CN118571677A - AgSnO by vacuum ion cladding method2Method for producing contact material - Google Patents
AgSnO by vacuum ion cladding method2Method for producing contact material Download PDFInfo
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- CN118571677A CN118571677A CN202410616387.7A CN202410616387A CN118571677A CN 118571677 A CN118571677 A CN 118571677A CN 202410616387 A CN202410616387 A CN 202410616387A CN 118571677 A CN118571677 A CN 118571677A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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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
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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
- H01H1/04—Co-operating contacts of different material
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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Abstract
The invention relates to a preparation method of AgSnO 2 contact material by vacuum ion cladding, which comprises the steps of preparing vacuum plasma cladding SnO 2 powder, oxidizing and sintering, crushing, granulating and screening to prepare additive-coated SnO 2 powder with specific granularity, and finally mixing, isostatic pressing, sintering, extruding and molding to obtain the required specification. The vacuum plasma cladding method realizes the uniform distribution of additives between Ag and SnO 2 and the maximum realization of the wetting function of the additives; and the metal material has wide requirements on the melting point of the additive metal material, the wettability of the oxide and other performances, and has wide application range. The oxide particles with specific granularity are prepared and perfectly matched with the application conditions of the silver oxide contact material, and the application requirements of different current grades are matched by subdividing the granularity of oxide powder, so that the application range and flexibility of the preparation method are greatly improved.
Description
Technical Field
The invention relates to the field of contact materials, in particular to a preparation method of an AgSnO 2 contact material by a vacuum ion cladding method.
Background
AgSnO 2 contact materials have been increasingly used in electrical appliances instead of AgCdO contacts due to their excellent fusion welding resistance, high electrical life and environmental protection properties, and AgSnO 2 has been primarily done in Western European developed countries to replace AgCdO. Since AgSnO 2 itself has a high contact resistance and SnO 2 tends to accumulate on the working surface after arcing, all studies on AgSnO 2 electrical contact materials have been around the problem of altering wetting between SnO 2 and Ag by additives. The preparation method of the AgSnO 2 contact material is an internal oxidation process, a powder mixing process, a powder pre-oxidation process, a coating process and the like, and the preparation method is as follows:
(1) The invention patent with the application number of CN201210335376.9 discloses a composite silver tin oxide electric contact material and a manufacturing method thereof, and the main principle is that a dispersion mixture of tin oxide and added oxide is prepared and fully mixed with silver solution to prepare the composite silver tin oxide material. The patent adopts a chemical method to prepare the silver metal oxide material, the method realizes the uniform dispersion among the additive, the oxide and the silver, but the chemical method has the problem of environmental pollution, oxide particles are not controlled, and in the subsequent electrical performance application, the oxide particles cannot be properly changed according to different current conditions.
(2) The invention patent with the application number of CN201210439786.8 discloses a preparation method of silver tin oxide, and the main principle is that an oxidizing atmosphere is added in the process of atomizing silver tin alloy powder to realize the oxidation of the powder. The patent adopts an atomization pulverizing process synchronous oxidation process, and oxide particles prepared by the process are relatively fine and dispersed, so that the process is not suitable for high-current-class application.
(3) The preparation method of the silver tin oxide with the application number of CN201110331046.8 by a physical metallurgy coating method mainly comprises the steps of coating an alloy layer on the surface of tin oxide particles by a physical metallurgy method, oxidizing and converting the tin oxide particles into tin oxide particles coated by an additive oxide, and mixing the tin oxide particles with silver powder to obtain the silver tin oxide material. The patent solves the problem of uniform distribution among additives, oxides and silver by adopting physical metallurgy, but the method for melting, wetting and coating the additive metal and the oxide high-temperature sintered metal on the surface of the oxide is only applicable to additive metal materials with lower melting points, is not applicable to high-melting-point metals such as W, mo, and the like, and is also not applicable to materials with lower wettability with the oxide, such as Fe, ni, zn and the like. The patent also does not classify the particle size of the powder and only can be applied to partial current condition materials.
