CN110923785A - Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition - Google Patents
Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition Download PDFInfo
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- CN110923785A CN110923785A CN201911270182.3A CN201911270182A CN110923785A CN 110923785 A CN110923785 A CN 110923785A CN 201911270182 A CN201911270182 A CN 201911270182A CN 110923785 A CN110923785 A CN 110923785A
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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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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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
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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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
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
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Abstract
The invention provides a method for preparing a silver alloy/copper alloy composite contact material for a circuit breaker by codeposition, which comprises the following steps: plating nickel on the surface of the silver alloy plate, and preparing a nickel plating solution: nickel sulfate, nickel chloride, boric acid and sodium dodecyl sulfate; taking the alloy plate to be silver-plated as a cathode and a pure nickel plate as an anode, plating the surface of the alloy plate to be silver-plated to face the anode, enabling the nickel layer to reach the thickness, and then cleaning and drying; and (3) silver alloy plate composite plating: preparing a composite plating solution: copper sulfate, sulfuric acid, solid particles with the average particle size of tin oxide, lanthanum oxide, titanium carbide, tungsten carbide, boron nitride, diamond and graphite are dispersed by ultrasonic waves; taking the alloy plate to be plated with silver as a cathode and stainless steel as an anode, plating the nickel-plated surface of the alloy plate to be plated with silver under ultrasonic dispersion, and then cleaning and drying; sintering; cold rolling to specified size; the invention can reliably combine the silver alloy and the copper alloy together with low cost; the composite plating layer has stronger fusion welding resistance.
Description
Technical Field
The invention relates to a method for preparing a silver alloy/copper alloy composite contact material for a circuit breaker by codeposition.
Background
The contact is a core element of a low-voltage apparatus and plays the roles of switching on, carrying current and breaking current. The development of contact materials has been accompanied by the implementation of various silver saving methods, wherein the most common method is to save silver by adopting a silver alloy/copper composite mode, and the structure of the contact material is shown in fig. 1, and the silver can be saved by more than 50%. The silver alloy/copper composite process mostly adopts a powder metallurgy method and a hot rolling cladding method.
The powder metallurgy method is to press silver alloy powder and copper powder into a two-layer blank, and then to obtain the final product through sintering, repressing and reburning. The hot rolling composite method is a process of heating a copper strip and a contact strip to a certain temperature, rolling the copper strip and the contact strip with a rolling mill in a large deformation amount, and then performing heat treatment to form metallurgical bonding of the two materials.
Both the two processes have certain problems and limitations, the density of the contact prepared by the powder metallurgy method is low and can only reach about 95% of the relative density, the electrical property is poor, the strength is low, and the problem of cracking caused by impact in the subsequent welding process can be caused. Meanwhile, due to the fact that the silver alloy powder and the copper alloy powder which are made of different materials are different in wettability and shrinkage rate when being sintered, a lot of materials cannot be compounded. The hot rolling compounding method solves the defects of the powder metallurgy method, but the contact material which is prepared by adopting an infiltration method or has poor extensibility and excellent electrical property and cannot compound silver carbide and silver oxide exists, and the application range is seriously limited.
In addition, the contact material for the circuit breaker is required to have good characteristics of electrical conductivity, resistance to welding, and resistance to arc burning. In the using process of the contact material compounded by pure copper or oxygen-free copper and silver alloy, after the silver alloy layer is ablated by electric arc, the contact fails due to the fact that the pure copper layer does not have fusion welding resistance, and great potential safety hazards appear.
Disclosure of Invention
The invention aims to provide a method for preparing a silver alloy/copper alloy composite contact material for a circuit breaker by codeposition, which can reliably and cheaply combine silver alloy and copper alloy together.
