CN110976801A - Method for preparing silver tin oxide indium oxide contact material by up-drawing continuous casting process - Google Patents
Method for preparing silver tin oxide indium oxide contact material by up-drawing continuous casting process Download PDFInfo
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- CN110976801A CN110976801A CN201911154306.1A CN201911154306A CN110976801A CN 110976801 A CN110976801 A CN 110976801A CN 201911154306 A CN201911154306 A CN 201911154306A CN 110976801 A CN110976801 A CN 110976801A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/14—Plants for continuous casting
- B22D11/145—Plants for continuous casting for upward casting
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- 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
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
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- 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
- C22C32/001—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 with only oxides
- C22C32/0015—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 with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- 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
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- 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
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
- H01H1/02376—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component SnO2
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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
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Abstract
The invention discloses a method for preparing a silver tin oxide indium oxide contact material by an up-drawing continuous casting process, which comprises the following steps: 1) calculating the required consumption of silver ingots, tin ingots, indium ingots and additives according to the material proportion of the silver tin oxide indium oxide contact to be prepared, and weighing for later use; 2) smelting a silver ingot, a tin ingot and an indium ingot, adding or not adding additives, and carrying out upward continuous casting on the alloy melt obtained by smelting to prepare an alloy wire material; 3) reducing the alloy wire material and drawing the alloy wire material into an alloy wire material; 4) processing the alloy wire into spherical or spheroidal particles; 5) carrying out internal oxidation on the spherical or spheroidal particles to obtain oxidized particles; 6) carrying out vacuum treatment on the oxidized particles; 7) and processing the obtained vacuum-treated particles into finished wires or strips after forming. The invention processes the alloy material into spherical or spheroidal particles and then carries out internal oxidation, thereby being easier to obtain the silver tin oxide indium oxide contact material with uniform tissue.
Description
Technical Field
The invention relates to a preparation method of a silver tin oxide indium oxide contact material, in particular to a method for preparing the silver tin oxide indium oxide contact material by an upward continuous casting process.
Background
A plurality of researches show that the silver tin oxide material is the most promising environment-friendly contact material for replacing silver cadmium oxide and has good application prospect. The silver tin oxide and indium oxide material is an important branch of silver tin oxide series materials, and the products are prepared by adopting an internal oxidation process. In the internal oxidation products, the oxide-poor defects or the structural defects such as oxide aggregation are typical defects which lead to product failure in the commercial production process. Related research works are also carried out by related research institutes and material manufacturers aiming at the problem, the improvement of the process of the internal oxidation method is expected, the defect of poor oxide of the product of the internal oxidation method is overcome to improve the organizational performance of the material, and the representative technology is as follows:
1. the invention patent with publication number CN101950592A (application number 201010275979.5) discloses a method for manufacturing a silver tin oxide indium oxide contact alloy material and an alloy manufactured by the method, wherein the method for manufacturing the silver tin oxide indium oxide contact alloy material comprises the following steps: smelting the silver-tin alloy (Sn5.1-6.8%, In1.5-2.5%, rare earth 1.5-2.5% and Ag in balance) → casting and forming a spindle → rolling → internal oxidation → high-energy crushing treatment after crushing → extrusion → drawing → finished products. The method adopts a high-energy crushing process to achieve the purposes of improving the hot workability of the alloy, refining the crystal grains of the material, ensuring uniform tissue, avoiding segregation in the surrounding structure, eliminating an oxide barren area and effectively improving the compactness of the product and the stability of the contact resistance.
2. Publication No. CN104201020A (Shen)Patent application No. 201410407710.6), discloses a manufacturing process of a silver tin oxide calcium oxide electrical contact and a product thereof, wherein the manufacturing process of the silver tin oxide calcium oxide electrical contact comprises the following steps: smelting → ingot casting → extrusion → drawing to form
The cold heading formed sheet is
Thickness of delta (0.5-3.0) mm → diffusion annealing for 1-8 hours under gas protection state stress diffusion annealing → differential temperature oxidation treatment in an electric furnace for oxidizing and introducing oxygen → finished product. The invention changes the general punching internal oxidation process (smelting, ingot casting, surface treatment, hot rolling covering welding layer, cold rolling, punching forming and reoxidation treatment in the general punching internal oxidation process), and after the sheet-shaped contact is formed by cold heading, the electric contact product is obtained by stress relief diffusion annealing and then differential temperature oxidation treatment. Compared with the general internal oxidation process, the process of plate rolling (hot rolling and welding layer repeating, cold rolling) and punching forming is omitted, the smelting frequency is reduced, the reciprocating turnover of the edge materials is solved, the impurities brought by repeatedly adding the edge materials are reduced, the probability of pollution to a contact substrate is reduced, and the electric conductivity is obviously improved; the material utilization rate is greatly improved (can reach more than 90 percent), and the existing material utilization rate is only 38 to 54 percent, so that the production cost is obviously reduced. On the other hand, the oxidation time is shortened by adopting differential temperature oxidation, so that the oxide is uniformly distributed, the oxide-poor region approaches zero, the oxide concentration is consistent from surface to inside, and the abrasion resistance is obviously enhanced.