By combining the above, the internal oxidation method is used for preparing AgSnO 2 contact materials, the oxide particles are relatively fine, and the application of high current level cannot be matched; the conventional powder mixing process does not subdivide the granularity of oxide powder, different current levels cannot be used universally, meanwhile, uniform distribution among additives, snO 2 and Ag cannot be realized, and the performance of the additives cannot be optimized. Along with the diversification of the application environments of electrical appliances, the conventional single preparation method of the AgSnO 2 contact material is not applicable any more, and development of a novel preparation method of the AgSnO 2 contact material with wider applicability is needed.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings in the prior art and provides a preparation method of an AgSnO 2 contact material by a vacuum ion cladding method.
The technical scheme adopted by the invention is as follows: a preparation method of AgSnO 2 contact material by a vacuum ion coating method comprises the following steps:
(1) Vacuum ion coating: sequentially coating Me layers on the surfaces of the SnO 2 powder by adopting a vacuum ion coating method to obtain Me/SnO 2 powder;
(2) Oxidizing powder: oxidizing the Me/SnO 2 powder obtained in the step (1) under the condition of oxygen to obtain MeO/SnO 2 powder;
(3) Crushing and granulating: crushing and granulating the MeO/SnO 2 powder obtained in the step (2), and screening to obtain the MeO/SnO 2 powder with the target particle size;
(4) Mixing powder: the target size grade MeO/SnO 2 powder is mixed with Ag powder to prepare AgMeO/SnO 2 powder.
Preferably, in step (1), me is selected from one or more of Cu, bi, W, mo, fe, in, ni, re.
Preferably, in the step (1), the diameter of the SnO 2 powder is 0.1-5 μm, and the thickness of the Me layer is 0.01-0.1 μm.
Preferably, in the step (1), in the powder vacuum ion coating equipment, a Me target material is adopted to prepare a Me layer.
Preferably, in step (2), the oxidation conditions are: the oxygen partial pressure is 0.1-10MPa, the oxidation time is 0-10h, and the oxidation temperature is 400-1300 ℃.
Preferably, in the step (3), the MeO/SnO 2 powder is crushed and granulated by adopting a mechanical crushing and ball milling method.
Preferably, the method further comprises the following steps:
(5) Isostatic pressing: carrying out cold isostatic pressing on the AgMeO/SnO 2 powder prepared in the step (4), and pressing into a spindle;
(6) Sintering: sintering the spindle;
(7) Hot extrusion forming: heating and extruding the sintered spindle;
(8) And (3) material molding processing: the extruded wire or sheet or strip is drawn or rolled into a final product.
Preferably, in the step (5), the isostatic pressure is 50-250Mpa.
Preferably, in the step (6), the sintering temperature is 700-900 ℃ and the sintering time is 2-10 hours, and the sintering atmosphere is vacuum or air or non-reducing atmosphere.
Preferably, in the step (7), the spindle heating temperature is 600-900 ℃ and the extrusion speed is 1-15mm/s.
The beneficial effects of the invention are as follows:
The invention prepares SnO 2 powder coated by vacuum plasma, carries out oxidation sintering, then prepares SnO 2 powder coated by additives with specific granularity through crushing, granulating and sieving, and finally carries out powder mixing, isostatic pressing, sintering, extrusion and molding processing to obtain the required specification. Compared with the traditional silver oxide contact material, the material prepared by the process has higher burning loss resistance, electric transfer resistance and fusion welding resistance, and can meet the requirements of miniaturization and performance superiority of the piezoelectric device; meanwhile, the process is simple, and the method is suitable for batch production. The prepared AgSnO 2 product can be widely applied to relays, contactors and circuit breakers.