The technical scheme of the invention is realized as follows: a method for preparing a silver alloy/copper alloy composite contact material for a circuit breaker by codeposition comprises the following steps:
step 2-1, preparing a nickel plating solution: 250g/L of nickel sulfate, 30-60g/L of nickel chloride and 35-40g/L of boric acid
g/L, 0.05-0.1g/L of sodium dodecyl sulfate and pH of 3-4;
step 2-2, plating: taking the alloy plate to be plated with silver as a cathode and a pure nickel plate as an anode, plating the surface of the alloy plate to be plated with silver, which is subjected to sand blasting, facing the anode to ensure that a nickel layer reaches the thickness required by the specification, and then cleaning and drying;
step 3, silver alloy plate composite plating:
step 3-1, preparing a composite plating solution: 150g/L of copper sulfate, 45-110g/L of sulfuric acid, 1-3g/L of tin oxide, lanthanum oxide, titanium carbide, tungsten carbide, boron nitride,
Dispersing solid particles of diamond and graphite or the combination of the solid particles in any proportion by ultrasonic waves;
step 3-2, taking the alloy plate to be silver-plated as a cathode and stainless steel as an anode, plating the nickel-plated surface of the alloy plate to be silver-plated under ultrasonic dispersion, and then cleaning and drying;
step 4, sintering;
step 5, repeating the steps 3 and 4 until a copper alloy layer with a specified thickness is obtained;
step 6, cold rolling: cold rolling the composite strip to a specified size;
and 7, annealing: sintering at 650 ℃ under the protection of argon for 2-3 h.
The invention also has the following features:
1. the plating is carried out at the temperature of 45-60 ℃ and the current density of 1-2.5A/dm in the step 22Plating for 2-5 min.
2. The plating is carried out at the temperature of 20-50 ℃ and the current density of 1-3A/dm2And plating for 15-30 min.
3. And 3.1, ultrasonically dispersing for 30-60 min.
4. And step 4, sintering at the temperature of argon 500-780 ℃ for 1-2 h.
5. In the step 7, sintering is carried out at the temperature of 350-650 ℃ under the protection of argon, and the heat preservation time is 2-3 h.
6. The silver alloy/copper alloy composite contact material for the circuit breaker is prepared by the method.
The invention has the following advantages and beneficial effects: the invention adopts dispersion electroplating, which is to use an electroplating method to co-deposit solid particles and metal, namely, insoluble solid particles are uniformly dispersed in electroplating solution to prepare suspension for electroplating, thereby obtaining a composite coating with a certain thickness of a particle structure dispersed and distributed on matrix metal on a substrate. The solid particles refer to various refractory oxides, carbides, borides, nitrides, simple substance carbon and the like, such as tin oxide, lanthanum oxide, titanium carbide, tungsten carbide, boron nitride, diamond, graphite and the like. The plating base metals are nickel, copper, chromium and some alloys. According to the characteristics of different particles, such as high hardness, high thermal conductivity, reducibility generated in arc ablation, easy shedding from a matrix metal to expose fresh matrix metal and the like of the diamond, the composite coating has stronger fusion welding resistance; for example, lanthanum oxide has the arcing characteristic, so that the composite coating has stronger arc moving capability, and the local arc ablation of the contact is reduced. Particularly, the existence of the intermediate nickel layer solves the defects of interlayer pores and the like formed by silver and copper diffusion caused by repeated plating and sintering, thereby applying the dispersion plating method and improving the composite strength.
Drawings
Fig. 1 is a structural diagram of a silver alloy/copper contact material, wherein 1 is silver alloy, and 2 is copper.
Detailed Description
The invention is further illustrated by the following examples:
example 1
step 2.1, preparing a nickel plating solution: preparing a nickel plating solution containing 250g/L of nickel sulfate, 30g/L of nickel chloride, 35g/L of boric acid and 0.05g/L of sodium dodecyl sulfate, and adjusting the pH value to be 3-4.
Step 2.2, taking the silver alloy plate to be plated as a cathode and a pure nickel plate as an anode, wherein the sand blasting surface of the silver alloy plate to be plated faces the anode, the temperature is 45 ℃, and the current density is 1.0A/dm2Plating is carried out for 5 min.
And 2.3, rinsing with tap water for three times, rinsing with distilled water for two times, and airing.
Step 3, composite plating
Step 3.1, preparing 150g/L copper sulfate and 45g/L sulfuric acid, adding 0.5g/L diamond with the average grain size of 0.5-1.5 mu m and 1.5g/L titanium carbide, and dispersing for 30min by ultrasonic waves.
Step 3.2, taking the alloy plate to be plated with silver as a cathode and stainless steel as an anode, facing the nickel-plated surface of the alloy plate to be plated with silver to the anode, and dispersing the alloy plate to be plated with silver at the temperature of 20 ℃ and the current density of 1.0A/dm under ultrasonic waves2Plating is carried out for 15 min.
And 3.3, rinsing with tap water for three times, rinsing with distilled water for two times, and airing.
And 4, sintering the plated strip at 500 ℃ under the protection of argon, and keeping the temperature for 2 hours.
And 5, repeating the steps 3 and 4 for 20 times to obtain a copper alloy layer with the thickness of 0.8 mm.
