CN102321838A - Method for preparing Ag/SnO2 composite material - Google Patents
Method for preparing Ag/SnO2 composite material Download PDFInfo
- Publication number
- CN102321838A CN102321838A CN201110307129A CN201110307129A CN102321838A CN 102321838 A CN102321838 A CN 102321838A CN 201110307129 A CN201110307129 A CN 201110307129A CN 201110307129 A CN201110307129 A CN 201110307129A CN 102321838 A CN102321838 A CN 102321838A
- Authority
- CN
- China
- Prior art keywords
- sno
- matrix material
- preparation
- sintering
- composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Powder Metallurgy (AREA)
- Manufacture Of Switches (AREA)
Abstract
The invention relates to preparation of silver-based composite materials, and aims to provide a method for preparing an Ag/SnO2 composite material. The method comprises the following steps of: simultaneously dripping ammonia water and an acid aqueous solution of SnCl4.5H2O into a WC suspended aqueous solution with stirring, reacting, filtering and washing, performing vacuum drying, and calcining to obtain core-shell coated structure composite SnO2 particles; performing ball milling on the particles and silver powder and uniformly mixing to obtain mixed powder; performing isostatic pressing on the mixed powder to obtain a blank; and sintering, re-pressing and re-sintering in turn; and performing hot extrusion forming to obtain the Ag/SnO2 composite material. By the Ag/SnO2 composite material prepared by the method, composite particles are ensured to have good characteristics similar to those of SnO2, and a defect of performance degradation caused by component segregation in the using process of the traditional electric contact material can be effectively overcome by regulating a compounding ratio of SnO2 to WC, so that adverse effects of contact resistance increase and temperature rise on electrical usability after long-term use are eliminated.
Description
Technical field
The present invention relates to a kind of preparation method of silver-based composite material, specifically, is a kind of Ag/SnO
2The preparation method of matrix material.
Background technology
Contact material and element are the key foundation of electrical equipment industry, are undertaking the task of connection and breaking current, and its performance directly has influence on break-make capacity, work-ing life and the serviceability of whole set equipment.The Ag/CdO electric contact composite material also begins large-scale application from the fifties; Have anti-electric arc, anti-melting welding, anti-electric and mechanical wear, corrosion-resistant and low contact resistance and good advantages such as processibility; In bigger WV or range of current; All show good electrical contact performance, be called as " omnipotent contact material ", Ag/CdO electric contact composite material decades leading in occupation of market always after this.Get into 21st century, environment protection receives countries in the world day by day and payes attention to, and in February, 2003, European Union issued RoHS instruction and WEEE instruction, and the application that contains the Cd material in the electronic and electrical equipment is limited, and has started the upsurge of the alternative contact material research of Ag/CdO.Over past ten years, the researchist does not have the Cd electric contact composite material around environment-friendly type and has carried out number of research projects, and wherein the most representative is Ag/SnO
2Material.
Usually, Ag/SnO
2Material is to adopt SnO
2Particle and Ag be compound making directly, thus obtained Ag/SnO
2Have anti-preferably arc erosion, anti-melting welding and performance such as wear-resistant.But, because SnO
2Density (6.38g/cm
3) than the density (10.53g/cm of matrix Ag
3) little, at Ag/SnO
2Matrix material is because of behind arc erosion forms little molten bath, SnO
2The meeting come-up is enriched in material surface and forms the not SnO of easy conductive
2Slag causes the contact material contact resistance to increase, and surface temperature rise is too high, the electrical property deterioration.Therefore, improve Ag/SnO through new preparation method
2The microtexture of material with further acquisition better properties, becomes the technical problem that needs to be resolved hurrily.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing contact material system, Ag/SnO is provided
2A kind of new preparation method of matrix material.
Be the technical solution problem, the invention provides a kind of Ag/SnO
2The preparation method of matrix material specifically comprises the steps:
(1) with ammoniacal liquor and pH value is 1～3 SnCl under agitation condition
45H
2It is that the pH value that makes reaction system is 2～4 in 5% the WC aqueous suspension that the acidic aqueous solution of O is added drop-wise to massfraction simultaneously, and the mol ratio of Sn and W is 1: 10～1: 4; After reacting 1～12h under 50～90 ℃ of conditions, with suspension filtered, washing, calcine after the vacuum-drying, obtain to have the composite S nO of nucleocapsid clad structure
2Particle;
(2) with above-mentioned composite S nO
2Particle and silver powder ball mill mixing are even, composite S nO
2Particle accounts for 8%～20% of mixed powder total mass, obtains mixed powder;
(3) powder after will mixing is pressed into base substrate through waiting static pressure, then successively through oversintering, press again, resintering technology, last hot extrusion molding obtains Ag/SnO
2Matrix material.
