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 24
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 claims abstract description 20
- 239000004332 silver Substances 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 39
- 239000007864 aqueous solution Substances 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000012752 auxiliary agent Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000009713 electroplating Methods 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000003518 caustics Substances 0.000 claims description 7
- PYIDGJJWBIBVIA-UYTYNIKBSA-N lauryl glucoside Chemical compound CCCCCCCCCCCCO[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O PYIDGJJWBIBVIA-UYTYNIKBSA-N 0.000 claims description 7
- GNMSLDIYJOSUSW-LURJTMIESA-N N-acetyl-L-proline Chemical compound CC(=O)N1CCC[C@H]1C(O)=O GNMSLDIYJOSUSW-LURJTMIESA-N 0.000 claims description 6
- 239000005643 Pelargonic acid Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 5
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002671 adjuvant Substances 0.000 claims description 2
- 238000005530 etching Methods 0.000 claims description 2
- 238000005238 degreasing Methods 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- 239000007921 spray Substances 0.000 abstract description 4
- 238000005987 sulfurization reaction Methods 0.000 abstract description 3
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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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
- C25D3/46—Electroplating: Baths therefor from solutions of silver
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- 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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention provides a preparation method of a clean graphite silver-plated electric contact material, which comprises the following steps: 1) preparing a plating solution: a, preparing a pre-silver plating solution; b, preparing silver-graphite composite plating solution; 2) preparing a plating layer: a, treating a substrate; b, pre-plating a silver layer; c silver-plated graphite composite layer. The plating layer has excellent conductivity, and the contact resistance is 28-40 mu omega (the applied torque is 5-20 N.m); good thermal conductivity, 260-280 W.m < -1 >. K < -1 >; the wear resistance is excellent, and the friction coefficient is 0.08-0.25 when the load is 260g at normal temperature and pressure; the service life is long, and in a mechanical life test (the clamping force is 400-600N), the mechanical life reaches between the M1 grade and the M2 grade standards of the mechanical life of the isolating switch (the separation and combination test is 4000-6000 times, and the loss of a plating layer is 5-10 mu M); the corrosion resistance is good, and the coating reaches the national standard of 10 grade of a neutral salt spray test in the salt spray test; the good sulfuration resistance, the sulfuration resistance of the plating layer reaches the requirement of navigation mark QJ 485-1988; the good comprehensive performance of the plating layer can completely meet the outdoor working conditions of the high-voltage isolating switch.
Description
Technical Field
The invention relates to an electrical contact protective material, in particular to a preparation method of a novel clean graphite silver-plated electrical contact material.
Background
The moving contact and the static contact of the existing outdoor high-voltage isolating switch are mostly designed by common silver plating or hard silver plating, the electric contact material can provide good electric conductivity, thermal conductivity and low and stable contact resistance, but the defects of large abrasion loss, poor fusion welding resistance, poor corrosion resistance and the like exist, and finally the heating fault of the isolating switch is caused. The working current of the high-voltage isolating switch is only 60% of the rated load current of the high-voltage isolating switch, overheating can occur when the working current exceeds 70%, and the abnormal heating defects account for 35% of the total defects of the isolating switch, so that the safe and stable operation of a power grid is severely restricted.
The graphite is a good self-lubricating material, the silver-graphite composite electric contact material prepared by an electroplating method or a powder metallurgy method can greatly improve the wear resistance and the service life of the electric contact material, and a layer of graphite layer protective film is easily formed on the surface of the electric contact material in the using process, so that the effect of reducing the surface contact resistance of the electric contact material is achieved. However, the silver graphite composite plating layer prepared at present has the problems of rough surface, low density, large abrasion loss and short service life. Therefore, a new method for preparing the silver-graphite composite electric contact material is needed to be invented, so that the electric contact material not only integrates the electric conduction and heat conduction capabilities and the wear-resistant and corrosion-resistant performances of silver and graphite, but also has the advantages of small friction coefficient, strong compactness and long service life.
