CN117004842A - Preparation method of flaky silver-nickel-graphite copper-coated contact material - Google Patents
Preparation method of flaky silver-nickel-graphite copper-coated contact material Download PDFInfo
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- CN117004842A CN117004842A CN202310991286.3A CN202310991286A CN117004842A CN 117004842 A CN117004842 A CN 117004842A CN 202310991286 A CN202310991286 A CN 202310991286A CN 117004842 A CN117004842 A CN 117004842A
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- silver
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- 239000010439 graphite Substances 0.000 title claims abstract description 62
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 62
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010949 copper Substances 0.000 title abstract description 31
- 229910052802 copper Inorganic materials 0.000 title abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 54
- 239000011812 mixed powder Substances 0.000 claims abstract description 41
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000003825 pressing Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000005751 Copper oxide Substances 0.000 claims abstract description 14
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 230000009467 reduction Effects 0.000 claims abstract description 8
- 230000000754 repressing effect Effects 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 28
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 30
- 229910052709 silver Inorganic materials 0.000 abstract description 22
- 239000004332 silver Substances 0.000 abstract description 22
- 230000008569 process Effects 0.000 abstract description 14
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 16
- 230000001681 protective effect Effects 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 14
- 229910052739 hydrogen Inorganic materials 0.000 description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 13
- 229910017727 AgNi Inorganic materials 0.000 description 12
- 239000010410 layer Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000002131 composite material Substances 0.000 description 10
- 238000003466 welding Methods 0.000 description 10
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(i) oxide Chemical compound [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 9
- 238000005261 decarburization Methods 0.000 description 5
- MOFOBJHOKRNACT-UHFFFAOYSA-N nickel silver Chemical compound [Ni].[Ag] MOFOBJHOKRNACT-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 238000007747 plating Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000004927 fusion Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000011246 composite particle Substances 0.000 description 2
- 229910018106 Ni—C Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000003475 lamination 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
- 239000002994 raw material Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Switches (AREA)
Abstract
The invention discloses a preparation method of a flaky silver-nickel-graphite copper-coated contact material, which comprises the steps of mixing silver-nickel-graphite mixed powder with copper powder and copper oxide powder according to the proportion of (0.65-0.8): 1, pressing and forming copper oxide mixed powder composed of the components in a weight ratio, placing the obtained primary pressed and formed pressed blank in inert atmosphere for primary sintering, then placing the primary pressed and formed pressed blank in reducing atmosphere for reduction, and carrying out secondary repressing to obtain primary repressed blank; and then sequentially carrying out secondary sintering, secondary re-pressing and annealing on the obtained primary re-pressing blank to obtain the flaky silver-nickel-graphite copper-clad contact material. The method provided by the invention has the advantages of silver saving effect, simple process, low cost and strong practicability, and can ensure the bonding strength of the bonding interface of the obtained contact material.
Description
Technical Field
The invention relates to a preparation method of an alloy contact material, in particular to a preparation method of a flaky silver-nickel-graphite copper-coated contact material.
Background
In a switching device, an electrical contact directly bears the functions of breaking and switching on a circuit and bearing normal working current or overload current in a certain time, and the working performance and quality of the electrical contact directly determine key functions of various switching devices, such as the on-off capability of a power distribution device, the electrical service life of a control device and the reliability of a relay.
The silver-nickel-graphite (AgNiC) contact material is a composite material formed by combining silver, nickel and graphite components, and has the advantages of good burning loss resistance, good fusion welding resistance and stable contact resistance, so that the silver-nickel-graphite contact material has the characteristics of good fusion welding resistance, low and stable contact resistance and is mainly applied to various molded case circuit breakers and frame type universal circuit breakers.
Because the silver-nickel-graphite contact material contains graphite, the graphite has the characteristic of fusion welding resistance, and the wettability of the graphite with silver, nickel and copper is poor, the silver-nickel-graphite and copper contact bridge is poor in wettability during direct welding, the cold joint is easy to form, and the welding quality cannot meet the requirements. The quality of welding has very important direct relation to the reliability of the operation of the electric appliance, the temperature rise of the electric appliance, the on-off capability of a contact, the burning loss of an electric arc and the service life. Therefore, in order to ensure the welding quality of the silver-nickel graphite contact and the copper contact bridge, when the flaky silver-nickel graphite contact is manufactured, a pure silver layer is designed to serve as a welding transition layer, for example:
the invention patent with publication number of CN113245547A discloses a preparation method of a silver-nickel graphite electrical contact with a continuous decarburized layer on the side surface. In the preparation process, the method needs to be cut or milled to generate more waste materials, so that the material processing yield is affected, and the manufacturing cost of the material is high; meanwhile, the overall silver content of the material is high, and the material cost is further increased.