And 6, cold rolling the sintered composite strip, wherein the rolling amount is more than or equal to 10% each time, and annealing the composite strip at 350 ℃ under the protection of argon after rolling for 2 hours. The rolling and annealing were repeated 6 times to a thickness of 1.0 mm.
In the embodiment, the composite plate material with the thickness of the AgSnO (10) layer being 0.5mm and the thickness of the copper alloy layer being 0.5mm and containing 5 wt% of diamond is obtained through the method.
Example 2
step 2.1, preparing a nickel plating solution: preparing a nickel plating solution containing 300g/L of nickel sulfate, 60g/L of nickel chloride, 40g/L of boric acid and 1.0g/L of sodium dodecyl sulfate, and adjusting the pH value to be 3-4.
Step 2.2, taking the silver alloy plate to be plated as a cathode and a pure nickel plate as an anode, wherein the sand blasting surface of the silver alloy plate to be plated faces the anode, the temperature is 60 ℃, and the current density is 2.5A/dm2Plating is carried out for 2 min.
And 2.3, rinsing with tap water for three times, rinsing with distilled water for two times, and airing.
Step 3, composite plating
Step 3.1, preparing the mixture containing 250g/L of copper sulfate and 110g/L of sulfuric acid, adding 0.5g/L of diamond with the average particle size of 0.5-1.5 mu m and 1.0g/L of titanium carbide, and dispersing for 60min by ultrasonic waves.
Step 3.2, taking the silver alloy plate to be plated as a cathode and stainless steel as an anode, facing the nickel-plated surface of the silver alloy plate to be plated to the anode, and dispersing the nickel alloy plate to be plated at the temperature of 50 ℃ and the current density of 3A/dm under ultrasonic waves2Plating is carried out for 30 min.
And 3.3, rinsing with tap water for three times, rinsing with distilled water for two times, and airing.
And 4, sintering the plated strip at 780 ℃ under the protection of argon, and keeping the temperature for 1 h.
And 5, repeating the steps 3 and 4 for 8 times to obtain a copper alloy layer with the thickness of 1.0 mm.
And 6, cold rolling the sintered composite strip, wherein the rolling amount is more than or equal to 10% each time, and annealing the composite strip at 650 ℃ under the protection of argon after rolling for 2 hours. The rolling and annealing were repeated 3 times until a thickness of 1.5mm was reached.
In the embodiment, the composite plate material with the thickness of the AgZnO (8) layer of 0.75mm and the thickness of the copper alloy layer of 0.75mm, wherein the copper alloy layer contains diamond and titanium carbide of 2 w% and 4 wt% is obtained by the method.
Example 3
step 2.1, preparing a nickel plating solution: preparing a nickel plating solution containing 280g/L of nickel sulfate, 50g/L of nickel chloride, 37g/L of boric acid and 0.08g/L of sodium dodecyl sulfate, and adjusting the pH value to be 3-4.
Step 2.2, taking the silver alloy plate to be plated as a cathode and a pure nickel plate as an anode, wherein the sand blasting surface of the silver alloy plate to be plated faces the anode, the temperature is 50 ℃, and the current density is 2.0A/dm2Plating is carried out for 3 min.
And 2.3, rinsing with tap water for three times, rinsing with distilled water for two times, and airing.
Step 3, composite plating
Step 3.1, preparing 200g/L copper sulfate and 75g/L sulfuric acid, adding 0.5g/L diamond with the average particle size of 0.5-1.5 mu m and 1.0g/L lanthanum oxide, and dispersing for 45min by ultrasonic waves.
Step 3.2, taking the silver alloy plate to be plated as a cathode and stainless steel as an anode, facing the nickel-plated surface of the silver alloy plate to be plated to the anode, and dispersing the nickel alloy plate to be plated at the temperature of 30 ℃ and the current density of 2.5A/dm under ultrasonic waves2Plating is carried out for 20 min.
And 3.3, rinsing with tap water for three times, rinsing with distilled water for two times, and airing.
And 4, sintering the plated strip at 750 ℃ under the protection of argon, and keeping the temperature for 1.5 h.
And 5, repeating the steps 3 and 4 for 8 times to obtain a copper alloy layer with the thickness of 0.6 mm.
And 6, cold rolling the sintered composite strip, wherein the rolling amount is more than or equal to 10% each time, and annealing the composite strip at 650 ℃ under the protection of argon after rolling for 2 hours. The rolling and annealing were repeated 2 times until the thickness reached 1.0 mm.