3. The invention patent with publication number CN102031438A (application number 201010620247.5) discloses a silver tin oxide electrical contact material and a preparation method thereof, and the specific preparation method comprises the following steps: silver tin smelting (AgSn and additives (any one or more of bismuth, copper, zinc and nickel)) → casting into ingots → extruding → drawing → crushing into alloy wire segments with the length of 10 mm-50 mm → internal oxidation → extruding into wire or plate. The invention achieves the purposes of grain refinement and improved structure uniformity of the material by adding the additive nickel.
4. The invention patent with publication number CN103700544A (application number 201310698853.2) discloses a preparation method of a silver tin oxide electrical contact material with uniform structure, which comprises the following steps: silver ingot, tin ingot and additive → smelting → ingot → surface treatment → extrusion → processing into small-sized wire
Cutting (filament breakage length of 20-30 mm) → pressing (spindle)
) → internal oxidation → repression → surface treatment → processing into wire. The core steps of the method are wire material punching, ingot pressing, internal oxidation, repressing and surface treatment, and are different from the conventional internal oxidation process steps of punching, internal oxidation and ingot pressing. After oxidation, the surface layer of the spindle has continuous oxidation film, silver aggregation and other phenomena, the surface layer is removed through turning treatment, and the internal structure of the spindle is uniform, so that the problems of large amount of silver aggregation, oxide aggregation and the like in the silver tin oxide material are solved, and the material transfer resistance, the electrical service life and the like of the silver tin oxide material in the application of a vehicle-mounted relay are improved.
The process routes of the above patents 1 to 4 are typical alloy internal oxidation processes, and the conventional internal oxidation processes are modified differently to improve the oxide-deficient defects of the conventional internal oxidation processes. However, the applicant has found through analysis that the materials entering the oxidation process of the patents 1 and 2 are in the form of sheets or strips, and the length and thickness of the materials have large size difference, while the materials of the patents 3 and 4 have short shapes but large length-diameter ratio difference, and oxygen diffuses from the surface of the materials to the interior of the materials during internal oxidation, so that the oxygen diffusion path length has large difference, and the final products have oxide-poor areas and uneven material structures.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a silver tin oxide indium oxide contact material by an up-drawing continuous casting process.
The method for preparing the silver tin oxide indium oxide contact material by the upward continuous casting process comprises the following steps:
1) calculating the required consumption of silver ingots, tin ingots, indium ingots and additives according to the material proportion of the silver tin oxide indium oxide contact to be prepared, and weighing for later use;
2) smelting a silver ingot, a tin ingot and an indium ingot, adding or not adding additives, and carrying out up-drawing continuous casting on the alloy melt obtained by smelting to prepare an alloy wire material with the required specification;
3) reducing the alloy wire and drawing to the alloy wire with the required specification;
4) processing the alloy wire into spherical or spheroidal particles;
5) placing the spherical or spheroidal particles in an oxygen-containing atmosphere for internal oxidation to obtain oxidized particles;
6) placing the oxidized particles in a vacuum atmosphere for vacuum treatment to obtain vacuum-treated particles;
7) the obtained particles after vacuum treatment are further processed into finished wire rods or strips after being formed.
In step 1) of the above method, the additive is a conventional choice in the prior art, and specifically may be one or a combination of two or more selected from tellurium (Te), copper (Cu), nickel (Ni), and bismuth (Bi), and the additive is added selectively according to specific needs. In the finally prepared silver tin oxide contact material, the content of each element is as follows by mass percent: 5-10% of Sn, 2-5% of In, 0-1.0% of Te, 0-0.5% of Cu, 0-1.0% of Ni, 0-1.0% of Bi and the balance of Ag.
In step 2) of the above method, the alloy melt is preferably prepared by continuous casting
The alloy wire of (3).