Disclosure of Invention
The invention aims to provide a preparation method of a novel clean graphite silver-plated electric contact material, which is characterized in that an electroplating method is adopted to prepare a silver-graphite composite coating on a copper substrate, and the electric contact material can be ensured to have excellent performances such as wear resistance, oxidation resistance, sulfuration resistance and the like through the configuration of a plating solution and the pre-plating of a silver layer.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a novel clean graphite silver-plated electric contact material comprises the following steps:
1) preparing plating solution
a, preparing a pre-silver plating solution: preparing a mixed aqueous solution of Ag and thiourea with the concentration of 20-30 g/L and 210-320 g/L respectively at 35-55 ℃ and pH of 1-7;
b, preparing silver graphite composite plating solution: preparing a mixed aqueous solution of Ag and KI with the concentration of 20-45 g/L and 360-410 g/L respectively at the temperature of 20-50 ℃ and the pH of 1-7; then sequentially adding a dispersing agent, an auxiliary agent and graphite according to the concentrations of 10-50 ml/L, 10-50 ml/L and 60-100 g/L, and stirring at the rotating speed of 300-1000 r/min for 10-60 min;
2) preparation of the coating
a, matrix treatment: corroding the surface of the polished, deoiled and cleaned substrate in a corrosive agent, and cleaning;
b, pre-plating a silver layer: in the pre-silver plating solution obtained in the step 1), the matrix treated in the step a is added at a ratio of 0.1-0.5A/dm2The current density of the substrate is reacted for 20-60 s, and the substrate is cleaned;
c, silver-plated graphite composite layer: at a rate of 0.1 to 0.5A/dm2And (c) electroplating the substrate obtained in the step (b) in the silver-graphite composite plating solution for 20-120 min at the current density and the stirring speed of 300-1000 r/min, and drying after cleaning.
According to the first preferable technical scheme of the preparation method, the dispersing agent is one or a mixture of more of 1-10 wt% of pelargonic acid, 0.3-3 wt% of N-acetyl-L-proline and 0.3-3 wt% of ethyl acetate.
According to the second preferable technical scheme of the preparation method, the auxiliary agent is one or a mixed solution of more than one of 2-20 wt% of hexadecane, 0.3-3 wt% of ethylene glycol and 2-20 wt% of dodecyl glucoside.
According to a third preferred technical scheme of the preparation method, the oil removal comprises the steps of putting the substrate into an oil removal solution, electrifying, and then respectively removing oil from the cathode and the anode for 10-100 s by adopting a combined oil removal method, and repeating for 1-2 times; soaking in deionized water at 50-80 ℃ and shaking up and down for 5-15 s, and then soaking in deionized water at normal temperature and shaking up and down for 5-15 s.
According to a fourth preferred technical scheme of the preparation method, the oil removing solution is NaOH and Na with the concentrations of 5-10 g/L, 20-50 g/L and 30-60 g/L respectively2CO3·10H2O and Na3PO4·12H2And (3) mixed solution of O.
In a fifth preferred embodiment of the preparation method, the surface etching comprises exposing the substrate to HNO3：H2SO4Soaking in a corrosive agent in a ratio of 1: 2-5, shaking up and down for 5-15 s, and soaking in deionized water for 5-15 s.
According to the sixth preferred technical scheme of the preparation method, the pre-silver plating solution is a mixed aqueous solution of Ag and thiourea, the concentration of which is respectively 25g/L and 250g/L, at 35 ℃ and pH of 4.
According to a seventh preferred technical scheme of the preparation method, the silver-graphite composite plating solution comprises the following components in parts by weight: preparing a mixed aqueous solution of Ag and KI with the concentration of 25g/L and 400g/L respectively at 25 ℃ and pH of 3; then adding the dispersing agent, the auxiliary agent and the graphite in turn according to the concentrations of 15ml/L, 15ml/L and 80g/L respectively, and stirring for 30min at the rotating speed of 700 r/min.
According to the eighth preferred technical scheme of the preparation method, the dispersing agent is a mixed aqueous solution of 4 wt% of pelargonic acid, 0.5 wt% of N-acetyl-L-proline and 0.5 wt% of ethyl acetate.
In a ninth preferred embodiment of the preparation method, the adjuvant is a mixed aqueous solution of 10 wt% of hexadecane, 0.4 wt% of ethylene glycol and 15 wt% of dodecyl glucoside.
In the electroplating process, the cathode adopts an oxygen-free copper sheet (the purity is more than or equal to 99.95%) as a base material for electroplating, and the anode adopts an electroplating silver plate with the purity of 99.99%.
Compared with the closest prior art, the invention has the following beneficial effects:
1) the friction coefficient of the prepared coating is 0.08-0.25 when the load is 260g at normal temperature and normal pressure, and the coating reaches the standard between the mechanical service life grades of M1 and M2 of an isolating switch in a mechanical service life experiment (the clamping force is 400-600N) under the actual working condition (the opening and closing test is 4000-6000 times, and the loss of the coating is 5-10 mu M);
2) the thermal conductivity of the coating prepared by the invention is 260-280 W.m < -1 >. K < -1 >; the contact resistance is 28-40 [ mu ] omega (the applied torque is 5-20 N.m); has good binding force and meets the requirements of national standard GB/T5270-;
3) the coating salt spray test of the invention reaches the national standard of 10 grade of the neutral salt spray test; the sulfur resistance of the cable material meets the requirements of a navigation mark QJ 485-1988;
4) the production process is efficient and low in cost; the prepared silver-graphite composite coating has excellent comprehensive performance, completely meets the outdoor working conditions of the high-voltage isolating switch, and has great application value.
