CN114438366A - Preparation method of silver tin oxide indium oxide electric contact material - Google Patents
Preparation method of silver tin oxide indium oxide electric contact material Download PDFInfo
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- CN114438366A CN114438366A CN202111618854.2A CN202111618854A CN114438366A CN 114438366 A CN114438366 A CN 114438366A CN 202111618854 A CN202111618854 A CN 202111618854A CN 114438366 A CN114438366 A CN 114438366A
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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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
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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 relates to the technical field of electric contact materials, in particular to a preparation method of a silver graphite electric contact material. The method comprises the following steps: (1) mixing and smelting silver, tin, indium and nickel to prepare an alloy ingot; (2) coating a silver layer on the surface of the alloy ingot and manufacturing a sheet; (3) and (3) carrying out internal oxidation treatment on the sheet to obtain the electric contact material, wherein an isobaric difference temperature internal oxidation process is adopted, and the isobaric difference temperature internal oxidation process sequentially comprises the following steps: a. constant-pressure low-temperature internal oxidation; b. constant-pressure medium-temperature internal oxidation; c. and (3) carrying out isobaric high-temperature internal oxidation. In the application, through adopting isobaric difference temperature internal oxidation process, the diffusion rate of internal elements to the outside in the internal oxidation process is slowed down, the internal oxidation rate is promoted, the internal oxidation time is shortened by nearly 20%, the uniformity and consistency of the structure and performance of the electric contact material from the surface layer to the central part are improved, and the risk of fusion welding in the use process of an electric appliance is reduced.
Description
Technical Field
The invention relates to the technical field of electric contact materials, in particular to a preparation method of a silver tin oxide indium oxide electric contact material.
Background
The silver cadmium oxide electric contact material plays an important role in the whole low-voltage electric contact material by virtue of comprehensive electrical properties such as unique arc extinguishing property, welding resistance, low and stable contact resistance and the like, but the cadmium element is harmful to human bodies and the environment and is gradually limited to be used or replaced. Silver tin oxide electric contact materials have become an environment-friendly nontoxic electric contact material which is the most promising to replace silver cadmium oxide due to excellent arc erosion resistance, abrasion resistance and welding resistance. The silver tin oxide material is prepared by adopting an internal oxidation method, and a layer of compact tin oxide film can be produced on the surface of the silver tin alloy when the silver tin alloy is oxidized, so that the alloy is prevented from being further oxidized. Research shows that a certain amount of indium is added, so that the blocking effect of a tin oxide film on oxygen atom diffusion can be broken through, the oxidation can be continuously carried out, the oxidation process of the silver-tin alloy can be accelerated, meanwhile, the addition of indium has an influence on the thermal stability of the material and the microstructure of an arc melting zone, and the arc erosion resistance and the fusion welding resistance of the silver-tin oxide contact material can be improved, so that the silver-tin oxide indium oxide is developed into a main electric contact material and is widely applied.
At present, the preparation process of the silver tin oxide indium oxide electric contact material applied to a contactor and a breaker is usually an alloy internal oxidation method. In order to ensure the welding strength between the silver tin oxide and the contact bridge, a pure silver layer needs to be compounded on the welding surface of the contact as a welding silver layer. Patent document CN105551838A discloses a method for processing such silver tin oxide indium oxide sheet-like electrical contact containing additives, which specifically comprises: calculating the required dosage of silver, tin, indium and additives according to the material proportion of the silver tin oxide indium oxide electrical contact to be prepared, and weighing for later use; placing silver, tin, indium and additives in an intermediate frequency smelting furnace to be smelted into molten liquid, casting the molten liquid into an ingot blank, and then obtaining an AgSnIn alloy strip with a certain specification through extrusion and rolling procedures; feeding the pure Ag strip and the obtained AgSnIn alloy strip into a tubular resistance furnace for heating, and feeding the strip from the tubular resistance furnace into a roller for hot rolling and compounding to obtain an AgSnIn/Ag composite strip; the AgSnIn/Ag composite strip is annealed, rolled, stamped and formed and then subjected to internal oxidation treatment.
