CN107740019A - A kind of fine grain silver-based electric contact material and preparation method thereof - Google Patents

A kind of fine grain silver-based electric contact material and preparation method thereof Download PDF

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Publication number
CN107740019A
CN107740019A CN201710981187.1A CN201710981187A CN107740019A CN 107740019 A CN107740019 A CN 107740019A CN 201710981187 A CN201710981187 A CN 201710981187A CN 107740019 A CN107740019 A CN 107740019A
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China
Prior art keywords
silver
contact material
electric contact
fine
molten metal
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CN201710981187.1A
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Inventor
陈晓
张泽忠
吴新合
穆成法
祁更新
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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Priority to CN201710981187.1A priority Critical patent/CN107740019A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/14Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/06Alloys based on silver
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/06Alloys based on silver
    • C22C5/08Alloys based on silver with copper as the next major constituent

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Contacts (AREA)

Abstract

The present invention provides a kind of fine grain silver-based electric contact material and preparation method thereof, and step is:The first step, argent and copper or silver are subjected to melting and insulation with nickel, obtain molten metal;Second step, molten metal is quickly cooled to blank, suppresses crystal grain in alloy structure and grow up;3rd step, blank is pulled out to form wire rod;4th step, is heat-treated to wire rod;5th step, large plastometric set is carried out to the wire rod after heat treatment, obtains fine grain silver-based electric contact material.The present invention combines horizontal casting and severe Plastic Deformation Methods, the silver-based electric contact material of preparation has crystal grain tiny, dense structure, mechanical property is good, and electrical property has a distinct increment, the fields such as autocontrol switch, electrothermal relay, adjuster, thermostat, baking machine, baker timer, computer are can be widely applied to.