Drawings
FIG. 1: scanning electron micrographs of the surface of the silver-graphite composite plating of example 1;
FIG. 2: scanning electron micrographs of the surface of the silver-graphite composite plating of example 2.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
1) Preparation of plating solution
a pre-plating silver solution: preparing 20g/L Ag and 210g/L thiourea mixed aqueous solution at 35 ℃ and pH 4;
b, silver graphite composite plating solution: preparing 20g/L Ag and 380g/L KI mixed aqueous solution at the temperature of 20 ℃ and the pH value of 4 respectively; then sequentially adding a dispersing agent, an auxiliary agent and graphite according to the concentrations of 10ml/L, 10ml/L and 70g/L, and stirring for 20min at the rotating speed of 500 r/min; the dispersant is a mixed aqueous solution of 3 wt% of pelargonic acid, 0.3 wt% of N-acetyl-L-proline and 0.4 wt% of ethyl acetate; the auxiliary agent is a mixed aqueous solution of 8 wt% of hexadecane, 0.3 wt% of ethylene glycol and 13 wt% of dodecyl glucoside;
2) preparation of the coating
a, matrix treatment: the matrix is evenly polished by 1000# sand paper and is added with 10g/L NaOH and 20g/L Na2CO3·10H2O and 30g/L Na3PO4·12H2In the oil removing solution consisting of O, the oil removal of the cathode is carried out for 30s, the oil removal of the anode is carried out for 10s, the operation is repeated for 1 time, the mixture is soaked in deionized water at 60 ℃ and shaken up and down for 5s, then soaked in the deionized water at normal temperature and shaken up and down for 5s, and finally is added into HNO3：H2SO4Soaking in 1:2 corrosive agent and shaking up and down to perform surface corrosionEtching for 5s, and cleaning in deionized water;
b, pre-plating a silver layer: putting the substrate treated in the step a) in the pre-silvering solution obtained in the step 1) at 0.5A/dm2Reacting for 30s under the current density of the solution, and cleaning a substrate by deionized water;
c, silver-plated graphite composite layer: at 0.4A/dm2B, electroplating the substrate obtained in the step b in the silver-graphite composite plating solution for 120min at the current density of 700r/min and the stirring speed of 700r/min, washing with deionized water and drying.
As shown in an electron microscope image of the surface of the prepared plating layer, the thickness of the plating layer is 25 mu m, the graphite content is 19.88 percent, the contact resistance is 29.9 mu omega (the applied torque is 10 N.m), the thermal conductivity is 265.662 W.m < -1 > K < -1 >, the friction coefficient is 0.2 when the load is 260g at normal temperature and normal pressure, and the loss of the plating layer is 5 mu m after 5000 times of mechanical life tests (the clamping force is 500N).
Example 2
1) Preparation of plating solution
a pre-plating silver solution: preparing a mixed aqueous solution of Ag and thiourea with the concentration of 25g/L and 250g/L respectively at the temperature of 35 ℃ and the pH value of 4;
b, silver graphite composite plating solution: preparing a mixed aqueous solution of Ag and KI with the concentration of 25g/L and 400g/L respectively at 25 ℃ and pH of 3; then sequentially adding a dispersing agent, an auxiliary agent and graphite according to the concentrations of 15ml/L, 15ml/L and 80g/L respectively, and stirring for 30min at the rotating speed of 600 r/min; the dispersant is a mixed aqueous solution of 4 wt% of pelargonic acid, 0.5 wt% of N-acetyl-L-proline and 0.5 wt% of ethyl acetate; the auxiliary agent is a mixed aqueous solution of 10 wt% of hexadecane, 0.4 wt% of glycol and 15 wt% of dodecyl glucoside;
2) preparation of the coating
a, matrix treatment: the matrix is evenly polished by 1000# sand paper and is added with 20g/L NaOH and 20g/L Na2CO3·10H2O and 30g/L Na3PO4·12H2Removing oil from cathode for 40s and anode for 20s in oil removing solution composed of O, repeating for 1 time, soaking in 70 deg.C deionized water and shaking up and down for 10s, soaking in normal temperature deionized water and shaking up and down for 10s, and then soaking in HNO3：H2SO4Soaking in 1:3 corrosive agent and shaking up and down to etch surfaceWashing in deionized water for 10 s;
b, pre-plating a silver layer: putting the substrate treated in the step a) in the pre-silvering solution obtained in the step 1) at 0.5A/dm2Reacting for 20s at the current density of (1), and washing the substrate by deionized water;
c, silver-plated graphite composite layer: at 0.2A/dm2B, electroplating the substrate obtained in the step b in the silver-graphite composite plating solution for 90min at the current density of 400r/min and the stirring speed of 400r/min, and drying after washing with deionized water.