The application has the following disadvantages: firstly, the internal oxidation process is carried out at the same temperature and the same oxygen pressure, the oxide distribution of the contact material tissue from the surface layer to the center shows a remarkably reduced trend, and the risk that the contact is burnt and damaged and gradually tends to the center from the surface to generate fusion welding or failure in the use process of the electric appliance is increased. Secondly, the hot rolling compounding process of two layers of different materials is in a solid phase diffusion mode, the compounding parameters, the deformation, the cleanness degree of a compounding interface of the two different materials (AgSnIn and Ag) and the like can influence the compounding strength of the interface and the subsequent internal oxidation, the process requirement on the processing process is high, the phenomenon of badness of a product is difficult to find, and the risk that a contact is separated from the compounding interface exists in the using process of an electric appliance. Thirdly, the processing methods need to add the processes of polishing, grinding and hot rolling of the strip besides the process of adding Ag as a welding layer, and have the disadvantages of complex production process, low yield and high production cost.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a silver tin oxide indium oxide electrical contact material.
The technical scheme for solving the problem is to provide a preparation method of the silver tin oxide indium oxide electric contact material, which comprises the following steps:
(1) mixing and smelting silver, tin, indium and nickel to prepare an alloy ingot;
(2) coating a silver layer on the surface of the alloy ingot and manufacturing a sheet;
(3) carrying out internal oxidation treatment on the sheet to obtain an electric contact material;
in the step (3), an isobaric difference temperature internal oxidation process is adopted, and the isobaric difference temperature internal oxidation process sequentially comprises the following steps: a. constant-pressure low-temperature internal oxidation; b. constant-pressure medium-temperature internal oxidation; c. constant-pressure high-temperature internal oxidation; in the steps a, b and c, the oxygen pressure is the same, and the temperature is increased in sequence.
In the application, the isobaric difference temperature internal oxidation process is adopted to be carried out according to isobaric low-temperature internal oxidation, isobaric medium-temperature internal oxidation and isobaric high-temperature internal oxidation in sequence, the diffusion rate of internal elements to the outside in the internal oxidation process is slowed down, the internal oxidation rate is improved, the internal oxidation time is shortened by nearly 20%, the uniformity and consistency of the structure and the performance of the electric contact material from the surface layer to the central part are improved, and the risk that fusion welding or failure occurs when the contact burning loss gradually tends to the center from the surface in the use process of an electric appliance is reduced.
Preferably, the steps a, b and c are as follows: a. isobaric low-temperature internal oxidation: the temperature is 500-600 ℃, and the oxygen pressure is 0.4-2.0 MPa; b. isobaric and medium-temperature internal oxidation: the temperature is 650-720 ℃, and the oxygen pressure is 0.4-2.0 MPa; c. isobaric high-temperature internal oxidation: the temperature is 750-800 ℃, and the oxygen pressure is 0.4-2.0 MPa.
In the process of internal oxidation, oxygen diffuses into the material and tends to diffuse into the gap between the alloy and the silver layer in the composite layer to influence the internal oxidation rate to a certain extent through the composite layer between the alloy and the silver layer, if the alloy and the silver layer are not tightly bonded and the interface bonding strength is low, the oxygen enters the composite layer and tends to diffuse into the gap between the alloy and the silver layer, the diffusion rate and the diffusion amount of the oxygen into the alloy are influenced, and the uniformity of the oxide distribution in the electric contact material is further influenced.
Therefore, as a preferred aspect of the present invention, in the step (1), silver, tin, indium, nickel, and additives including one or more of transition metals and rare earths are mixed and melted to form an alloy ingot. The transition metal and the rare earth have an empty d track, unpaired electrons in the empty d track have extremely high activity, and easily form chemical bonds with silver powder coated with a silver layer subsequently, so that the interface bonding strength between the alloy ingot and the coated silver layer can be improved. Among them, the more the number of unpaired electrons in the d-orbital in the additive increases, the more easily the bond is formed with the silver atom. Preferably, the additive comprises one or more of Cu, Zn, Al, Bi, La, Y and Ce. Preferably, the alloy ingot comprises 5-12% by mass of tin, 2-6% by mass of indium, 0.08-0.5% by mass of nickel, 0.05-1.5% by mass of additives and the balance of silver. In order to enable the components to be completely homogenized and smelted, the smelting and refining temperature is 1050-1150 ℃, and the refining time is 10-30 min. Preferably, the diameter of the prepared alloy ingot is 60-110 mm, and the length of the prepared alloy ingot is 150-550 mm.