In step 3) of the above method, the above is further performedThe original treatment operation is the same as the prior art, specifically, the treatment is carried out in a hydrogen atmosphere or a hydrogen-nitrogen mixed gas at the temperature of 400-700 ℃, and the reduction treatment time is preferably 3-5 hours. After the reduction treatment is preferably drawn to
Alloy wire rod of
In the step 4) of the method, the spherical or spheroidal particles are processed by the conventional equipment (such as a cold header or a riveting machine), and the diameter of the spherical or spheroidal particles is preferably 2-3.5 mm.
In the step 5) of the method, the internal oxidation operation is the same as that in the prior art, preferably, the internal oxidation operation is carried out under the conditions that the oxygen partial pressure is 0.1-2 MPa and the temperature is 700-800 ℃, and the oxidation time is preferably 20-30 hours.
In the step 6) of the method, the vacuum treatment is preferably performed under the conditions that the vacuum degree is 0.05-0.1 Pa and the temperature is 600-800 ℃, and the time of the vacuum treatment is preferably 3-10 hours.
Compared with the prior art, the invention processes the alloy material into spherical or spheroidal particles and then carries out internal oxidation, thereby effectively reducing the difference of diffusion paths of oxygen from the surface of the material to the inside, and further more easily obtaining the silver tin oxide indium oxide contact material with uniform tissue. On the other hand, because the materials are spherical, the contact between the materials is usually point contact, the contact area is small, the diffusion consistency of oxygen is good, and the material with uniform tissue is easier to obtain. Moreover, the processes of ingot casting peeling, extrusion and the like of the alloy materials in the conventional internal oxidation process are reduced by adopting the upward continuous casting process, the production flow is short, and the efficiency is high.
Drawings
FIG. 1 is a photograph of a metallographic structure of a wire rod finally obtained in example 1 of the present invention.
FIG. 2 is a metallographic structure photograph of a wire rod finally obtained in comparative example 1 of the present invention.
FIG. 3 is a metallographic structure photograph of a sheet finally obtained in example 2 of the present invention.
FIG. 4 is a metallographic structure photograph of a sheet finally obtained in comparative example 2 of the present invention.
FIG. 5 is a metallographic structure photograph of a wire rod finally obtained in example 3 of the present invention.
Detailed Description
The present invention will be better understood from the following detailed description of specific examples, which should not be construed as limiting the scope of the present invention.
Example 1
Weighing silver ingots, tin ingots, indium ingots and tellurium blocks according to the mass ratio of Ag to Sn to In to Te to 91.2 to 5.5 to 2.5 to 0.8, smelting, and carrying out upward continuous casting on the alloy melt obtained by smelting to obtain the alloy melt with the specification of
Then placing the wire material in a hydrogen atmosphere, keeping the temperature of the wire material at 500 ℃ for 2 hours, taking out the wire material and drawing the wire material to the specification
The alloy wire rod of (1) is processed into the wire rod by using a cold header
Placing the spherical particles in an oxygen-containing atmosphere, keeping the temperature for 24 hours under the conditions that the oxygen partial pressure is 0.5MPa and the temperature is 720 ℃, keeping the temperature of the oxidized particles for 2 hours in an environment with the vacuum degree of 0.1Pa and the temperature of 650 ℃, and carrying out compression molding on the particles subjected to vacuum treatment to obtain the spherical particles
Then extruded to specification
The wire material is further drawn into the specification
The wire rod of (1). The metallographic structure of the obtained wire rod is shown in fig. 1.
Comparative example 1
Is repeatedly carried outExample 1, except that: after obtaining the specification of
The alloy wire of (1) is then cut into short wires with a length of 20-30 mm, and the short wires are subjected to subsequent oxidation, extrusion, drawing and other processes.
Comparative example Final
The metallographic structure of the wire rod is shown in fig. 2.
Example 2
Weighing silver ingots, tin ingots, indium ingots and bismuth blocks according to the mass ratio of Ag to Sn to In to Bi of 89.7 to 6.5 to 3.5 to 0.2, smelting, and carrying out up-drawing continuous casting on the obtained alloy melt to obtain the alloy with the specification of
Then placing the wire material in a hydrogen atmosphere, keeping the temperature of the wire material at 600 ℃ for 2 hours, taking out the wire material and drawing the wire material to the specification
The alloy wire rod of (1) is processed into the wire rod by using a cold header
Placing the spherical particles in an oxygen-containing atmosphere, keeping the temperature for 28 hours under the conditions that the oxygen partial pressure is 0.3MPa and the temperature is 750 ℃, keeping the temperature of the oxidized particles for 2 hours in an environment with the vacuum degree of 0.1Pa and the temperature of 650 ℃, and carrying out compression molding on the particles subjected to vacuum treatment to obtain the spherical particles
Then extruded to specification
The wire is further drawn and cold-headed into the specification
The sheet of (1). The metallographic structure of the obtained sheet is shown in fig. 3.