The invention patent with publication number of CN102808098A discloses a preparation method of a silver/nickel/graphite electric contact material, which comprises the steps of firstly plating nickel on colloidal graphite and then plating silver to obtain powder with an Ag-Ni-C core-shell structure by adopting a chemical plating method, then mixing the powder with pure silver powder, reducing the content of the colloidal graphite to a specified value, and then obtaining the silver/nickel/graphite material after sintering, extruding and drawing processes. The invention adopts the chemical plating method to improve the oxidation resistance of the composite particles and the sintering granulation performance, and the deformability of the intermediate composite particles in the processing process, thereby improving the technological performance, but the overall silver content of the material is higher, and the problem of higher material cost is also existed.
From the standpoint of reducing the silver content in the material and reducing the cost of raw materials, copper having similar physical, chemical, electrical and other properties to silver has been used in the prior art to replace silver as a solder layer. The invention patent with publication number of CN115810494A discloses a manufacturing method of a silver-graphite composite copper electrical contact material, which comprises the steps of mixing silver powder, graphite powder and additives, sintering and granulating, pressing and forming the obtained particles and copper powder by a composite lamination automatic tablet press, sintering the obtained blank in hydrogen, and re-pressing. However, the primary press forming pressed compact obtained by pressing silver graphite powder particles and copper powder is directly sintered, and because the wettability of graphite, silver and copper is poor, the physical bonding strength between non-wetting materials is poor, and certain gaps exist at the bonding position of a silver graphite layer and a copper layer due to the existence of graphite, so that the bonding strength of a bonding interface of the obtained contact material is affected, the middle bonding strength is not ideal, and the material has the risk of layering in the actual use process of the product.
Disclosure of Invention
The invention aims to provide a preparation method of a flaky silver-nickel-graphite copper-coated contact material which can reduce silver content and ensure bonding strength of a bonding interface.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a flaky silver-nickel-graphite copper-clad contact material comprises the following steps:
1) Obtaining silver-nickel-graphite mixed powder;
2) According to (0.65-0.8): 1, weighing copper powder and copper oxide powder in a weight ratio, and mixing the copper powder and the copper oxide powder to obtain copper oxide mixed powder;
3) Pressing and forming the silver-nickel-graphite mixed powder and the copper oxide mixed powder to obtain an initial-press formed pressed compact;
4) The primary pressed compact is firstly placed in inert atmosphere for primary sintering, then placed in reducing atmosphere for reduction, and secondary pressing is carried out again to obtain primary pressed blank;
5) And sequentially performing secondary sintering, secondary repressing and annealing procedures on the obtained primary repressing blank to obtain the flaky silver-nickel-graphite copper-clad contact material.
The invention comprises two parts of copper required by a copper coating layer, wherein one part is pure oxygen-free copper powder, and the other part is copper oxide powder, and the aim and the principle are as follows: the reduction of graphite at high temperature and the oxidation-reduction reaction of copper oxide are utilized to play a role of decarburization, so that the existence of graphite at the bonding interface is avoided, and the bonding strength between the bonding interfaces is improved. On the other hand, since the workability of the copper oxide powder is poor, it cannot be directly press-formed with the silver-nickel-graphite mixed powder, and therefore, a certain amount of copper powder is added to mix with the silver-nickel-graphite mixed powder, so that the silver-nickel-graphite mixed powder and the copper-copper oxide mixed powder can be press-formed. The specific process flow and principle are as follows: in the process of placing the pressed blank in inert atmosphere for primary sintering, the copper oxide at the bonding interface and the contacted graphite undergo oxidation-reduction reaction at high temperature to consume the graphite, thereby playing the role of decarburization at the bonding interface; then placing the blank subjected to decarburization under a reducing atmosphere for reduction, and further reducing copper oxide into copper, wherein in the process, as the bonding interface of the blank is decarburized, silver, nickel and copper of the bonding interface can be fully contacted, the mutual diffusion among silver, nickel and copper particles is improved, the effective bonding of the interface is promoted in the secondary sintering process, and the bonding strength of the composite interface of the silver-nickel-graphite copper-clad contact material is improved; the subsequent secondary sintering and secondary repressing procedures improve the compactness of the material, reduce the resistivity of the material and effectively ensure the performance and quality of the obtained contact material.