In the present invention, in the step (2), the surface of the alloy ingot is subjected to sand blasting and then silver coating. The active surface can be obtained by sand blasting treatment, the adhesive force of the silver powder coated with the silver layer subsequently is further improved, and the effective combination of the interface can be promoted in the subsequent internal oxidation process. Preferably, in the sand blasting treatment, the aluminum oxide abrasive is used for dry sand blasting, the particle size of the aluminum oxide abrasive is 20-150 μm, and the sand blasting pressure is 0.4-1.5 MPa. Further preferably, before sandblasting, turning is performed on the alloy ingots, wherein the turning can eliminate the difference of shrinkage sizes of the alloy ingots in the diameter direction, so that the diameter sizes of the alloy ingots are consistent, and the problem of uneven sandblasting is avoided.
Preferably, in the step (2), the surface of the alloy ingot is coated with the silver layer by adopting an isostatic pressing treatment process. The silver layer is coated on the alloy ingot in an isostatic pressing mode, other impurities cannot be introduced between the alloy ingot and the silver layer, and the interface connection strength between the alloy ingot and the silver layer is ensured. Meanwhile, the powder is filled without an additional isolating device, only the ingot blank needs to be fixed in the isostatic pressure die sleeve in a centering way, the operation is easy, the problems of coating and matching of the silver layer and the alloy ingot are solved, and the thickness of the coated silver layer is uniform and controllable. In the present invention, the isostatic pressure is preferably 50 to 300 MPa. Preferably, in the present invention, the diameter of the silver coated ingot blank obtained after the silver coating is increased by 10 to 25mm with respect to the diameter of the alloy ingot.
Preferably, in step (2), after coating the silver layer on the surface of the alloy ingot, sintering treatment is further performed: the sintering temperature is 600-750 ℃, the sintering time is 2-6 h, and the protective atmosphere is hydrogen. The sintered alloy ingot and the silver are still integrated, foreign matter pollutants influencing the bonding strength cannot be introduced into a composite interface, and the bonding strength of the interface between the alloy ingot and the silver is ensured. In the present invention, it is preferable to perform a hot-pressing treatment after sintering. The ingot blank can generate different degrees of shrinkage along the diameter direction and the length direction due to sintering, the silver-coated ingot blank with a regular shape can be obtained through hot re-pressing treatment, the silver-coated ingot blank is convenient to be subsequently made into a sheet, and the bonding tightness between the silver alloy ingot and the silver coating layer is further improved. The preferable temperature of the hot repressing is 600-750 ℃, and the pressure maintaining time is 20-60 s.
Preferably, in step (2), the alloy ingot is coated with a silver layer on its surface and then hot-pressed in the reverse direction to form a sheet. So as to further improve the reliability and consistency of the bonding strength between the alloy ingot and the cladding silver layer through large deformation extrusion. In the reverse extrusion, because there is no relative motion between the cast ingot surface layer and the inner liner of the extrusion container, the mechanical condition of metal flowing in the extrusion container is changed, the non-uniformity and extrusion force of deformation are reduced, and simultaneously, because the metal flows uniformly, the outer surface layer of the cast ingot can completely enter the surface layer of the extruded product. The heating temperature of the reverse hot extrusion is preferably 600-750 ℃, and the protective atmosphere is hydrogen. After the strip is made by reverse hot extrusion, the strip is preferably trimmed at the end and rolled on a rolling mill to the desired thickness, preferably with at least one intermediate annealing treatment to stabilize the dimensions. Preferably, the annealing is carried out in a hydrogen protective atmosphere at the temperature of 400-600 ℃ for 1-6 h.
The invention has the beneficial effects that:
1. the application improves the isobaric isothermal internal oxidation process in the prior art, and the temperature of internal oxidation is increased in a gradient manner by adopting the isobaric difference isothermal internal oxidation process, so that the diffusion rate of internal elements to the outside in the internal oxidation process is reduced, the internal oxidation rate is increased, the internal oxidation time is shortened by nearly 20%, and the uniformity and consistency of the structure and the performance of the electric contact material from the surface layer to the central part are improved.
2. The silver tin oxide indium oxide electric contact material which has the characteristics of good welding performance, high interface bonding strength, oxide dispersion distribution and needle-shaped structure is prepared by realizing rapid compounding through a reverse hot extrusion method and assisting an isobaric difference temperature internal oxidation technology. The advantages of the reverse hot extrusion composite process and the isobaric differential temperature internal oxidation process are integrated, the size ratio of the silver-tin-indium ingot blank to the silver coating layer can be adjusted according to the requirements of customers, the extrusion ratio is increased, the extrusion specification of the strip is reduced, the production period is shortened, and the yield and the production efficiency are improved.