Among the present invention, calcining temperature is 400～800 ℃ in the said step (1), and calcination time is 2h.
Among the present invention, said composite S nO
2The particle grain size scope is 0.05 μ m～1 μ m, and the particle size range of silver powder is 0.1～50 μ m.
Among the present invention, in the said ball-milling technology of step (2), the rotational speed of ball-mill scope is 50～200r/min, ball-to-powder weight ratio scope 1: 1～10: 1, ball milling time 1～24h.
Among the present invention, wait static pressure pressure 50～500MPa described in the step (3).
Among the present invention, sintering process described in the step (3) is meant sintering under the hydrogen atmosphere protection, 600～900 ℃ of sintering temperatures, sintering time 1～12h.
Among the present invention, multiple compression technology is under 500～800 ℃, to carry out hot pressing described in the step (3), pressure 200～700MPa, soaking time 10～60min.
Among the present invention, resintering technology described in the step (3) is meant under hydrogen atmosphere protection sintering once more, 700～900 ℃ of sintering temperatures, sintering time 1～12h.
Among the present invention, described in the step (3) in the hot extrusion molding technology, 200～700 ℃ of mold preheating temperatures, 300～900 ℃ of blank temperatures, the extrusion ratio scope is 10～200, extrusion speed is 1～10cm/min.
With existing Ag/SnO
2Preparation methods is compared, and the invention has the beneficial effects as follows:
The Ag/SnO for preparing through the present invention
2Matrix material, its SnO
2It is nuclear, SnO that the wild phase particle has with WC
2Microcosmic composite structure for shell.This structure has guaranteed that on the one hand composite particles has and SnO
2Similar good characteristic is on the other hand because WC has higher density (15.63g/cm
3), therefore can be through adjustment SnO
2Make composite S nO with the compositely proportional of WC
2Particle has the density that is complementary with the Ag matrix, thereby effectively overcomes traditional Ag/SnO
2The performance degradation that contact material in use causes because of component segregation, and then eliminate contact contact resistance increase, temperature rise behind life-time service and improve the disadvantageous effect to electric use properties.
Embodiment
Below further present invention is described through instance.
Ag/SnO provided by the invention
2The preparation method of matrix material specifically comprises the steps:
(1) with ammoniacal liquor and pH value is 1～3 SnCl under agitation condition
45H
2It is that the pH value that makes reaction system is 2～4 in 5% the WC aqueous suspension that the acidic aqueous solution of O is added drop-wise to massfraction simultaneously, and the mol ratio of Sn and W is 1: 10～1: 4; After reacting 1～12h under 50～90 ℃ of conditions, with suspension filtered, washing, calcine after the vacuum-drying, obtain to have the composite S nO of nucleocapsid clad structure
2Particle;
(2) with above-mentioned composite S nO
2Particle and silver powder ball mill mixing are even, composite S nO
2Particle accounts for 8%～20% of mixed powder total mass, obtains mixed powder;
(3) powder after will mixing is pressed into base substrate through waiting static pressure, then successively through oversintering, press again, resintering technology, last hot extrusion molding obtains Ag/SnO
2Matrix material.
Testing data among each embodiment sees the following form.
At last, it is also to be noted that what more than enumerate only is part specific embodiment of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (9)
1. Ag/SnO
2The preparation method of matrix material specifically comprises the steps:
(1) with ammoniacal liquor and pH value is 1～3 SnCl under agitation condition
45H
2It is that the pH value that makes reaction system is 2～4 in 5% the WC aqueous suspension that the acidic aqueous solution of O is added drop-wise to massfraction simultaneously, and the mol ratio of Sn and W is 1: 10～1: 4; After reacting 1～12h under 50～90 ℃ of conditions, with suspension filtered, washing, calcine after the vacuum-drying, obtain to have the composite S nO of nucleocapsid clad structure
2Particle;
(2) with above-mentioned composite S nO
2Particle and silver powder ball mill mixing are even, composite S nO
2Particle accounts for 8%～20% of mixed powder total mass, obtains mixed powder;
(3) powder after will mixing is pressed into base substrate through waiting static pressure, then successively through oversintering, press again, resintering technology, last hot extrusion molding obtains Ag/SnO
2Matrix material.
2. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, calcining temperature is 400～800 ℃ in the said step (1), and calcination time is 2h.
3. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, said composite S nO
2The particle grain size scope is 0.05 μ m～1 μ m, and the particle size range of silver powder is 0.1～50 μ m.
4. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, in the said ball-milling technology of step (2), the rotational speed of ball-mill scope is 50～200r/min, ball-to-powder weight ratio scope 1: 1～10: 1, ball milling time 1～24h.
5. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, waits static pressure pressure 50～500MPa described in the step (3).
6. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, sintering process described in the step (3) is meant sintering under the hydrogen atmosphere protection, 600～900 ℃ of sintering temperatures, sintering time 1～12h.
7. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, multiple compression technology is under 500～800 ℃, to carry out hot pressing described in the step (3), pressure 200～700MPa, soaking time 10～60min.
8. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, resintering technology described in the step (3) is meant under hydrogen atmosphere protection sintering once more, 700～900 ℃ of sintering temperatures, sintering time 1～12h.
9. according to the said Ag/SnO of claim 1
2The preparation method of matrix material is characterized in that, described in the step (3) in the hot extrusion molding technology, and 200～700 ℃ of mold preheating temperatures, 300～900 ℃ of blank temperatures, the extrusion ratio scope is 10～200, extrusion speed is 1～10cm/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110307129 CN102321838B (en) | 2011-10-11 | 2011-10-11 | Method for preparing Ag/SnO2 composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110307129 CN102321838B (en) | 2011-10-11 | 2011-10-11 | Method for preparing Ag/SnO2 composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102321838A true CN102321838A (en) | 2012-01-18 |
| CN102321838B CN102321838B (en) | 2013-02-27 |
Family
ID=45449668
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110307129 Expired - Fee Related CN102321838B (en) | 2011-10-11 | 2011-10-11 | Method for preparing Ag/SnO2 composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102321838B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102528055A (en) * | 2012-02-13 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | Preparation method for silver and stannic oxide composite powder and application thereof |
| CN105551811A (en) * | 2016-01-18 | 2016-05-04 | 吉林大学 | SnO2 and TiO2 coated porous Ag@C nanosphere with hierarchical structure, and preparation method and application of nanosphere |
| CN106041061A (en) * | 2016-07-06 | 2016-10-26 | 同济大学 | High-performance low-loss compound magnetic powder core and preparation method thereof |
| CN106181132A (en) * | 2016-07-15 | 2016-12-07 | 哈尔滨工业大学深圳研究生院 | A kind of high-temp solder preparation method based on Ag@Sn nucleocapsid structure |
| CN106636723A (en) * | 2016-12-30 | 2017-05-10 | 衢州学院 | Preparation method of Ag-based electric contact material with La1-xSrxInO3 microspheres as strengthening phase |
| CN108330315A (en) * | 2018-02-13 | 2018-07-27 | 浙江大学 | A kind of superplasticity Ag/SnO2Alloy material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6455358A (en) * | 1987-08-26 | 1989-03-02 | Matsushita Electric Works Ltd | Electric contact material |
| CN1417817A (en) * | 2002-11-05 | 2003-05-14 | 天津大学 | Nano silver-tin oxide electric contact and its prepn |
| CN101649399A (en) * | 2009-07-20 | 2010-02-17 | 温州宏丰电工合金有限公司 | Preparation method of tin-oxygen-silver electric contact material |
-
2011
- 2011-10-11 CN CN 201110307129 patent/CN102321838B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6455358A (en) * | 1987-08-26 | 1989-03-02 | Matsushita Electric Works Ltd | Electric contact material |
| CN1417817A (en) * | 2002-11-05 | 2003-05-14 | 天津大学 | Nano silver-tin oxide electric contact and its prepn |
| CN101649399A (en) * | 2009-07-20 | 2010-02-17 | 温州宏丰电工合金有限公司 | Preparation method of tin-oxygen-silver electric contact material |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102528055A (en) * | 2012-02-13 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | Preparation method for silver and stannic oxide composite powder and application thereof |