Meanwhile, a layer of additive material is wrapped on the surfaces of the SnO 2 particles by a vacuum plasma cladding method, so that the additive is uniformly distributed between Ag and SnO 2, and the wetting function of the additive is maximally realized; the vacuum plasma cladding method has wide requirements on the melting point of the additive metal material, the wettability of the oxide and other performances, and has wide application range.
Furthermore, the oxide particles with specific granularity are prepared and perfectly matched with the application conditions of the silver oxide contact material, when the current grade is low, fine particles are selected to coat SnO 2 powder, when the current grade is medium or the like, medium particles are selected to coat SnO 2 powder, when the current grade is high, coarse particles are selected to coat SnO 2 powder, and the specific particle powder is suitable for the specific current grade material. The application requirements of different current grades are matched by subdividing the granularity of the oxide powder, so that the application range and flexibility of the preparation method are greatly improved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that it is within the scope of the invention to one skilled in the art to obtain other drawings from these drawings without inventive faculty.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent.
Example 1
This example prepares an Ag/Bi 2O3CuO/SnO2 (12) material by the following steps:
s1, preparing a Bi target and a Cu target;
S2, selecting SnO 2 powder with the average granularity of 2.25 mu m, coating a film in vacuum ion plating equipment, and simultaneously plating Bi and Cu films, wherein the thickness of the film is controlled to be 0.02-0.15 mu m, so as to prepare BiCu/SnO 2 powder, and the powder coating rate is more than 90%;
s3, oxidizing BiCu/SnO 2 under the air condition, wherein the temperature is 600 ℃ and the time is 1h, so as to prepare a Bi 2O3CuO/SnO2 block;
S4, mechanically crushing the Bi 2O3CuO/SnO2 block, screening in a fluid powder screening machine, taking powder with the granularity of 3-5 mu m, and warehousing the powder with the rest granularity for use as other condition materials to prepare Bi 2O3CuO/SnO2 powder with the specific granularity;
s5, mixing 17.6kg of atomized Ag powder with the average particle size of 9.8 mu m and 2.4kg of Bi 2O3CuO/SnO2 powder with the average particle size of 3-5 mu m in a three-dimensional dynamic powder mixer for 4 hours to prepare Ag/Bi 2O3CuO/SnO2 (12) powder;
S6, pressing the Ag/Bi 2O3CuO/SnO2 (12) powder into ingots by using cold isostatic pressing equipment, wherein the pressure is 250MPa, and the spindle diameter is 86-88mm, so as to prepare Ag/Bi 2O3CuO/SnO2 (12) powder ingots;
S7, sintering Ag/Bi 2O3CuO/SnO2 (12) powder ingots at 850 ℃ for 4.5 hours under vacuum;
S8, extruding Ag/Bi 2O3CuO/SnO2 (12) at 800 ℃ at an extrusion speed of 2.5-3.5mm/S, wherein the extrusion specification is phi 5.5 or 3 multiplied by 20 strips;
S9, drawing and riveting Ag/Bi 2O3CuO/SnO2 (12) wires to form rivet contacts; the Ag/Bi 2O3CuO/SnO2 (12) strip is processed into sheet contact for contactor by silver coating, rolling, solder coating and punching.
The physical properties of the Ag/Bi 2O3CuO/SnO2 (12) solderable sheet contact and the riveted contact prepared in this example are as follows: the density is 9.9g/cm 3, the resistivity is 2.21 mu omega cm, the hardness (HV 0.3) is 75 (annealed state), the SnO 2 particles are tiny, are suitable for the current condition with the grade of 10-60A, and can resist 30 times of capacitive load on current impact.