As shown in an electron microscope image of the surface of the prepared plating layer, the thickness of the plating layer is 20 μm, the graphite content is 18.58%, the contact resistance is 30.3 μ omega (the applied torque is 10N · m), the thermal conductivity is 272.577W · m-1 · K-1, the friction coefficient is 0.09 when the load is 260g at normal temperature and normal pressure, and the loss of the plating layer is 7 μm after 8000 times of a mechanical life test (500N clamping force).
Example 3
1) Preparation of plating solution
a pre-plating silver solution: preparing a mixed aqueous solution of Ag and thiourea with the concentration of 25g/L and 310g/L respectively at 45 ℃ and pH of 4;
b, silver graphite composite plating solution: preparing a mixed aqueous solution of Ag and KI with the concentration of 30g/L and 380g/L respectively at the temperature of 30 ℃ and the pH value of 4; then sequentially adding a dispersing agent, an auxiliary agent and graphite according to the concentrations of 20ml/L, 15ml/L and 80g/L respectively, and stirring for 20min at the rotating speed of 500 r/min; the dispersant is a mixed aqueous solution of 4 wt% of pelargonic acid, 0.5 wt% of N-acetyl-L-proline and 0.4 wt% of ethyl acetate; the auxiliary agent is a mixed aqueous solution of 10 wt% of hexadecane, 0.5 wt% of glycol and 15 wt% of dodecyl glucoside;
2) preparation of the coating
a, matrix treatment: the matrix is evenly polished by 1000# abrasive paper and is added with 10g/L NaOH and 25g/L Na2CO3·10H2O and 35g/L Na3PO4·12H2In the oil removing solution consisting of O, the oil removal of the cathode is carried out for 30s, the oil removal of the anode is carried out for 10s, the operation is repeated for 1 time, the mixture is soaked in deionized water at 60 ℃ and shaken up and down for 5s, then soaked in the deionized water at normal temperature and shaken up and down for 5s, and finally is added into HNO3：H2SO4Soaking in 1:2 corrosive agent and shaking up and down to perform surface corrosion for 5sCleaning in deionized water;
b, pre-plating a silver layer: putting the substrate treated in the step a) in the pre-silvering solution obtained in the step 1) at 0.5A/dm2Reacting for 40s at the current density of the substrate, and washing the substrate by deionized water;
c, silver-plated graphite composite layer: at 0.4A/dm2B, electroplating the substrate obtained in the step b in the silver-graphite composite plating solution for 100min at the current density of 700r/min and the stirring speed of 700r/min, and drying after washing with deionized water.
As shown in an electron microscope image of the surface of the prepared plating layer, the thickness of the plating layer is 23 mu m, the graphite content is 18.96%, the contact resistance is 30.2 mu omega (the applied torque is 10 N.m), the thermal conductivity is 268.882 W.m < -1 > K < -1 >, the friction coefficient is 0.12 when the load is 260g at normal temperature and normal pressure, and the loss of the plating layer is 6 mu m after 5000 times of mechanical life tests (the clamping force is 500N).
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.
Claims (8)
1. A preparation method of a clean graphite silver-plated electric contact material is characterized by comprising the following steps:
1) preparing plating solution
a, preparing a pre-silver plating solution: preparing a mixed aqueous solution of Ag and thiourea with the concentration of 20-30 g/L and 210-320 g/L respectively at 35-55 ℃ and pH of 1-7;
b, preparing silver graphite composite plating solution: preparing a mixed aqueous solution of Ag and KI with the concentration of 20-45 g/L and 360-410 g/L respectively at the temperature of 20-50 ℃ and the pH of 1-7; then sequentially adding a dispersing agent, an auxiliary agent and graphite according to the concentrations of 10-50 ml/L, 10-50 ml/L and 60-100 g/L, and stirring at the rotating speed of 300-1000 r/min for 10-60 min;
2) preparation of the coating
a, matrix treatment: corroding the surface of the polished, deoiled and cleaned substrate in a corrosive agent, and cleaning;
b, pre-plating a silver layer: in the pre-silver plating solution obtained in the step 1), the matrix treated in the step a is added at a ratio of 0.1-0.5A/dm2The current density of the substrate is reacted for 20-60 s, and the substrate is cleaned;
c, silver-plated graphite composite layer: at a rate of 0.1 to 0.5A/dm2B, electroplating the substrate obtained in the step b in the silver-graphite composite plating solution for 20-120 min at the current density of 300-1000 r/min and at the stirring speed of 300-1000 r/min, cleaning and drying,
the dispersant is a mixed aqueous solution of 4 wt% of pelargonic acid, 0.5 wt% of N-acetyl-L-proline and 0.5 wt% of ethyl acetate.