Drawings
FIG. 1 is a process flow diagram of a method of making a silver tin oxide indium oxide electrical contact material;
fig. 2 is a 200-fold metallographic structure diagram of the electrical contact material prepared in example 1.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
A preparation method of a silver tin oxide indium oxide electric contact material is shown in figure 1, and comprises the following steps:
(1) mixing and smelting silver, tin, indium and nickel to prepare an alloy ingot;
according to the mass parts, 8.1 parts of tin, 3.4 parts of indium, 0.25 part of nickel, 0.05 part of bismuth and 88.2 parts of silver are mixed and then placed in a smelting furnace for smelting, wherein the smelting and refining temperature is 1050 ℃, and the refining time is 30 min. And casting the melted silver alloy after smelting, and performing machining treatment on the surface of the cast ingot to obtain an alloy ingot, wherein the diameter of the alloy ingot is 60mm, and the length of the alloy ingot is 150 mm.
(2) Coating a silver layer on the surface of the alloy ingot and manufacturing a sheet;
sand blasting: and carrying out sand blasting treatment on the surface of the alloy ingot, wherein the sand blasting mode is a dry method, the grain diameter of an alumina abrasive is 20 mu m, and the sand blasting pressure is 0.4 MPa.
Coating silver: and placing the alloy ingot subjected to sand blasting treatment in an isostatic pressing device, and pressing the alloy ingot into a silver-coated ingot blank under 50MPa, wherein the diameter of the silver-coated ingot blank is 85mm, and the length of the silver-coated ingot blank is 150 mm.
And (3) sintering: and sintering the silver-coated ingot blank in a protective atmosphere, wherein the sintering temperature is 600 ℃, the sintering time is 6h, and the protective atmosphere is hydrogen.
Hot repressing: and carrying out hot repressing treatment on the sintered silver-coated ingot blank, wherein the hot repressing temperature is 600 ℃, and the pressure maintaining time is 20 s.
Preparing a sheet: and performing backward hot extrusion after re-pressing treatment to obtain a strip, wherein the heating temperature of an extrusion ingot blank is 600 ℃, and the protective atmosphere is hydrogen. Cutting off the head and the tail of the obtained strip, rolling the strip on a rolling mill to the required thickness, annealing at least once in the middle, and annealing in a hydrogen protective atmosphere at the temperature of 400 ℃ for 6 hours. And finally, punching a sheet by adopting a punching die.
(3) Carrying out internal oxidation treatment on the sheet to obtain an electric contact material;
and treating the obtained sheet by adopting an isobaric difference temperature internal oxidation process according to isobaric low-temperature internal oxidation, isobaric medium-temperature internal oxidation and isobaric high-temperature internal oxidation in sequence to obtain the electric contact material. Wherein the isobaric low-temperature internal oxidation temperature is 500 ℃, and the oxygen pressure is 0.4 MPa; the isobaric medium-temperature internal oxidation temperature is 650 ℃, and the oxygen pressure is 0.4 MPa; the isobaric high-temperature internal oxidation temperature is 750 ℃, and the oxygen pressure is 0.4 MPa.
The metallographic structure diagram of 200 times of the prepared electric contact material is respectively shown in fig. 2, and it can be seen that the electric contact material prepared by the method has the characteristics of oxide dispersion distribution and needle-shaped structure.
Example 2
This embodiment is substantially the same as embodiment 1, except that:
in the step (1), 8.1 parts of tin, 3.4 parts of indium, 0.25 part of nickel and 88.25 parts of silver are mixed according to parts by mass and then placed in a smelting furnace for smelting, wherein the smelting and refining temperature is 1050 ℃ and the refining time is 30 min. And casting the melted silver alloy after smelting, and performing machining treatment on the surface of the cast ingot to obtain an alloy ingot, wherein the diameter of the alloy ingot is 60mm, and the length of the alloy ingot is 150 mm.
Example 3
This embodiment is substantially the same as embodiment 1, except that:
no sand blasting was performed.
