CN101633986B - Method for preparing silver-tungsten composite material - Google Patents
Method for preparing silver-tungsten composite material Download PDFInfo
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- CN101633986B CN101633986B CN200810133294XA CN200810133294A CN101633986B CN 101633986 B CN101633986 B CN 101633986B CN 200810133294X A CN200810133294X A CN 200810133294XA CN 200810133294 A CN200810133294 A CN 200810133294A CN 101633986 B CN101633986 B CN 101633986B
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Abstract
The invention relates to a method for preparing a silver-tungsten composite material. The method for preparing the silver-tungsten composite material comprises the following steps: pressing a mixture containing forming agent and surface modified tungsten into a blank, and then infiltrating and sintering silver and the blank; and the preparation method for the surface modified tungsten comprises the following steps: placing tungsten powder into aqueous solution of silver nitrate, and optically decomposing the silver nitrate. The silver-tungsten composite material prepared by the method, in particular the silver-tungsten composite material with high tungsten content has low resistivity.
Description
Technical field
The invention relates to a kind of preparation method of silver-tungsten composite material.
Background technology
Silver has good conduction and thermal conductivity, thereby is suitable as very much electrical contact material, but easy deliquescing when under hot conditions, using, thereby limited its application.Tungsten then has high rigidity, low conductivity and very low burn out rate.Along with the continuous development of electrical apparatus industry, the composite electric contact material of being made up of silver and tungsten (content of Ag is usually at 20%-80%) has obtained to use widely in electrical equipment such as heavy loading switch, Mgs, isolating switch and tap changer.
When the silver-tungsten composite material of preparation high W content, because the silver and fusing point, the density of tungsten differs greatly, can not the melting manufacturing.If adopt conventional mixed powder, compacting, sintering process, owing to make the finished product alloy phase skewness easily when mixing powder, the inner stress that produces of contact during compacting, easily layering, difficulty is shaped.Therefore, generally adopt the melting infiltration sintering legal system to be equipped with silver-tungsten composite material.In actual applications, high W content silver-tungsten composite material have higher using value, but therefore because silver is relatively poor to the diffusibility of tungsten,, under the situation of low silver content, be difficult to make the material of low-resistivity by melting infiltration sintering.
At " electric locomotive tap changer Ag-W
70Contact material " disclose in (thank sound, powder metallurgy industry, the 10th the 4th phase of volume, in August, 2000,30-33 page or leaf) a kind of with tungsten powder and a certain amount of silver powder and add the method that metal nickel powder carries out melting infiltration sintering on a small quantity.Can improve the wettability of silver by this method, improve the conductive capability that makes material to a certain extent, yet because the nickel that adds is solid-solubilized in the silver, the solid solution defective can play the effect of scattering to the transmission of electronics, has reduced conductive capability tungsten.
Summary of the invention
The objective of the invention is to solve the very difficult high problem of resistivity for preparing the silver-tungsten composite material of silver-tungsten composite material, particularly high W content in the prior art, a kind of preparation method of silver-tungsten composite material is provided with low-resistivity.
The invention provides a kind of preparation method of silver-tungsten composite material, wherein, this method comprises that the mixture that will contain the tungsten of forming agent and surface modification is pressed into blank, then with silver and blank melting infiltration sintering together, the preparation method of the tungsten of described surface modification comprises the aqueous solution that tungsten powder is placed Silver Nitrate, makes the Silver Nitrate photolysis then.
The resistivity of the silver-tungsten composite material of the silver-tungsten composite material, particularly high W content that makes according to method provided by the invention is low.
Embodiment
The preparation method of silver-tungsten composite material provided by the invention comprises, the mixture that will contain the tungsten of forming agent and surface modification is pressed into blank, then with silver and blank melting infiltration sintering together, the preparation method of the tungsten of described surface modification comprises the aqueous solution that tungsten powder is placed Silver Nitrate, makes the Silver Nitrate photolysis then.
Wherein, the weight ratio of tungsten powder and Silver Nitrate can be 1: 0.005-0.08 is preferably 1: 0.01-0.05.
Described tungsten powder can obtain by commercial the purchase, as (Shanghai Weiliang Enterprise Development Co., Ltd., FWC-A).The average particulate diameter of tungsten powder can be the 0.5-100 micron, is preferably the 10-50 micron.
The preparation method of the aqueous solution of described nitrate is an ordinary method.In order to realize purpose of the present invention, the concentration of the aqueous solution of Silver Nitrate can change in a big way, as 0.02-2mol/L, is preferably 0.1-1mol/L.
The method of described photolysis can be the described aqueous solution of rayed with wavelength 200-1064 nanometer, and optimal wavelength is the light wave of 250-400 nanometer.Under the preferable case, described light source can be mercury lamp.Under the preferable case, use 10-10 on average every square centimeter the area
4The light irradiation of milliwatt, irradiation time can be 0.5-10 hour, is preferably 2-5 hour.
Under the preferable case, in irradiation process, can make tungsten powder be in suspended state by stirring.
After making the tungsten of surface modification, can filter and drying it.Filtration and exsiccant method are ordinary method, for conventionally known to one of skill in the art, do not repeat them here.