2. The preparation method according to claim 1, wherein the adjuvant is a mixed solution of one or more of 2 to 20 wt% of hexadecane, 0.3 to 3 wt% of ethylene glycol and 2 to 20 wt% of dodecyl glucoside.
3. The preparation method according to claim 1, wherein the oil removal comprises the steps of putting the substrate in an oil removal solution, sequentially and respectively removing oil from the cathode and the anode for 10-100 s after electrification, and repeating for 1-2 times; soaking in deionized water at 50-80 ℃ and shaking up and down for 5-15 s, and then soaking in deionized water at normal temperature and shaking up and down for 5-15 s.
4. The preparation method according to claim 3, wherein the degreasing solution is NaOH or Na having a concentration of 5 to 10g/L, 20 to 50g/L, or 30 to 60g/L2CO3·10H2O and Na3PO4·12H2And (3) mixed solution of O.
5. The method of claim 1, wherein the surface etching comprises exposing the substrate to HNO3：H2SO4Soaking in a corrosive agent in a ratio of 1: 2-5, shaking up and down for 5-15 s, and soaking in deionized water for 5-15 s.
6. The method according to claim 1, wherein the pre-silver plating solution is a mixed aqueous solution of Ag and thiourea prepared at a concentration of 25g/L and 250g/L, respectively, at 35 ℃ and pH 4.
7. The method for preparing according to claim 1, wherein the silver-graphite composite plating solution: preparing a mixed aqueous solution of Ag and KI with the concentration of 25g/L and 400g/L respectively at 25 ℃ and pH of 3; then adding the dispersing agent, the auxiliary agent and the graphite in turn according to the concentrations of 15ml/L, 15ml/L and 80g/L respectively, and stirring for 30min at the rotating speed of 700 r/min.
8. The method for preparing a skin care preparation according to claim 2, wherein the auxiliary is a mixed aqueous solution of 10 wt% hexadecane, 0.4 wt% ethylene glycol and 15 wt% dodecyl glucoside.
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| CN109137011A (en) * | 2018-09-20 | 2019-01-04 | 吕莉 | A kind of preparation method of high voltage isolator contact material |
| CN109267124B (en) * | 2018-10-19 | 2019-11-19 | 西安西电电气研究院有限责任公司 | A kind of silver coated graphite composite deposite and preparation method thereof |
| JP7233991B2 (en) * | 2019-03-18 | 2023-03-07 | Ｄｏｗａメタルテック株式会社 | Composite plated material and its manufacturing method |
| CN111519232B (en) * | 2020-04-20 | 2022-03-11 | 国网江西省电力有限公司电力科学研究院 | Silver/graphene composite plating solution, use method thereof and silver/graphene composite plating layer |
| CN114108043B (en) * | 2021-11-19 | 2023-08-11 | 山东省路桥集团有限公司 | Repairing and regenerating pretreatment method for rusted area of steel structure bridge |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102691081A (en) * | 2012-06-11 | 2012-09-26 | 东莞市闻誉实业有限公司 | Electrosilvering solution and electrosilvering method |
| CN103173817A (en) * | 2011-12-24 | 2013-06-26 | 黄小飞 | Environmental-friendly electrosilvering solution |
-
2016
- 2016-01-19 CN CN201610032856.6A patent/CN106978614B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173817A (en) * | 2011-12-24 | 2013-06-26 | 黄小飞 | Environmental-friendly electrosilvering solution |
| CN102691081A (en) * | 2012-06-11 | 2012-09-26 | 东莞市闻誉实业有限公司 | Electrosilvering solution and electrosilvering method |
Non-Patent Citations (2)
| Title |
|---|
| 户外高压隔离开关用银石墨复合镀层的热稳定性研究;叶志国 等;《第十一次全国热处理大会论文集》;20150731;855-858页 * |
| 无氰镀银添加剂的研究;单颖会;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20120215(第2期);正文第10-12页 * |
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