CN117127046B - SnO (tin oxide)2@In2O3Preparation method of reinforced silver-based composite material - Google Patents
SnO (tin oxide)2@In2O3Preparation method of reinforced silver-based composite material Download PDFInfo
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- CN117127046B CN117127046B CN202311104105.7A CN202311104105A CN117127046B CN 117127046 B CN117127046 B CN 117127046B CN 202311104105 A CN202311104105 A CN 202311104105A CN 117127046 B CN117127046 B CN 117127046B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 43
- 239000004332 silver Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims description 31
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title description 2
- 229910001887 tin oxide Inorganic materials 0.000 title description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims abstract description 70
- 239000000843 powder Substances 0.000 claims abstract description 46
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000011258 core-shell material Substances 0.000 claims abstract description 13
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 9
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000011159 matrix material Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 description 19
- 239000000463 material Substances 0.000 description 13
- 229910044991 metal oxide Inorganic materials 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 230000007547 defect Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000011257 shell material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
-
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/12—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of wires
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- 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
-
- 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 preparation method of a SnO 2@In2O3 reinforced silver-based composite material. Under the protection of inert gas, mixing commercially available nano SnO 2 with indium powder In proportion, and performing ball milling In a high-energy ball mill to obtain SnO 2 @In powder; uniformly mixing SnO 2 @In powder with silver powder and silver oxide powder according to a proportion, pressing into an ingot blank, and sintering In an In-situ reaction sintering furnace to obtain a SnO 2@In2O3 reinforced silver-based composite material sintered blank; and finally, densifying, extruding and drawing the sintered blank to prepare the wire. The preparation method has the greatest advantages that the SnO 2@In2O3 core-shell structure reinforced silver-based composite material can be obtained through in-situ reaction synthesis, the formed composite material has clean interface and firm interface combination, the synergistic effect of the core-shell structure is greatly exerted, and finally the SnO 2@In2O3 reinforced silver-based composite material with excellent mechanical properties and basically no reduction of conductivity is obtained.
Description
Technical Field
The invention relates to a preparation method of a SnO 2@In2O3 reinforced silver-based composite material, belonging to the field of new electronic information materials.
Background
The contact material in the switch of the piezoelectric device is mainly silver-based composite material, and the earliest developed and applied Ag/CdO electrical contact material is limited to use by European Union ROS instructions because of environmental pollution and harm to human health caused by the existence of element Cd; there is an urgent need to develop novel microstructural-enhanced environment-friendly silver-based composite materials.
The preparation process of the silver metal oxide composite material in the current market comprises the following steps: powder metallurgy, internal oxidation of alloys, and powder pre-oxidation. Powder metallurgy is the most basic silver metal oxide material preparation process, and has simple flow, relatively easy addition of elements and no constraint of material components. However, the simple powder mixing process is difficult to ensure uniform distribution of the reinforcing phase in the silver matrix, and the raw materials are easy to be polluted by the outside in the preparation process, and the defects are numerous, so that the electrical contact performance of the material is deteriorated. Silver metal oxide materials prepared by an internal oxidation method of the alloy often have incomplete oxidation, and the usability of the materials is affected. The powder pre-oxidation method is also one of the powder metallurgy methods, and has the defects that raw materials are easy to be polluted by the outside and have a plurality of defects, so that the electric contact performance of the materials is deteriorated. In order to solve the defects of the traditional preparation process, researchers successively develop novel silver metal oxide material preparation processes such as a chemical coprecipitation method, an electroless plating method, a high-energy ball milling method, a sol-gel method and the like. Although the novel preparation process makes up for the defects of the traditional preparation process to a certain extent, the silver metal oxides prepared by the methods have a larger gap compared with expectations. The main reason is that the silver-based electrical contact material obtained by any preparation method has the comprehensive performance which does not reach the excellent degree of Ag/CdO of the traditional electrical contact material.
Based on the industry background, the invention provides a method for preparing the metal oxide reinforced silver-based material with a core-shell structure by adopting an in-situ reaction synthesis preparation technology. The method has the greatest advantages that the SnO 2@In2O3 core-shell structure reinforced silver-based composite material can be obtained through in-situ reaction synthesis, has good composite material interface cleaning and firm interface combination, greatly exerts the synergistic effect of the core-shell structure, and finally obtains the SnO 2@In2O3 reinforced silver-based composite material with excellent mechanical properties and basically no reduction of conductivity.
Disclosure of Invention
The invention aims to provide a preparation method of a SnO 2@In2O3 reinforced silver-based composite material, which specifically comprises the following steps: mixing commercially available nano SnO 2 with indium powder In proportion under the protection of inert gas, and performing ball milling In a high-energy ball mill to obtain SnO 2 @In powder; uniformly mixing SnO 2 @In powder with silver powder and silver oxide powder according to a proportion, pressing into an ingot blank, and sintering In an In-situ reaction sintering furnace to obtain a SnO 2@In2O3 reinforced silver-based composite material sintered blank; and finally, densifying, extruding and drawing the sintered blank to prepare the wire.