Example 4
This embodiment is substantially the same as embodiment 1, except that:
the step (2) is different:
carrying out hot rolling compounding on the pure Ag strip and the strip extruded by the alloy ingot: setting the temperature in a tubular resistance furnace at 600 ℃, introducing hydrogen into the tubular resistance furnace, igniting, feeding pure Ag strips and alloy strips into the tubular resistance furnace for heating, and feeding the strips from the tubular resistance furnace into a roller for hot rolling and compounding to obtain the composite strips. Cutting off the head and the tail of the obtained composite strip, rolling the composite strip on a rolling mill to a required thickness, annealing at least once in the midway, and annealing in a hydrogen protective atmosphere at the temperature of 400 ℃ for 6 hours. And finally, punching a sheet by adopting a punching die.
Example 5
A preparation method of a silver tin oxide indium oxide electric contact material is shown in figure 1, and comprises the following steps:
(1) mixing and smelting silver, tin, indium and nickel to prepare an alloy ingot;
6.4 parts of tin, 3.4 parts of indium, 0.08 part of nickel, 0.8 part of lanthanum and 89.32 parts of silver are mixed according to parts by mass and then placed in a smelting furnace for smelting, wherein the smelting and refining temperature is 1100 ℃, and the refining time is 20 min. And casting the melted silver alloy after smelting, and performing machining treatment on the surface of the cast ingot to obtain an alloy ingot, wherein the diameter of the alloy ingot is 80mm, and the length of the alloy ingot is 350 mm.
(2) Coating a silver layer on the surface of the alloy ingot and manufacturing a sheet;
sand blasting: and carrying out sand blasting treatment on the surface of the alloy ingot, wherein the sand blasting mode is a dry method, the grain diameter of an alumina abrasive is 100 mu m, and the sand blasting pressure is 1.0 MPa.
Coating silver: and placing the alloy ingot subjected to sand blasting treatment in an isostatic pressing device, and pressing the alloy ingot into a silver-coated ingot blank under 200MPa, wherein the diameter of the silver-coated ingot blank is 98mm, and the length of the silver-coated ingot blank is 350 mm.
And (3) sintering: and sintering the silver-coated ingot blank in a protective atmosphere, wherein the sintering temperature is 700 ℃, the sintering time is 4h, and the protective atmosphere is hydrogen.
Hot repressing: and carrying out hot repressing treatment on the sintered silver-coated ingot blank, wherein the hot repressing temperature is 700 ℃, and the pressure maintaining time is 40 s.
Preparing a sheet: and performing backward hot extrusion after re-pressing treatment to obtain a strip, wherein the heating temperature of an extrusion ingot blank is 700 ℃, and the protective atmosphere is hydrogen. Cutting off the head and the tail of the obtained strip, rolling the strip on a rolling mill to the required thickness, annealing at least once in the middle, and annealing in a hydrogen protective atmosphere at the temperature of 550 ℃ for 3 hours. And finally, punching a sheet by adopting a punching die.
(3) Carrying out internal oxidation treatment on the sheet to obtain an electric contact material;
and treating the obtained sheet by adopting an isobaric difference temperature internal oxidation process according to isobaric low-temperature internal oxidation, isobaric medium-temperature internal oxidation and isobaric high-temperature internal oxidation in sequence to obtain the electric contact material. Wherein the isobaric low-temperature internal oxidation temperature is 550 ℃, and the oxygen pressure is 1.5 MPa; the isobaric medium-temperature internal oxidation temperature is 700 ℃, and the oxygen pressure is 1.5 MPa; the isobaric high-temperature internal oxidation temperature is 780 ℃ and the oxygen pressure is 1.5 MPa.
Example 6
A preparation method of a silver tin oxide indium oxide electric contact material is shown in figure 1, and comprises the following steps:
(1) mixing and smelting silver, tin, indium and nickel to prepare an alloy ingot;
mixing 4.0 parts of tin, 3.4 parts of indium, 0.5 part of nickel, 0.5 part of yttrium, 1 part of bismuth and 90.6 parts of silver according to parts by mass, and then putting the mixture into a smelting furnace for smelting, wherein the smelting and refining temperature is 1150 ℃ and the refining time is 10 min. And casting the melted silver alloy after smelting, and performing machining treatment on the surface of the cast ingot to obtain an alloy ingot, wherein the diameter of the alloy ingot is 110mm, and the length of the alloy ingot is 550 mm.
(2) Coating a silver layer on the surface of the alloy ingot and manufacturing a sheet;
sand blasting: and carrying out sand blasting treatment on the surface of the alloy ingot, wherein the sand blasting mode is a dry method, the grain diameter of an alumina abrasive is 150 mu m, and the sand blasting pressure is 1.5 MPa.