In the step 1) of the preparation method, the graphite content in the silver-nickel-graphite mixed powder is preferably 2-4wt%, the nickel content is preferably 1.5-30wt%, and the balance is silver, wherein the graphite is preferably colloidal graphite. The specific proportion of graphite powder, nickel powder and silver powder in the silver-nickel-graphite mixed powder is determined according to the silver-nickel-graphite contact which is required to be prepared, weighing is carried out after the determination, and the conventional operation is adopted for powder mixing so as to obtain the silver-nickel-graphite mixed powder. For example, the weighed graphite powder, nickel powder and silver powder may be placed in a mixer and mixed for 2 to 4 hours at a rotational speed of 20 to 40 r/min.
In step 2) of the above production method, the particle diameters of the copper powder and the copper oxide powder are preferably 74 μm (-200 mesh) or less, more preferably 48 μm (-300 mesh) or less. As regards the ratio of copper powder to copper oxide powder, the applicant found in the test that when the weight ratio of copper powder to copper oxide powder is lower than 0.65:1, copper powder with a too low proportion is difficult to form and is easy to delaminate in initial pressure; and when the weight ratio of copper powder to copper oxide powder is higher than 0.8: in the process 1, the consumption of graphite in the subsequent sintering process is low due to the fact that the copper oxide powder is too low in proportion, and the decarburization effect of a bonding interface is not ideal.
In the step 3) of the preparation method, the dosage of the silver-nickel-graphite mixed powder and the copper-copper oxide mixed powder is determined according to the size of the contact to be prepared, and after the specification size of the contact to be prepared is determined, the dosage of the copper-copper oxide mixed powder is determined by combining the thickness of the copper-clad layer. The silver-nickel-graphite mixed powder and the copper oxide-copper mixed powder are pressed and formed by adopting a composite automatic tablet press, and the forming pressure is usually 3-4T/cm 2 。
The preparation methodIn step 4) of the method, the processes of primary sintering, reduction and primary repressing are the same as those in the prior art. Specifically, the temperature of primary sintering is preferably 750-800 ℃, and the time is preferably 4-6 hours; the temperature of the reduction is preferably 500-600 ℃ and the time is preferably 3-4 hours; the pressure of the primary re-pressing is preferably 5-7T/cm 2 . The inert atmosphere involved in this step may be, in particular, nitrogen, argon or helium, and the reducing atmosphere is typically hydrogen.
In step 5) of the above preparation method, the operations of the secondary sintering, secondary repressing and annealing process are the same as those of the prior art. Specifically, the secondary sintering is carried out in a reducing atmosphere, the sintering temperature is 750-800 ℃, and the sintering time is 4-5 hours; the pressure of the secondary re-compression is preferably 11-12T/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The annealing is carried out in a reducing atmosphere, the annealing temperature is 400-500 ℃ and the annealing time is 1-2 hours.
Compared with the prior art, the invention is characterized in that:
1. copper is used for replacing silver in the welding layer, so that a good silver saving effect is achieved. Copper has physical, chemical, electrical and other properties similar to those of silver, can be used as an electrical contact material, and has the advantages of good electrical and thermal conductivity, large heat capacity, low contact temperature rise, excellent processing and forming properties, low cost and the like. In addition, the invention adopts the powder metallurgy method to prepare the flaky silver-nickel graphite contact, the process is flexible, the size ratio of the silver-nickel graphite to the copper-clad layer can be adjusted according to the requirements of customers, the thickness of the copper-clad layer is increased, copper is a working layer and a welding layer, and a better silver-saving effect can be achieved.
2. The primary press forming pressed compact obtained by press forming the silver-nickel-graphite mixed powder and the copper-copper oxide mixed powder is sintered in inert atmosphere, copper oxide at the bonding interface and graphite contacted with the copper oxide are subjected to oxidation-reduction reaction at high temperature to consume the graphite, and the effect of decarburization of the bonding interface is achieved, so that silver, nickel and copper at the bonding interface are fully contacted, and sintering bonding of the silver, nickel and copper is improved through secondary sintering. By optimizing the process, the influence of graphite on the bonding interface is eliminated, so that the bonding strength of the silver-nickel-graphite-coated copper composite interface is improved.
3. The method has the advantages of strong practicability, simple process, convenient operation, low cost and obvious price advantage of the material.