Described forming agent is thermoplastic low-molecular-weight organic matter, in order to realize purpose of the present invention, can use the forming agent of this area routine, as in polyoxyethylene glycol, polyvinyl alcohol, stearic acid, paraffin, polyethylene, the polyvinyl acetate (PVA) one or more, be preferably in polyvinyl alcohol, stearic acid, the paraffin one or more, the consumption of forming agent does not have particular restriction, can be conventional amount used, as the weight with tungsten powder is benchmark, the content of forming agent can be 1-8 weight %, is preferably 3-6 weight %.
With the tungsten blended method of forming agent and surface modification is ordinary method, for conventionally known to one of skill in the art, for example can use stirring method.
The method of described compacting is conventional method, for example can be in mould with solid, and be to keep the 0.1-10 time of second under the condition of 50-250MPa at pressure.Described Mould design is identical with conventional powder metallurgy, does not repeat them here.
Described melting infiltration sintering is an ordinary method, is high temperature meltability metal or alloy is placed on dystectic skeleton, immerses under capillary force action in the stephanoporate framework at metal or alloy liquid under the high temperature sintering temperature, obtains the dense sintering composite material.Among the present invention, the condition of described melting infiltration sintering can be included in the reducing gas, and temperature is 1050-1250 ℃, keeps 0.5-10 hour time.Wherein, reducing gas can decompose the gas that obtains for hydrogen or ammonia.
The weight ratio of silver and blank can be 0.1-0.35: 1, be preferably 0.15-0.3: 1.The silver that described herein and blank carry out melting infiltration sintering does not together comprise the silver that nitrate coats at tungsten powder surface after photolysis.Silver can exist with block, sheet and form such as Powdered, is preferably Powdered.Described silver can be by commercially available, as the silver powder of east, Leqing city hundred million electrical alloy material factories production.
The present invention will be further described below by specific embodiment.
Embodiment 1
0.3 gram Silver Nitrate is dissolved in 200 ml distilled waters, adds 50 gram tungsten powders (Shanghai Weiliang Enterprise Development Co., Ltd., FWC-A, average particulate diameter are 30 microns), stir.When stirring with 300 watts mercury lamp (500 milliwatts/centimetre
2) shone solution 1 hour.With solid filtering, drying.Add the polyoxyethylene glycol of 2 grams, after mixing, in mould, suppressed 1 second, obtain blank with the pressure of 150 MPas.Getting 14.81 gram thickness is 1.5 millimeters silver strip, and silver strip is contacted with blank, under 1100 ℃ temperature, moltenly in hydrogen atmosphere oozes sintering 3 hours, obtains silver-tungsten composite material A1.
The volume specific resistance test is according to the national standard of GB 5167-1985 (mensuration of sintered metal materials and Wimet resistivity), and the result is as shown in table 1.
Embodiment 2
Make silver-tungsten composite material A2 according to the mode identical with embodiment 1, difference was, uses the Silver Nitrate of 0.6 gram, and the weight of silver strip is 14.62 grams, 1070 ℃ sintering temperatures 8 hours.
Measure the resistivity of silver-tungsten composite material according to the mode identical with embodiment 1, the result is as shown in table 1.
Embodiment 3
Make silver-tungsten composite material A3 according to the mode identical with embodiment 1, difference was, uses the Silver Nitrate of 1 gram, and the weight of silver strip is 14.36 grams, 1100 ℃ sintering temperatures 5 hours.
Measure the resistivity of silver-tungsten composite material according to the mode identical with embodiment 1, the result is as shown in table 1.
Embodiment 4
Make silver-tungsten composite material A4 according to the mode identical with embodiment 1, difference was, uses the Silver Nitrates of 3 grams, and the weight of silver strip is 13.09 grams, 1200 ℃ sintering temperatures 2 hours.
Measure the resistivity of silver-tungsten composite material according to the mode identical with embodiment 1, the result is as shown in table 1.
Comparative Examples 1
50 gram tungsten powders were suppressed in mould 1 second with the pressure of 150 MPas, obtained blank.Getting 15 gram thickness is 1.5 millimeters silver strip, and silver strip is contacted with blank, 1070 ℃ sintering temperatures 8 hours, obtains silver-tungsten composite material B1.
Measure the resistivity of silver-tungsten composite material according to the mode identical with embodiment 1, the result is as shown in table 1.
Comparative Examples 2
50 gram tungsten powders, 2 gram silver powder and 0.5 gram nickel powder are mixed, in mould, suppressed 1 second, obtain blank with the pressure of 150 MPas.Getting 12.5 gram thickness is 1.5 millimeters silver strip, and silver strip is contacted with blank, 1070 ℃ sintering temperatures 8 hours, obtains silver-tungsten composite material B2.
Measure the resistivity of silver-tungsten composite material according to the mode identical with embodiment 1, the result is as shown in table 1.
Comparative Examples 3
50 gram tungsten powders and 3 gram silver powder are mixed, in mould, suppressed 1 second, obtain blank with the pressure of 150 MPas.Getting 12 gram thickness is 1.5 millimeters silver strip, and silver strip is contacted with blank, 1070 ℃ sintering temperatures 8 hours, obtains silver-tungsten composite material B3.