Coating silver: and placing the alloy ingot subjected to sand blasting treatment in an isostatic pressing device, and pressing the alloy ingot into a silver-coated ingot blank under the pressure of 300MPa, wherein the diameter of the silver-coated ingot blank is 120mm, and the length of the silver-coated ingot blank is 550 mm.
And (3) sintering: and sintering the silver-coated ingot blank in a protective atmosphere, wherein the sintering temperature is 750 ℃, the sintering time is 2 hours, and the protective atmosphere is argon.
Hot repressing: and carrying out hot repressing treatment on the sintered silver-coated ingot blank, wherein the hot repressing temperature is 750 ℃, and the pressure maintaining time is 60 s.
Preparing a sheet: and performing backward hot extrusion after re-pressing treatment to obtain a strip, wherein the heating temperature of an extrusion ingot blank is 750 ℃, and the protective atmosphere is hydrogen. Cutting off the head and the tail of the obtained strip, rolling the strip on a rolling mill to the required thickness, annealing at least once in the middle, and annealing in a hydrogen protective atmosphere at the temperature of 600 ℃ for 1 h. And finally, punching a sheet by adopting a punching die.
(3) Carrying out internal oxidation treatment on the sheet to obtain an electric contact material;
and treating the obtained sheet by adopting an isobaric difference temperature internal oxidation process according to isobaric low-temperature internal oxidation, isobaric medium-temperature internal oxidation and isobaric high-temperature internal oxidation in sequence to obtain the electric contact material. Wherein the isobaric low-temperature internal oxidation temperature is 600 ℃, and the oxygen pressure is 2.0 MPa; the isobaric medium-temperature internal oxidation temperature is 720 ℃, and the oxygen pressure is 2.0 MPa; the isobaric high-temperature internal oxidation temperature is 800 ℃, and the oxygen pressure is 2.0 MPa.
Comparative example 1
This comparative example is essentially the same as example 1 except that:
and (3) treating the obtained sheet by adopting an isobaric isothermal internal oxidation process to obtain the electric contact material. Wherein the oxidation temperature is 650 ℃ and the oxygen pressure is 0.4 MPa.
[ PROPERTIES DETECTION ]
After the electrical contact materials prepared in the examples and the comparative examples are made into a contact, the AC-4 electrical property parameters of the contact material are detected on an STK-80E type contact material electrical property testing machine. The experimental parameters were as follows: test voltage AC 400V; test current 6X 40A; a power factor of 0.35; the electrifying time is 0.05 s; the operation frequency is 300 times/h.
The results of the measurements are shown in Table 1 below.
Table 1.
As shown in table 1, it can be seen from comparison between example 1 and comparative example 1 that the uniformity of oxide distribution in the contact can be effectively improved by the isobaric and isothermal internal oxidation process, compared with the isobaric and isothermal internal oxidation process, thereby improving the welding resistance of the contact.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of a silver tin oxide indium oxide electric contact material comprises the following steps:
(1) mixing and smelting silver, tin, indium and nickel to prepare an alloy ingot;
(2) coating a silver layer on the surface of the alloy ingot and manufacturing a sheet;
(3) carrying out internal oxidation treatment on the sheet to obtain an electric contact material;
the method is characterized in that: in the step (3), an isobaric difference temperature internal oxidation process is adopted, and the method sequentially comprises the following steps: a. constant-pressure low-temperature internal oxidation; b. constant-pressure medium-temperature internal oxidation; c. constant-pressure high-temperature internal oxidation; in the steps a, b and c, the oxygen pressure is the same, and the temperature is increased in sequence.
2. The method for preparing a silver tin oxide indium oxide electrical contact material according to claim 1, wherein: the steps a, b and c are specifically as follows:
a. isobaric low-temperature internal oxidation: the temperature is 500-600 ℃, and the oxygen pressure is 0.4-2.0 MPa;
b. isobaric and medium-temperature internal oxidation: the temperature is 650-720 ℃, and the oxygen pressure is 0.4-2.0 MPa;
c. isobaric high-temperature internal oxidation: the temperature is 750-800 ℃, and the oxygen pressure is 0.4-2.0 MPa.
3. The method for preparing a silver tin oxide indium oxide electrical contact material according to claim 1, wherein: in the step (1), silver, tin, indium, nickel and additives are mixed and smelted to prepare alloy ingots, and the additives comprise one or more of transition metals and rare earths.