Description

Fine-grain silver-based electric contact material and preparation method thereof
Technical Field
The invention relates to the technical field of electric contact materials, in particular to a fine-grain silver-based electric contact material and a preparation method thereof.
Background
The electrical contact material is a key functional material in the switching apparatus, and the performance of the electrical contact material directly affects the safety, reliability and service life of the switching apparatus.
The fine-grained silver is fine-grained silver-based alloy formed by adding a small amount of alloy elements into pure silver, particularly nickel, copper and the like. The fine-grained silver has excellent electrical conductivity and thermal conductivity, very low and stable contact resistance, good welding and processing performances, and higher mechanical strength and temperature resistance than pure silver. Fine-grained silver is one of the most commonly used materials in low-voltage appliances with small capacity at present, such as automatic switches, thermal relays, regulators, thermostats, toasters, oven timers, computers, etc.
At present, the preparation methods of fine-grained silver mainly comprise a fusion casting method and a powder metallurgy method, but the methods have some defects, such as the fusion casting method brings problems of subsequent machining and homogenization treatment, the powder metallurgy method has uneven structure, and the like. For example, in an article "development of fine-grained silver by a powder method" published in the 2 nd phase of 2000 from "electrical alloy", through experimental research on different preparation processes and additive elements, the influence of relevant process factors on the structure and the performance of a fine-grained silver material is discussed, and the powder method is considered to be superior to a smelting method. The above technical problems cannot be solved.
Through searching, reports which are the same as or similar to the subject matter of the invention are not found in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a fine-grain silver-based electric contact material and a preparation method thereof. By adding alloy elements such as copper, nickel and the like into silver and combining the horizontal continuous casting and large plastic deformation technology, the novel fine-grain silver-based electric contact material is prepared, and has the advantages of fine grains, compact structure, good mechanical property and great improvement on electrical property.
According to a first aspect of the present invention, there is provided a method of preparing a fine-grained silver-based electrical contact material, comprising the steps of:
firstly, smelting and insulating metal silver and copper or silver and nickel to obtain molten metal;
secondly, rapidly cooling the molten metal into a blank to inhibit the growth of crystal grains in an alloy structure;
thirdly, drawing the blank to form a wire;
fourthly, carrying out heat treatment on the wire;
and fifthly, performing large plastic deformation on the wire rod after the heat treatment to obtain the fine-grain silver-based electric contact material.
Preferably, in the first step:
the content of silver in the molten metal is 95-99.9 wt%, and the content of copper is 0.1-5 wt%; or
The content of silver in the molten metal is 99.5 wt.% to 99.9 wt.%, and the content of nickel is 0.1 wt.% to 0.5 wt.%.
Preferably, in the first step, the smelting is carried out by adopting a medium-frequency smelting furnace for medium-frequency smelting, the smelting temperature is 1000-1350 ℃, and the heat preservation time is 10-60 min, so that the metal melting and the molten liquid are fully homogenized.
In the second step, the molten metal is rapidly cooled by a crystallizer on the side surface of the bottom of the intermediate frequency smelting furnace through a water cooling device to form a blank.
Preferably, in the third step, the blank is continuously drawn out in the wire specification by the drawing device and is collected to form the wire.
Preferably, in the fourth step, the heat treatment is carried out at a temperature of 450-650 ℃ for 1-5 hours in a protective atmosphere of hydrogen, so that the material is subjected to stress relief and certain physical and mechanical properties are maintained.
Preferably, in the fifth step, the large plastic deformation technique is mainly cutting, extruding or drawing.
According to a second aspect of the present invention, there is provided a fine-grained silver-based electrical contact material obtained by the above-mentioned preparation method, wherein the fine-grained silver-based electrical contact material has a uniform and dense structure, no segregation and aggregation, and the grain size can be controlled within 12 μm, and further, the grain size can be controlled within 4 μm.
Compared with the prior art, the invention has the following beneficial effects:
through the organic coordination among the steps, the invention can solve the technical problem of fine-grained silver preparation in the background technology, wherein: the smelting method is adopted to obtain the homogenized silver-copper or silver-nickel metal solution, so that the defects of uneven tissue distribution and the like are avoided; the molten metal is rapidly cooled to inhibit the growth of crystal grains in an alloy structure; the large plastic deformation is carried out on the wire rod, so that grains in the structure are rearranged and refined, and the prepared silver-based electric contact material is small in grains, compact in structure, good in mechanical property and greatly improved in electrical property.
The material prepared by the invention can be widely applied to the fields of automatic switches, thermal relays, regulators, thermostats, baking machines, oven timers, computers and the like.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a flow chart of a preparation method according to an embodiment of the present invention;
FIG. 2 is a metallographic photograph of a fine grained AgCu3 electrical contact material prepared according to an embodiment of the invention;
fig. 3 is a metallographic photograph of a fine-grained agni0.3 electrical contact material prepared according to an embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
As shown in FIG. 1, the production methods in the following examples of the present invention were carried out according to the procedures shown in FIG. 1.
Example 1
Taking the preparation of fine-grain AgCu3 electrical contact material as an example
1. Weighing 48.5Kg of silver ingot, placing the silver ingot in a medium frequency induction furnace, heating to 1100 ℃ for melting, then adding 1.5Kg of copper block, homogenizing for 40 minutes and preserving heat to obtain silver-copper molten metal;