In the embodiment, the composite plate material with the thickness of 0.50mm of AgWC30 layer, the thickness of 0.50mm of copper alloy layer and the thickness of 2 w% and 4 wt% of diamond and lanthanum oxide in the copper alloy layer is obtained through the method.
Claims (7)
1. A method for preparing a silver alloy/copper alloy composite contact material for a circuit breaker by codeposition is characterized by comprising the following steps:
step 1, performing sand blasting treatment on the surface of a silver alloy plate to be plated;
step 2, plating nickel on the surface of the silver alloy plate:
step 2-1, preparing a nickel plating solution: 250g/L of nickel sulfate, 30-60g/L of nickel chloride, 35-40g/L of boric acid, 0.05-0.1g/L of sodium dodecyl sulfate and 3-4 of pH;
step 2-2, plating: taking the alloy plate to be plated with silver as a cathode and a pure nickel plate as an anode, plating the surface of the alloy plate to be plated with silver, which is subjected to sand blasting, facing the anode to ensure that a nickel layer reaches the thickness required by the specification, and then cleaning and drying;
step 3, silver alloy plate composite plating:
step 3-1, preparing a composite plating solution: 150g/L of copper sulfate, 45-110g/L of sulfuric acid, 1-3g/L of solid particles of tin oxide, lanthanum oxide, titanium carbide, tungsten carbide, boron nitride, diamond and graphite with the average particle size of 0.5-6 mu m or the combination of the above in any proportion, and dispersing by ultrasonic wave;
step 3-2, taking the alloy plate to be silver-plated as a cathode and stainless steel as an anode, plating the nickel-plated surface of the alloy plate to be silver-plated under ultrasonic dispersion, and then cleaning and drying;
step 4, sintering;
step 5, repeating the steps 3 and 4 until a copper alloy layer with a specified thickness is obtained;
step 6, cold rolling: cold rolling the composite strip to a specified size;
and 7, annealing: sintering at 650 ℃ under the protection of argon for 2-3 h.
2. The method for preparing the silver alloy/copper alloy composite contact material for the circuit breaker by codeposition according to claim 1, characterized in that: step 2, plating is carried out at the temperature of 45-60 ℃ and the current density of 1-2.5A/dm2Plating for 2-5 min.
3. The silver alloy/copper alloy composite contact material for the circuit breaker prepared by the codeposition according to claim 1The method of (2), characterized by: step 3, plating is carried out at the temperature of 20-50 ℃ and the current density of 1-3A/dm2And plating for 15-30 min.
4. The method for preparing the silver alloy/copper alloy composite contact material for the circuit breaker by codeposition according to claim 1, characterized in that: and 3-1, ultrasonically dispersing for 30-60 min.
5. The method for preparing the silver alloy/copper alloy composite contact material for the circuit breaker by codeposition according to claim 1, characterized in that: and 4, sintering at the temperature of argon 500-780 ℃ for 1-2 h.
6. The method for preparing the silver alloy/copper alloy composite contact material for the circuit breaker by codeposition according to claim 1, characterized in that: and step 7, sintering at the temperature of 350-650 ℃ under the protection of argon, and keeping the temperature for 2-3 h.
7. A silver alloy/copper alloy composite contact material for a circuit breaker, produced by the method according to any one of claims 1 to 6.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114453584A (en) * | 2021-12-28 | 2022-05-10 | 温州中希电工合金有限公司 | Preparation method of silver graphite electrical contact material |
| CN114571130A (en) * | 2021-11-22 | 2022-06-03 | 祥博传热科技股份有限公司 | Preparation method of welding material for welding copper and nonmetal base material and welding piece |
| CN116550975A (en) * | 2023-07-04 | 2023-08-08 | 赣州金顺科技有限公司 | Preparation method of diamond/copper composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114571130A (en) * | 2021-11-22 | 2022-06-03 | 祥博传热科技股份有限公司 | Preparation method of welding material for welding copper and nonmetal base material and welding piece |
| CN114453584A (en) * | 2021-12-28 | 2022-05-10 | 温州中希电工合金有限公司 | Preparation method of silver graphite electrical contact material |
| CN116550975A (en) * | 2023-07-04 | 2023-08-08 | 赣州金顺科技有限公司 | Preparation method of diamond/copper composite material |
| CN116550975B (en) * | 2023-07-04 | 2023-09-26 | 赣州金顺科技有限公司 | Preparation method of diamond/copper composite material |
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