Example 2
This example prepares an Ag/In 2O3Bi2O3/SnO2 (14) material by the following steps:
S1, preparing a Bi target and an In target;
S2, selecting SnO 2 powder with the average granularity of 2.25 mu m, coating a film In vacuum ion plating equipment, and simultaneously plating Bi and In films, wherein the thickness of the film is controlled to be 0.05-0.2 mu m, so as to prepare InBi/SnO 2 powder, and the powder coating rate is more than 94%;
S3, oxidizing InBi/SnO 2 under the air condition, wherein the temperature is 600 ℃ and the time is 1h, and preparing an In 2O3Bi2O3/SnO2 block;
S4, mechanically crushing the In 2O3Bi2O3/SnO2 blocks, screening In a fluid screening machine, taking powder with the granularity of 7-10 mu m, and warehousing the powder with the rest granularity for use as other condition materials to prepare In 2O3Bi2O3/SnO2 powder with the specific granularity;
S5, mixing 17.2kg of atomized Ag powder with the average particle size of 9.8 mu m and 2.8kg of In 2O3Bi2O3/SnO2 powder with the average particle size of 7-10 mu m In a three-dimensional dynamic powder mixer for 4 hours to prepare Ag/In 2O3Bi2O3/SnO2 (14) powder;
S6, pressing the Ag/In 2O3Bi2O3/SnO2 (14) powder into ingots by using cold isostatic pressing equipment, wherein the pressure is 250MPa, and the spindle diameter is 86-88mm, so as to prepare Ag/In 2O3Bi2O3/SnO2 (14) powder ingots;
S7, sintering Ag/In 2O3Bi2O3/SnO2 (14) powder ingots at 870 ℃ for 5 hours under vacuum;
S8, ag/In 2O3Bi2O3/SnO2 (14) is extruded at 820 ℃ at an extrusion speed of 15mm/S, and the extrusion specification is 6X 45X L plate;
S9, carrying out procedures of hot rolling silver coating, cold rolling, annealing, solder coating and the like on the Ag/In 2O3Bi2O3/SnO2 (14) plate to manufacture a welded sheet product.
The physical properties of the Ag/In 2O3Bi2O3/SnO2 (14) solder type sheet contact prepared In this example are as follows: the density is 9.85g/cm 3, the resistivity is 2.40 mu omega cm, the hardness (HV 0.3) is 80 (annealed state), and the particles are medium particles coated SnO 2, and the method is suitable for inductive load conditions under the condition of 50-250A.
Example 3
This example prepares an Ag/In 2O3Bi2O3CuOWO3/SnO2 (16) material by the following steps:
S1, preparing a Bi target, a InCu target and a W target;
S2, selecting SnO 2 powder with the average granularity of 4-7 mu m, coating films in vacuum ion plating equipment, and simultaneously plating Bi, inCu films and W films, wherein the thickness of the films is controlled to be 0.1-0.2 mu m, so as to prepare InBiCuW/SnO 2 powder, and the powder coating rate is more than 95%;
S3, inBiCuW/SnO 2 is oxidized under the air condition, the temperature is 800 ℃, the time is 2 hours, and the In 2O3Bi2O3CuOWO3/SnO2 block is prepared;
S4, mechanically crushing the In 2O3Bi2O3CuOWO3/SnO2 blocks, screening In a fluid screening machine, taking powder with the granularity of 12-16 mu m, and warehousing the powder with the rest granularity for special use as other condition materials to prepare In 2O3Bi2O3CuOWO3/SnO2 powder with the specific granularity;
S5, mixing 16.8kg of atomized Ag powder with the average particle size of 9.8 mu m and 3.2kg of screened In 2O3Bi2O3CuOWO3/SnO2 powder with the average particle size of 12-16 mu m In a three-dimensional dynamic powder mixer for 5 hours to prepare Ag/In 2O3Bi2O3CuO WO3/SnO2 (16) powder;
S6, pressing the Ag/In 2O3Bi2O3CuOWO3/SnO2 (16) powder into ingots by using cold isostatic pressing equipment, wherein the pressure is 250MPa, and the spindle diameter is 86-88mm, so as to prepare Ag/In 2O3Bi2O3CuO WO3/SnO2 (16) powder ingots;
S7, sintering Ag/In 2O3Bi2O3CuOWO3/SnO2 (16) powder ingots at the temperature of 880 ℃ for 5 hours under vacuum condition;
S8, ag/In 2O3Bi2O3CuOWO3/SnO2 (16) is extruded at 850 ℃ at an extrusion speed of 15mm/S, wherein the extrusion specification is 6X 45X L plate;
s9, carrying out procedures of hot rolling silver coating, cold rolling, annealing, solder coating and the like on the Ag/In 2O3Bi2O3CuOWO3/SnO2 (16) plate to prepare a welding type offset product.