2. rapidly cooling the molten metal into a formed blank by a crystallizer on the side surface of the bottom of the induction furnace through a water cooling device;
3. continuously pulling out the formed blank by a wire rod with the diameter of 12.5mm by a traction device, and receiving the material to form a coil material to obtain a silver-copper alloy wire rod coil material;
4. carrying out diffusion annealing on the silver-copper alloy wire at the annealing temperature of 600 ℃ for 2h in a protective atmosphere of hydrogen so as to remove stress of the material and maintain certain physical and mechanical properties;
5. and continuously extruding and annealing the wire for multiple times through large plastic deformation to obtain the fine-grain AgCu3 electric contact material with the required specification.
In the embodiment, the extrusion deformation is generally controlled to be 18-30% during extrusion and annealing, the specific deformation depends on the diameter of the extruded wire, the annealing parameters are the same as those of the wire heat treatment in the fourth step, and the protective atmosphere is hydrogen.
In this example, the resulting fine-grained AgCu3 electrical contact material was prepared with a silver content of 97 wt.% and a copper content of 3 wt.%; the properties of the obtained fine-grain AgCu3 electric contact material are as follows: a tensile strength of 466MPa, an elongation of 6%, a hardness of 91HV, a resistivity of 2.51 [ mu ] omega-cm, and a grain size of 1 to 12 [ mu ] m.
Example 2
Taking the preparation of fine-grain AgNi0.3 electrical contact material as an example
1. Weighing 49.85Kg of silver ingot, placing the silver ingot in a medium-frequency induction furnace, heating to 1150 ℃ for melting, then adding 0.15Kg of nickel block, homogenizing for 40 minutes and preserving heat to obtain silver-nickel molten metal;
2. rapidly cooling the molten metal into a formed blank by a crystallizer on the side surface of the bottom of the induction furnace through a water cooling device;
3. continuously pulling out the formed blank by a wire rod with the diameter of 12.5mm by a traction device, and receiving the material to form a coil material to obtain a silver-nickel alloy wire rod coil material;
4. carrying out diffusion annealing on the silver-nickel alloy wire rod, wherein the annealing temperature is 500 ℃, and the annealing time is 2.5 hours, so that the material is subjected to stress relief and certain physical and mechanical properties are kept;
5. and (3) carrying out large plastic deformation on the wire rod through continuous extrusion-annealing, and extruding to the required specification of the product to obtain the fine-grain AgNi0.3 electrical contact material with the diameter of 1.85 mm.
In the embodiment, the extrusion deformation is generally controlled to be 18-30% during extrusion and annealing, the specific deformation depends on the diameter of the extruded wire, the annealing parameters are the same as those of the wire heat treatment in the fourth step, and the protective atmosphere is hydrogen.
In this example, the obtained fine-grained agni0.3 electrical contact material was prepared, in which the silver content was 99.7 wt.% and the nickel content was 0.3 wt.%; the properties of the obtained fine-grain AgNi0.3 electric contact material are as follows: a tensile strength of 256MPa, an elongation of 14%, a hardness of 80HV, a resistivity of 1.88 mu omega cm, and a grain size of 1 to 6 mu m.
Example 3
Taking the preparation of fine-grain AgNi0.15 electrical contact material as an example
1. Weighing 49.925Kg of silver ingot, placing the silver ingot in a medium frequency induction furnace, heating to 1150 ℃ for melting, then adding 0.075Kg of nickel block, homogenizing for 30 minutes and preserving heat to obtain silver-nickel molten metal;
2. rapidly cooling the molten metal into a formed blank by a crystallizer on the side surface of the bottom of the induction furnace through a water cooling device;
3. continuously pulling out the formed blank by a wire rod with the diameter of 12.5mm by a traction device, and receiving the material to form a coil material to obtain a silver-nickel alloy wire rod coil material;
4. carrying out diffusion annealing on the silver-nickel alloy wire rod, wherein the annealing temperature is 460 ℃ and the annealing time is 3h, so that the material is subjected to stress relief and certain physical and mechanical properties are kept;
5. and performing large plastic deformation on the silver-nickel wire rod through multiple times of extrusion-annealing to obtain the phi 1.65mm fine-grain AgNi0.15 electric contact material.
In the embodiment, the extrusion deformation is generally controlled to be 18-30% during extrusion and annealing, the specific deformation depends on the diameter of the extruded wire, the annealing parameters are the same as those of the wire heat treatment in the fourth step, and the protective atmosphere is hydrogen.
In this example, the obtained fine-grained agni0.15 electrical contact material was prepared, in which the silver content was 99.85 wt.% and the nickel content was 0.15 wt.%; the properties of the obtained fine-grain AgNi0.15 electric contact material are as follows: the tensile strength is 201MPa, the elongation is 21%, the hardness is 56HV, the resistivity is 1.72 mu omega cm, and the grain diameter is 1-4 mu m.
As shown in fig. 2, which is a metallographic photograph of a fine-grained AgCu3 electrical contact material prepared according to an embodiment of the present invention, wherein: the tissue distribution is uniform, and no obvious tissue segregation and aggregation exist; the grain size is 1 to 12 μm.
Fig. 3 is a metallographic photograph of a fine-grained agni0.3 electrical contact material prepared according to an embodiment of the present invention, in which: the tissue is uniformly distributed, and the tissue has no segregation and aggregation; the crystal grains are fine and have a grain size of 1 to 6 μm.
The foregoing examples set forth some of the detailed descriptions of the examples of the present invention, but it is to be understood that the invention is not limited to the specific embodiments described above, as there are other embodiments of the invention, such as varying the metal content to any number within the following ranges: the content of silver in the molten metal is 95-99.9 wt.%, the content of copper is 0.1-5 wt.%, or the content of silver in the molten metal is 99.5-99.9 wt.%, and the content of nickel is 0.1-0.5 wt.%; or the values of the variation parameters can be realized within the scope of the claims of the present invention, and various changes or modifications within the scope of the claims by those skilled in the art do not affect the essence of the present invention.