| CN102528055B (en) * | 2012-02-13 | 2013-12-04 | 中国科学院宁波材料技术与工程研究所 | Preparation method for silver and stannic oxide composite powder and application thereof |
| CN105551811A (en) * | 2016-01-18 | 2016-05-04 | 吉林大学 | SnO2 and TiO2 coated porous Ag@C nanosphere with hierarchical structure, and preparation method and application of nanosphere |
| CN106041061A (en) * | 2016-07-06 | 2016-10-26 | 同济大学 | High-performance low-loss compound magnetic powder core and preparation method thereof |
| CN106041061B (en) * | 2016-07-06 | 2018-06-26 | 同济大学 | A kind of preparation method of the low-loss composite magnetic powder core of high-performance |
| CN106181132A (en) * | 2016-07-15 | 2016-12-07 | 哈尔滨工业大学深圳研究生院 | A kind of high-temp solder preparation method based on Ag@Sn nucleocapsid structure |
| CN106181132B (en) * | 2016-07-15 | 2018-07-20 | 哈尔滨工业大学深圳研究生院 | A kind of high-temp solder preparation method based on Ag@Sn nucleocapsid structures |
| CN106636723A (en) * | 2016-12-30 | 2017-05-10 | 衢州学院 | Preparation method of Ag-based electric contact material with La1-xSrxInO3 microspheres as strengthening phase |
| CN108330315A (en) * | 2018-02-13 | 2018-07-27 | 浙江大学 | A kind of superplasticity Ag/SnO2Alloy material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102321838B (en) | 2013-02-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102321838B (en) | Method for preparing Ag/SnO2 composite material | |
| CN101651050B (en) | Submicron particle reinforced Ag-based electrical contact material and preparation method thereof | |
| CN102723142B (en) | Preparation method of nickel-based silver conductive slurry | |
| CN104505137A (en) | Conductive copper paste and preparation method and use thereof | |
| CN102312150A (en) | Preparation method of Ag / Ti3SiC2 electric contact composite material | |
| CN102808097A (en) | Silver/nickel/metallic oxide electrical contact material preparation method | |
| CN102737863B (en) | Silver nickel graphite composite contact terminal material and processing method thereof | |
| CN102618773B (en) | Method for preparing Ag/La1-xSrxCoO3 electric contact composite material | |
| CN102683050A (en) | Preparation method of nano Ag-SnO2 electric contact composite | |
| CN104801709A (en) | Nickel-coated copper clad metal powder and preparation method and application thereof | |
| CN106683914B (en) | A kind of low-voltage electrical apparatus copper-based electrical contact material and preparation method thereof | |
| CN107130231B (en) | The preparation method of nanometer metallic silver cladding synthetic fluoromica powder | |
| CN103938193B (en) | A kind of environmental protection high phosphorus chemical plating nickel liquid and application thereof for airtight glass sealing-in line terminals | |
| Li et al. | Electrochemical properties of powder-pressed Pb–Ag–PbO2 anodes | |
| CN102324307B (en) | High-porosity carbon-based composite counter electrode for dye sensitized solar cell and preparation method of high-porosity carbon-based composite counter electrode | |
| CN104889416A (en) | Preparation method of silver tin dioxide intermediate composite powder | |
| CN102912324B (en) | High-stability palladium catalyst concentrated solution and preparation method thereof | |
| CN107720837B (en) | The method for preparing nickel protoxide with waste nickel catalyst | |
| CN109402586B (en) | Preparation method of corrosion-resistant and high-conductivity composite coating for electrode | |
| CN105108150A (en) | Preparation method of silver-copper-oxide electrical contact material | |
| CN104588672A (en) | Preparation method of in-situ doped copper-bearing tin oxide powder and silver tin oxide material | |
| CN103480855A (en) | Preparation method of superfine copper powder for copper paste | |
| CN102568643B (en) | AgSnO contact material and preparation method thereof | |
| CN104402237B (en) | Low-cost electro-conductive glass and preparation method thereof | |
| CN102808098B (en) | Preparation method for silver/nickel/graphite electric contact material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130227 Termination date: 20201011 |