The physical properties of the Ag/In 2O3Bi2O3CuOWO3/SnO2 (16) solder type sheet contact prepared In this example are as follows: the density is 9.75g/cm 3, the resistivity is 2.50 mu omega cm, the hardness (HV 0.3) is 84 (annealed state), and the particles are coarse coated SnO 2, and the coating is suitable for the condition of inductive load above 250A.
The foregoing disclosure is illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. The preparation method of the AgSnO 2 contact material by the vacuum ion coating method is characterized by comprising the following steps:
(1) Vacuum ion coating: sequentially coating a Me layer and an Ag layer on the surface of the SnO 2 powder by adopting a vacuum ion coating method to obtain Me/SnO 2 powder;
(2) Oxidizing powder: oxidizing the Me/SnO 2 powder obtained in the step (1) under the condition of oxygen to obtain MeO/SnO 2 powder;
(3) Crushing and granulating: crushing and granulating the MeO/SnO 2 powder obtained in the step (2), and screening to obtain the MeO/SnO 2 powder with the target particle size;
(4) Mixing powder: the target size grade MeO/SnO 2 powder is mixed with Ag powder to prepare AgMeO/SnO 2 powder.
2. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method according to claim 1 is characterized in that: in step (1), me is selected from one or more of Cu, bi, W, mo, fe, in, ni, re.
3. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method according to claim 1 is characterized in that: in the step (1), the diameter of the SnO 2 powder is 0.1-5 μm, and the thickness of the Me layer is 0.01-0.1 μm.
4. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method according to claim 1 is characterized in that: in the step (1), in powder vacuum ion coating equipment, a Me target material is adopted to prepare a Me layer.
5. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method according to claim 1 is characterized in that: in the step (2), the oxidation conditions are: the oxygen partial pressure is 0.1-10MPa, the oxidation time is 0-10h, and the oxidation temperature is 400-1300 ℃.
6. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method according to claim 1 is characterized in that: in the step (3), the MeO/SnO 2 powder is crushed and granulated by adopting a mechanical crushing and ball milling method.
7. The method for preparing the AgSnO 2 contact material by using the vacuum ion cladding method according to any one of claims 1 to 6, further comprising the following steps:
(5) Isostatic pressing: carrying out cold isostatic pressing on the AgMeO/SnO 2 powder prepared in the step (4), and pressing into a spindle;
(6) Sintering: sintering the spindle;
(7) Hot extrusion forming: heating and extruding the sintered spindle;
(8) And (3) material molding processing: the extruded wire or sheet or strip is drawn or rolled into a final product.
8. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method as claimed in claim 7, which is characterized in that: in the step (5), the isostatic pressure is 50-250Mpa.
9. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method as claimed in claim 7, which is characterized in that: in the step (6), the sintering temperature is 700-900 ℃ and the sintering time is 2-10 hours, and the sintering atmosphere is vacuum or air or non-reducing atmosphere.
10. The preparation method of the AgSnO 2 contact material by the vacuum ion cladding method as claimed in claim 7, which is characterized in that: in the step (7), the heating temperature of the spindle is 600-900 ℃, and the extrusion speed is 1-15mm/s.
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| CN202410616387.7A CN118571677A (en) | 2024-05-17 | 2024-05-17 | AgSnO by vacuum ion cladding method2Method for producing contact material |
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| CN202410616387.7A CN118571677A (en) | 2024-05-17 | 2024-05-17 | AgSnO by vacuum ion cladding method2Method for producing contact material |
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