Claims (10)

1. The preparation method of the fine-grain silver-based electric contact material is characterized by comprising the following steps of:
firstly, smelting and insulating metal silver and copper or silver and nickel to obtain molten metal;
secondly, rapidly cooling the molten metal into a blank to inhibit the growth of crystal grains in an alloy structure;
thirdly, drawing the blank to form a wire;
fourthly, carrying out heat treatment on the wire;
and fifthly, performing large plastic deformation on the wire rod after the heat treatment to obtain the fine-grain silver-based electric contact material.
2. The method of producing a fine crystalline silver-based electrical contact material of claim 1 wherein in the first step:
the content of silver in the molten metal is 95-99.9 wt%, and the content of copper is 0.1-5 wt%; or,
the content of silver in the molten metal is 99.5 wt.% to 99.9 wt.%, and the content of nickel is 0.1 wt.% to 0.5 wt.%.
3. The method for preparing the fine crystalline silver-based electric contact material according to claim 1, wherein in the first step, the smelting is carried out by adopting a medium frequency smelting furnace for medium frequency smelting, the smelting temperature is 1000-1350 ℃, and the holding time is 10-60 min, so that the metal melting and the melt liquid are fully homogenized.
4. The method for producing a fine crystalline silver-based electric contact material according to claim 3, wherein in the second step, the molten metal is rapidly cooled by a mold provided in the bottom side of the intermediate frequency melting furnace by means of a water cooling device to form a billet.
5. The method for producing a fine crystalline silver-based electric contact material according to claim 1, wherein in the third step, the ingot is continuously drawn out in a wire size by a drawing means and collected to form a wire.
6. The method for preparing a fine crystalline silver based electric contact material according to claim 5, wherein in the third step, the wire has a diameter of 10 to 20 mm.
7. The method for producing a fine crystalline silver based electrical contact material according to claim 5 wherein in the third step, the wire is received in the form of a coil.
8. A method of producing a fine crystalline silver based electrical contact material as claimed in any one of claims 1 to 7 wherein in the fourth step, said heat treatment wherein: the temperature is 450-650 ℃, the time is 1-5 h, and the protective atmosphere is hydrogen.
9. A method of producing a fine crystalline silver based electrical contact material according to any one of claims 1 to 7 wherein in the fifth step the large plastic deformation is cutting, extruding or drawing to cause rearrangement and refinement of the grains in the structure.
10. A fine-grained silver-based electrical contact material prepared by the method of any one of claims 1 to 9.
CN201710981187.1A 2017-10-20 2017-10-20 A kind of fine grain silver-based electric contact material and preparation method thereof Pending CN107740019A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109594029A (en) * 2018-11-23 2019-04-09 福达合金材料股份有限公司 A kind of preparation method of nickel particle Dispersed precipitate AgNi contact material
CN113238020A (en) * 2021-04-13 2021-08-10 贵研铂业股份有限公司 Method for rapidly researching and developing novel electric contact material
CN114985507A (en) * 2022-04-25 2022-09-02 昆明理工大学 Silver-nickel alloy and preparation method thereof

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CN103614588A (en) * 2013-11-19 2014-03-05 苏州衡业新材料科技有限公司 Preparation method of silver/silver alloy microwire

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109594029A (en) * 2018-11-23 2019-04-09 福达合金材料股份有限公司 A kind of preparation method of nickel particle Dispersed precipitate AgNi contact material
CN109594029B (en) * 2018-11-23 2020-12-25 福达合金材料股份有限公司 Preparation method of AgNi electric contact material with nickel particles dispersed and distributed
CN113238020A (en) * 2021-04-13 2021-08-10 贵研铂业股份有限公司 Method for rapidly researching and developing novel electric contact material
CN114985507A (en) * 2022-04-25 2022-09-02 昆明理工大学 Silver-nickel alloy and preparation method thereof

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