4. The method for preparing an Ag-ITO-InO electrical contact material according to claim 3, wherein the method comprises the following steps: the additive comprises one or more of Cu, Zn, Al, Bi, La, Y and Ce.
5. The method for preparing a silver tin oxide indium oxide electrical contact material according to claim 1, wherein: and (2) performing sand blasting treatment on the surface of the alloy ingot and then performing silver layer coating treatment.
6. The method for preparing an Ag-ITO-InO electrical contact material according to claim 5, wherein: in the sand blasting treatment, aluminum oxide abrasive is adopted for dry sand blasting, the particle size of the aluminum oxide abrasive is 20-150 mu m, and the sand blasting pressure is 0.4-1.5 MPa.
7. The method for preparing a silver tin oxide indium oxide electrical contact material according to claim 1, wherein: and (2) coating a silver layer on the surface of the alloy ingot by adopting an isostatic pressing treatment process.
8. The method for preparing a silver tin oxide indium oxide electrical contact material according to claim 1, wherein: in the step (2), sintering treatment is required after the surface of the alloy ingot is coated with the silver layer.
9. The method for preparing an indium tin oxide silver electrical contact material according to claim 8, wherein: after sintering, hot re-pressing treatment is also needed.
10. The method for preparing a silver tin oxide indium oxide electrical contact material according to claim 1, wherein: and (2) coating a silver layer on the surface of the alloy ingot, and then performing reverse hot extrusion to prepare the sheet.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115537594A (en) * | 2022-10-28 | 2022-12-30 | 台州慧模科技有限公司 | Silver-based electrical contact material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747248A (en) * | 2012-07-20 | 2012-10-24 | 浙江乐银合金有限公司 | Sliver-oxide ternary alloy electrical contact material and production method thereof |
| US20130266468A1 (en) * | 2010-12-30 | 2013-10-10 | Lesheng Chen | Method of Preparing Silver-Based Oxide Electrical Contact Materials with Fiber-like Arrangement |
| CN105551837A (en) * | 2015-12-29 | 2016-05-04 | 桂林电器科学研究院有限公司 | Preparation method of silver-tin oxide-indium oxide flake electrical contact containing additive |
| CN105551838A (en) * | 2015-12-29 | 2016-05-04 | 桂林电器科学研究院有限公司 | Processing method for silver-tin oxide-indium oxide flake electrical contact containing additive |
| CN107794389A (en) * | 2017-10-20 | 2018-03-13 | 温州宏丰电工合金股份有限公司 | A kind of silver-tin oxide or indium oxide contact material and preparation method thereof |
| CN112126810A (en) * | 2020-09-03 | 2020-12-25 | 大都克电接触科技（中国）有限公司 | Preparation method of silver tungsten carbide graphite electrical contact material |
-
2021
- 2021-12-28 CN CN202111618854.2A patent/CN114438366A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130266468A1 (en) * | 2010-12-30 | 2013-10-10 | Lesheng Chen | Method of Preparing Silver-Based Oxide Electrical Contact Materials with Fiber-like Arrangement |
| CN102747248A (en) * | 2012-07-20 | 2012-10-24 | 浙江乐银合金有限公司 | Sliver-oxide ternary alloy electrical contact material and production method thereof |
| CN105551837A (en) * | 2015-12-29 | 2016-05-04 | 桂林电器科学研究院有限公司 | Preparation method of silver-tin oxide-indium oxide flake electrical contact containing additive |
| CN105551838A (en) * | 2015-12-29 | 2016-05-04 | 桂林电器科学研究院有限公司 | Processing method for silver-tin oxide-indium oxide flake electrical contact containing additive |
| CN107794389A (en) * | 2017-10-20 | 2018-03-13 | 温州宏丰电工合金股份有限公司 | A kind of silver-tin oxide or indium oxide contact material and preparation method thereof |
| CN112126810A (en) * | 2020-09-03 | 2020-12-25 | 大都克电接触科技（中国）有限公司 | Preparation method of silver tungsten carbide graphite electrical contact material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115537594A (en) * | 2022-10-28 | 2022-12-30 | 台州慧模科技有限公司 | Silver-based electrical contact material and preparation method thereof |
| CN115537594B (en) * | 2022-10-28 | 2023-04-25 | 台州慧模科技有限公司 | Silver-based electrical contact material and preparation method thereof |
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