Drawings
FIG. 1 is a photograph (200X) of a metallographic structure of an AgNi (30) C (3)/Cu contact prepared in example 1 of the present invention;
FIG. 2 is a photograph (200X) of the metallographic structure of AgNi (25) C (2)/Cu contact prepared in example 2 of the present invention;
FIG. 3 is a photograph (200X) of the metallographic structure of AgNi (20) C (2)/Cu contact prepared in example 3 of the present invention;
FIG. 4 is a photograph (200X) of the metallographic structure of AgNi (1.5) C (4)/Cu contact prepared in example 4 of the present invention.
Detailed Description
In order to better explain the technical scheme of the present invention, the present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
1) Weighing silver powder, nickel powder and graphite powder according to the weight ratio of 67:30:3, mixing the powder by using a double-cone mixer at the rotating speed of 30r/min for 3 hours to obtain AgNi (30) C (3) mixed powder;
2) Weighing copper powder of-200 meshes and copper oxide powder of-300 meshes according to the proportion of 0.7:1, mixing the powder by using a double-cone mixer at the rotating speed of 30r/min for 2 hours to obtain copper oxide mixed powder;
3) Pressing and forming the silver-nickel-graphite mixed powder and the copper oxide-copper mixed powder by using a composite automatic tablet press, wherein the forming pressure is 4T/cm 2 ；
4) Placing the blank obtained in the step 3) into a sintering furnace, and sintering at 760+/-10 ℃ by taking nitrogen as a protective gas, wherein the sintering time is 5 hours;
5) Placing the blank processed in the step 4) into a sintering furnace, and reducing at 550 ℃ for 3 hours by taking hydrogen as a protective gas;
6) Re-pressing the blank processed in the step 5) for one time, wherein the re-pressing pressure is 7T/cm 2 ；
7) Placing the blank processed in the step 6) into a sintering furnace, and performing secondary sintering at 760+/-10 ℃ by taking hydrogen as a protective gas, wherein the sintering time is 4 hours;
8) Performing secondary re-pressing on the blank processed in the step 7), wherein the re-pressing pressure is 12T/cm 2 ；
9) And (3) placing the blank processed in the step (8) into a sintering furnace, and annealing at 500 ℃ for 2 hours by taking hydrogen as a protective gas to obtain the flaky AgNi (30) C (3)/Cu contact material.
Example 2
1) Weighing silver powder, nickel powder and graphite powder according to the weight ratio of 73:25:2, mixing the powder by using a double-cone mixer at the rotating speed of 25r/min for 2 hours to obtain AgNi (25) C (2) mixed powder;
2) Weighing copper powder of-200 meshes and copper oxide powder of-300 meshes according to the weight ratio of 0.8:1, mixing the powder by using a double-cone mixer at the rotating speed of 25r/min for 2 hours to obtain copper oxide mixed powder;
3) Pressing and forming the silver-nickel-graphite mixed powder and the copper oxide-copper mixed powder by using a composite automatic tablet press, wherein the forming pressure is 3T/cm 2 ；
4) Placing the blank obtained in the step 3) into a sintering furnace, and sintering at 760+/-10 ℃ for 4 hours by taking nitrogen as a protective gas;
5) Placing the blank processed in the step 4) into a sintering furnace, and reducing at 500 ℃ for 3 hours by taking hydrogen as a protective gas;
6) Re-pressing the blank processed in the step 5) for one time, wherein the re-pressing pressure is 6T/cm 2 ；
7) Placing the blank processed in the step 6) into a sintering furnace, and performing secondary sintering at 760+/-10 ℃ by taking hydrogen as a protective gas, wherein the sintering time is 4 hours;
8) Performing secondary re-pressing on the blank processed in the step 7), wherein the re-pressing pressure is 11T/cm 2 ；
9) And (3) placing the blank processed in the step (8) into a sintering furnace, and annealing at 400 ℃ by taking hydrogen as a protective gas for 1 hour to obtain the flaky AgNi (25) C (2)/Cu contact material.