Comparative example 2
Example 2 was repeated except that: after obtaining the specification of
After the alloy wire rod is formed, the wire rod is upset by a cold header to form
The sheet of (2) is subjected to a subsequent oxidation step or the like in the form of a sheet.
The metallographic structure of the sheet finally obtained in this comparative example is shown in FIG. 4.
Example 3
Weighing silver ingots, tin ingots and indium ingots according to the mass ratio of Ag to Sn to In of 92.6 to 5.2 to 2.2, smelting, and carrying out up-drawing continuous casting on the alloy melt obtained by smelting to obtain the alloy with the specification of
Then placing the wire material in a hydrogen atmosphere, keeping the temperature of the wire material at 400 ℃ for 3 hours, taking out the wire material and drawing the wire material to the specification
The alloy wire rod of (1) is processed into the wire rod by using a cold header
Placing the spherical particles in an oxygen-containing atmosphere, keeping the temperature for 20 hours under the conditions that the oxygen partial pressure is 1MPa and the temperature is 790 ℃, keeping the temperature of the oxidized particles for 8 hours in an environment with the vacuum degree of 0.05Pa and the temperature of 600 ℃, and carrying out compression molding on the particles subjected to vacuum treatment to obtain the spherical particles
Then extruded to specification
The wire material is further drawn into the specification
The wire rod of (1). The metallographic structure of the obtained wire rod is shown in fig. 5.
The properties of the finally obtained wire rods or sheets of the above examples 1 to 3 and comparative examples 1 to 2 were measured, and the results are shown in the following Table 1:
TABLE 1
The tensile strength and elongation after fracture in the table are detected according to the JB/T7780.4 standard, the hardness is detected according to the JB/T7780.2 standard, and the density is detected according to the JB/T7780.1 standard.
The data in the table show that the distribution of tensile strength, elongation after fracture and hardness of the material of the invention is more uniform, because the material structure is uniform, and the corresponding properties are more stable.
Claims (5)
1. A method for preparing a silver tin oxide indium oxide contact material by an upward continuous casting process comprises the following steps:
1) calculating the required consumption of silver ingots, tin ingots, indium ingots and additives according to the material proportion of the silver tin oxide indium oxide contact to be prepared, and weighing for later use;
2) smelting a silver ingot, a tin ingot and an indium ingot, adding or not adding additives, and carrying out up-drawing continuous casting on the alloy melt obtained by smelting to prepare an alloy wire material with the required specification;
3) reducing the alloy wire and drawing to the alloy wire with the required specification;
4) processing the alloy wire into spherical or spheroidal particles;
5) placing the spherical or spheroidal particles in an oxygen-containing atmosphere for internal oxidation to obtain oxidized particles;
6) placing the oxidized particles in a vacuum atmosphere for vacuum treatment to obtain vacuum-treated particles;
7) the obtained particles after vacuum treatment are further processed into finished wire rods or strips after being formed.
2. The method of claim 1, wherein: in the step 1), the additive is one or a combination of more than two of tellurium, copper, nickel and bismuth.
3. The method of claim 1, wherein: in the step 3), the reduction treatment is carried out in a hydrogen atmosphere or a hydrogen-nitrogen mixed gas at the temperature of 400-700 ℃.
4. The method of claim 1, wherein: in the step 5), the internal oxidation is carried out under the conditions that the oxygen partial pressure is 0.1-2 MPa and the temperature is 700-800 ℃.
5. The method of claim 1, wherein: in the step 6), the vacuum treatment is carried out under the conditions that the vacuum degree is 0.05-0.1 Pa and the temperature is 600-800 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113500170A (en) * | 2021-07-13 | 2021-10-15 | 桂林金格电工电子材料科技有限公司 | Method for mixing and recycling silver tin oxide indium oxide waste and silver graphite waste |
| CN114086020A (en) * | 2021-10-28 | 2022-02-25 | 浙江福达合金材料科技有限公司 | Preparation method of silver tin oxide electric contact material based on spontaneous thermal oxidation process and product thereof |
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| CN106653410A (en) * | 2016-10-14 | 2017-05-10 | 佛山市诺普材料科技有限公司 | High-performance environment-friendly silver tin oxide electrical contact material and preparation method thereof |
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| US6791045B1 (en) * | 1999-07-07 | 2004-09-14 | Tanaka Kikinzoku Kogyo K.K. | Shielded-type automotive relay controlling a magnet clutch load of a vehicle air-conditioner |
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