Preferably, the granularity of the commercial nano SnO 2 powder is 40-80 nm, and the purity is 99.9%.
Preferably, the granularity of the indium powder is 0.5-50 mu m, and the purity is 99.9%.
Preferably, the granularity of the silver powder is 10-80 mu m, and the purity is 99.9%.
Preferably, the granularity of the silver oxide powder is 10-50 mu m, and the purity is 99.9%.
Preferably, the mass ratio of the nano SnO 2 to the indium powder is SnO 2: in=12, (0.5-3.5) or 10, (2.5-4.5).
Preferably, the SnO 2 @In powder, silver powder and silver oxide powder are prepared according to the mass percentage of 13% -15% of SnO 2@In2O3 generated In a silver matrix.
Preferably, the ball milling conditions of the invention are as follows: ball milling is carried out for 0.5 to 2 hours at the rotating speed of 400 to 800r/min.
Preferably, the conditions for pressing into ingots according to the present invention are: 150-500MPa.
Preferably, the sintering conditions of the present invention are: heat preservation is carried out for 2h at 100 ℃, then the temperature is raised to 200 ℃, the heat preservation is carried out for 2h, and finally the temperature is raised to 830-840 ℃, and the heat preservation is carried out for 1-2 h.
The method can improve the SnO 2 to strengthen the interface wettability of the silver-based composite material through the characteristic that the shell In 2O3 and silver have good interface wettability, and improves the processing performance and the yield of the silver-based composite material. The obtained SnO 2@In2O3 reinforced silver-based composite material has excellent mechanical properties.
The invention has the beneficial effects that: compared with the traditional silver metal oxide, the metal oxide reinforced silver-based composite material with the SnO 2@In2O3 core-shell structure is prepared; compared with the AgSnO 2 composite material, the composite material not only improves the interface wettability of SnO 2 and silver and improves the processing performance of the composite material, but also obtains the SnO 2@In2O3 core-shell structure reinforced silver-based composite material with excellent mechanical properties.
Drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is a high resolution transmission electron microscope image of the SnO 2@In2O3 core-shell structure reinforced silver-based composite material prepared in example 1.
Detailed description of the preferred embodiments
The invention is further illustrated in the following in connection with the accompanying drawings and examples, but the scope of the invention is not limited to the examples.
Example 1
As the process flow of fig. 1, commercially available nano SnO 2 and In powder are mixed according to SnO 2: mixing in=12:2.6 ratio (mass ratio), and ball milling for 0.5h under the protection of inert argon at the rotating speed of 400r/min to obtain SnO 2 @In powder; then preparing SnO 2 @In powder, silver powder and silver oxide powder according to the condition that 14.8% (mass percent) of SnO 2@In2O3 is generated In a silver matrix, and ball milling for 1h at the rotating speed of 300r/min to obtain uniformly mixed composite powder; putting the composite powder into a mould, forming under the condition of 350MPa pressing pressure, putting the formed ingot blank into an in-situ reaction sintering furnace, and sintering according to the sintering process of 100 ℃ (heat preservation 2 h) →200 ℃ (heat preservation 2 h) →300 ℃ (heat preservation 2 h) →830 ℃ (heat preservation 1 h) to obtain a SnO 2@In2O3 reinforced silver-based composite material sintered blank; finally, densifying, extruding and drawing the sintered blank to prepare a wire; by the process, the silver metal oxide composite material with the tensile strength reaching 390MPa can be obtained.
As can be seen from fig. 2, the intermediate particles are SnO 2, the tin oxide is surrounded by In 2O3, and the core-shell material reinforced silver-based composite material with In 2O3 coating SnO 2 is prepared In this embodiment.
Example 2
As the process flow of fig. 1, commercially available nano SnO 2 and In powder are mixed according to SnO 2: mixing in=12:0.5 ratio (mass ratio), and ball milling for 2 hours under the protection of inert argon at the rotating speed of 400r/min to obtain SnO 2 @In powder; then SnO 2 @In powder, silver powder and silver oxide powder are prepared according to the condition that 14% (mass percent) of SnO 2@In2O3 is generated In a silver matrix, and ball milling is carried out for 1.5 hours at the rotating speed of 200r/min to obtain uniformly mixed composite powder; putting the composite powder into a mould, forming under the condition of 350MPa pressing pressure, putting the formed ingot blank into an in-situ reaction sintering furnace, and sintering according to the sintering process of 100 ℃ (heat preservation 2 h) →200 ℃ (heat preservation 2 h) →390 ℃ (heat preservation 2 h) →840 ℃ (heat preservation 1 h) to obtain a SnO 2@In2O3 reinforced silver-based composite material sintered blank; and finally, densifying, extruding and drawing the sintered blank to prepare the wire. By the process, the silver metal oxide composite material with the tensile strength reaching 380MPa can be obtained.