Example 3
1) Weighing silver powder, nickel powder and graphite powder according to the weight ratio of 78:20:2, mixing the powder by using a double-cone mixer at the rotating speed of 25r/min for 2 hours to obtain AgNi (20) C (2) mixed powder;
2) Weighing copper powder of-200 meshes and copper oxide powder of-300 meshes according to the weight ratio of 0.8:1, mixing the powder by using a double-cone mixer at the rotating speed of 25r/min for 2 hours to obtain copper oxide mixed powder;
3) Pressing and forming the silver-nickel-graphite mixed powder and the copper oxide-copper mixed powder by using a composite automatic tablet press, wherein the forming pressure is 3T/cm 2 ；
4) Placing the blank obtained in the step 3) into a sintering furnace, and sintering at 760+/-10 ℃ for 4 hours by taking nitrogen as a protective gas;
5) Placing the blank processed in the step 4) into a sintering furnace, and reducing at 500 ℃ for 3 hours by taking hydrogen as a protective gas;
6) Re-pressing the blank processed in the step 5) for one time, wherein the re-pressing pressure is 6T/cm 2 ；
7) Placing the blank processed in the step 6) into a sintering furnace, and performing secondary sintering at 760+/-10 ℃ by taking hydrogen as a protective gas, wherein the sintering time is 4 hours;
8) Performing secondary re-pressing on the blank processed in the step 7), wherein the re-pressing pressure is 11T/cm 2 ；
9) And (3) placing the blank processed in the step (8) into a sintering furnace, and annealing at 400 ℃ by taking hydrogen as a protective gas for 1 hour to obtain the flaky AgNi (20) C (2)/Cu contact material.
Example 4
1) Weighing silver powder, nickel powder and graphite powder according to the weight ratio of 94.5:1.5:4, mixing the powder by using a double-cone mixer at the rotating speed of 40r/min for 4 hours to obtain AgNi (1.5) C (4) mixed powder;
2) Weighing copper powder of 300 meshes below zero and copper oxide powder of 200 meshes below zero according to the weight ratio of 0.65:1, mixing the powder by using a double-cone mixer at the rotating speed of 30r/min for 3 hours to obtain copper oxide mixed powder;
3) Pressing and forming the silver-nickel-graphite mixed powder and the copper oxide-copper mixed powder by using a composite automatic tablet press, wherein the forming pressure is 3T/cm 2 ；
4) Placing the blank obtained in the step 3) into a sintering furnace, and sintering at 760+/-10 ℃ by taking nitrogen as a protective gas, wherein the sintering time is 6 hours;
5) Placing the blank processed in the step 4) into a sintering furnace, and reducing at 600 ℃ for 4 hours by taking hydrogen as a protective gas;
6) Re-pressing the blank processed in the step 5) for one time, wherein the re-pressing pressure is 5T/cm 2 ；
7) Placing the blank processed in the step 6) into a sintering furnace, and performing secondary sintering at 760+/-10 ℃ by taking hydrogen as a protective gas, wherein the sintering time is 5 hours;
8) Performing secondary re-pressing on the blank processed in the step 7), wherein the re-pressing pressure is 10T/cm 2 ；
9) And (3) placing the blank processed in the step (8) into a sintering furnace, and annealing at 400 ℃ by taking hydrogen as a protective gas for 1 hour to obtain the flaky AgNi (1.5) C (4)/Cu contact material.
Claims (6)
1. A preparation method of a flaky silver-nickel-graphite copper-clad contact material comprises the following steps:
1) Obtaining silver-nickel-graphite mixed powder;
2) According to (0.65-0.8): 1, weighing copper powder and copper oxide powder in a weight ratio, and mixing the copper powder and the copper oxide powder to obtain copper oxide mixed powder;
3) Pressing and forming the silver-nickel-graphite mixed powder and the copper oxide mixed powder to obtain an initial-press formed pressed compact;
4) The primary pressed compact is firstly placed in inert atmosphere for primary sintering, then placed in reducing atmosphere for reduction, and secondary pressing is carried out again to obtain primary pressed blank;
5) And sequentially performing secondary sintering, secondary repressing and annealing procedures on the obtained primary repressing blank to obtain the flaky silver-nickel-graphite copper-clad contact material.
2. The preparation method of claim 1, wherein in the step 1), the content of graphite in the silver-nickel-graphite mixed powder is 2-4wt% and the content of nickel is 1.5-30wt%.
3. The method of claim 1, wherein in step 2), the copper powder and copper oxide powder have a particle size of 74 microns or less.
4. The method according to claim 1, wherein in the step 4), the temperature of the primary sintering is 750 to 800 ℃ for 4 to 6 hours.
5. The method according to claim 1, wherein in step 4), the reduction is carried out at a temperature of 500 to 600 ℃ for 3 to 4 hours.
6. The method according to claim 1, wherein in step 5), the secondary sintering is performed at a temperature of 750 to 800 ℃ for 4 to 5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310991286.3A CN117004842A (en) | 2023-08-08 | 2023-08-08 | Preparation method of flaky silver-nickel-graphite copper-coated contact material |
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| CN202310991286.3A CN117004842A (en) | 2023-08-08 | 2023-08-08 | Preparation method of flaky silver-nickel-graphite copper-coated contact material |
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