Example 3
As the process flow of fig. 1, commercially available nano SnO 2 and Cu powder are mixed according to SnO 2: mixing in=10:3.6 ratio (mass ratio), and ball milling for 1.5h under the protection of inert argon at the rotating speed of 500r/min to obtain SnO 2 @In powder; then SnO 2 @In powder, silver powder and silver oxide powder are prepared according to the condition that about 15% (mass percent) of SnO 2@In2O3 is generated In a silver matrix, and ball milling is carried out for 1h at the rotating speed of 400r/min to obtain uniformly mixed composite powder; putting the composite powder into a mould, forming under the condition of 500MPa pressing pressure, putting the formed ingot blank into an in-situ reaction sintering furnace, and sintering according to a sintering process of 100 ℃ (heat preservation for 2 h), 200 ℃ (heat preservation for 2 h), 400 ℃ (heat preservation for 1 h), 820 ℃ (heat preservation for 1.5 h), so as to obtain a SnO 2@In2O3 reinforced silver-based composite material sintered blank; and finally, densifying, extruding and drawing the sintered blank to prepare the wire. By the process, the silver metal oxide composite material with the tensile strength reaching 385MPa can be obtained.
Example 4
As the process flow of fig. 1, commercially available nano SnO 2 and Cu powder are mixed according to SnO 2: mixing in=10:2.6 ratio (mass ratio), and ball milling for 1h under the protection of inert argon at the rotating speed of 200r/min to obtain SnO 2 @In powder; then SnO 2 @In powder, silver powder and silver oxide powder are prepared according to the condition that about 13% (mass percent) of SnO 2@In2O3 is generated In a silver matrix, and ball milling is carried out for 1h at the rotating speed of 500r/min to obtain uniformly mixed composite powder; putting the composite powder into a mould, forming under the pressing pressure of 450MPa, putting the formed ingot blank into an in-situ reaction sintering furnace, and sintering according to the sintering process of 100 ℃ (heat preservation for 2 h), 200 ℃ (heat preservation for 2 h), 600 ℃ (heat preservation for 1 h), 830 ℃ (heat preservation for 2 h) to obtain a SnO 2@In2O3 reinforced silver-based composite material sintered blank; and finally, densifying, extruding and drawing the sintered blank to prepare the wire. By the process, the silver metal oxide composite material with the tensile strength reaching 370MPa can be obtained.
Claims (7)
1. The preparation method of the SnO 2@In2O3 reinforced silver-based composite material is characterized by comprising the following steps of: mixing commercially available nano SnO 2 with indium powder In proportion under the protection of inert gas, and ball milling In a high-energy ball mill to obtain SnO 2 @In powder with a core-shell structure; uniformly mixing SnO 2 @In powder with a core-shell structure with silver powder and silver oxide powder according to a proportion, pressing into an ingot blank, and sintering In an In-situ reaction sintering furnace to obtain a SnO 2@In2O3 reinforced silver-based composite material sintered blank with a core-shell structure; finally, densifying, extruding and drawing the sintered blank to prepare a wire;
The granularity of the commercial nano SnO 2 powder is 40-80 nm, the granularity of the indium powder is 0.5-50 mu m, the granularity of the silver powder is 10-80 mu m, the granularity of the silver oxide powder is 10-50 mu m,
The mass ratio of the nano SnO 2 to the indium powder is SnO 2: in=12, (0.5-3.5) or 10, (2.5-4.5);
SnO 2 @In powder with a core-shell structure and silver powder, and silver oxide powder are prepared according to the condition that 13-15 mass percent of SnO 2@In2O3 is generated In a silver matrix;
The ball milling conditions are as follows: ball milling is carried out for 0.5 to 2 hours at the rotating speed of 400 to 800 r/min.
2. The method for preparing the SnO 2@In2O3 reinforced silver-based composite material according to claim 1, characterized in that: the purity of the commercial nano SnO 2 powder is 99.9%.
3. The method for preparing the SnO 2@In2O3 reinforced silver-based composite material according to claim 1, characterized in that: the purity of the indium powder was 99.9%.
4. The method for preparing the SnO 2@In2O3 reinforced silver-based composite material according to claim 1, characterized in that: the purity of the silver powder was 99.9%.
5. The method for preparing the SnO 2@In2O3 reinforced silver-based composite material according to claim 1, characterized in that: the purity of the silver oxide powder was 99.9%.
6. The method for preparing the SnO 2@In2O3 reinforced silver-based composite material according to claim 1, characterized in that: the conditions for pressing into the ingot blank are as follows: 150-500MPa.
7. The method for preparing the SnO 2@In2O3 reinforced silver-based composite material according to claim 1, characterized in that: the sintering conditions are as follows: and (3) preserving heat for 2 hours at 100 ℃, then raising the temperature to 200 ℃, preserving heat for 2 hours, and finally raising the temperature to 830-840 ℃ and preserving heat for 1-2 hours.
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2023
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反应合成AgSnO_2电接触材料烧结坯的显微组织分析;吴春萍, 陈敬超, 鲜春桥, 李玉华;电工材料;20040320(第01期);全文 * |
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