Measure the resistivity of silver-tungsten composite material according to the mode identical with embodiment 1, the result is as shown in table 1.
Comparative Examples 4
50 gram tungsten powders and 0.5 gram nickel powder are mixed, in mould, suppressed 1 second, obtain blank with the pressure of 150 MPas.Getting 14.5 gram thickness is 1.5 millimeters silver strip, and silver strip is contacted with blank, 1070 ℃ sintering temperatures 8 hours, obtains silver-tungsten composite material B4.
Measure the resistivity of silver-tungsten composite material according to the mode identical with embodiment 1, the result is as shown in table 1.
Table 1
| The embodiment numbering | Sample number into spectrum | Resistivity (μ Ω cm) |
| Embodiment 1 | A1 | 3.72 |
| Embodiment 2 | A2 | 3.70 |
| Embodiment 3 | A3 | 3.63 |
| Embodiment 4 | A4 | 3.51 |
| Comparative Examples 1 | B1 | 3.86 |
| Comparative Examples 2 | B2 | 3.80 |
| Comparative Examples 3 | B3 | 3.81 |
| Comparative Examples 4 | B4 | 3.83 |
From the result of table 1 as can be seen, under W content situation about equally, the resistivity of the silver-tungsten composite material A1-A4 that makes according to method provided by the invention is higher than the silver-tungsten composite material B1-B4 that the method according to Comparative Examples 1-4 makes.This explanation makes the low silver-tungsten composite material of resistivity according to method provided by the invention.
Claims (8)
1. the preparation method of a silver-tungsten composite material, it is characterized in that, this method comprises that the mixture that will contain the tungsten powder of forming agent and surface modification is pressed into blank, then with silver and blank melting infiltration sintering together, wherein, the preparation method of the tungsten powder of described surface modification comprises the aqueous solution that tungsten powder is placed Silver Nitrate, makes the Silver Nitrate photolysis then; The weight ratio of described tungsten powder and Silver Nitrate is 1: 0.005-0.08, and the concentration of the aqueous solution of Silver Nitrate is 0.02-2mol/L; The average particulate diameter of described tungsten powder is the 0.5-100 micron.
2. method according to claim 1, wherein, the method for described photolysis comprises with the described aqueous solution of rayed of wavelength 200-1064 nanometer, use 10-10 on every square centimeter area
4The light irradiation of milliwatt, irradiation time are 0.5-10 hour.
3. method according to claim 1, wherein, the weight ratio of silver and blank is 0.1-0.35: 1.
4. method according to claim 1 wherein, in described mixture, is a benchmark with the weight of tungsten powder, and the content of forming agent is 1-8 weight %.
5. according to claim 1 or 4 described methods, wherein, forming agent is one or more in polyoxyethylene glycol, polyvinyl alcohol, stearic acid, paraffin, polyethylene, the polyvinyl acetate (PVA).
6. method according to claim 1, wherein, the condition of described compacting is, at pressure is to keep 0.1-10 second under the condition of 50-250MPa.
7. method according to claim 1, wherein, the condition of melting infiltration sintering is included in the reducing gas and kept 0.5-10 hour under 1050-1250 ℃.
8. method according to claim 7, wherein, reducing gas is that hydrogen or ammonia decompose the gas that obtains.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104209520B (en) * | 2014-09-12 | 2016-05-25 | 福达合金材料股份有限公司 | A kind of preparation method of electrical contact |
| CN107794399B (en) * | 2017-10-13 | 2022-03-15 | 浙江福达合金材料科技有限公司 | Preparation method of superfine high-dispersion silver-tungsten electrical contact material |
| CN107983967A (en) * | 2017-11-06 | 2018-05-04 | 江苏精研科技股份有限公司 | A kind of injection moulding preparation method of AgW electrical contacts |
| CN110129603B (en) * | 2019-04-15 | 2021-03-30 | 福达合金材料股份有限公司 | Method for manufacturing silver-tungsten contact material and product thereof |
| CN110064762B (en) * | 2019-05-21 | 2021-12-14 | 福达合金材料股份有限公司 | Silver tungsten carbide contact material and preparation method thereof |
| CN112170862A (en) * | 2020-09-30 | 2021-01-05 | 桂林金格电工电子材料科技有限公司 | Preparation method of silver-tungsten contact material |
| CN112170861A (en) * | 2020-09-30 | 2021-01-05 | 桂林金格电工电子材料科技有限公司 | Preparation method of silver tungsten carbide contact material |
| CN113245548B (en) * | 2021-05-27 | 2021-10-01 | 攀时（上海）高性能材料有限公司 | Infiltration processing technology and silver-tungsten contact material prepared by same |
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| CN1651590A (en) * | 2005-02-03 | 2005-08-10 | 西安建筑科技大学 | Preparation technology of tungsten copper or tungsten silver composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1651590A (en) * | 2005-02-03 | 2005-08-10 | 西安建筑科技大学 | Preparation technology of tungsten copper or tungsten silver composite material |
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Effective date of registration: 20201116 Address after: 215500 No.13, Caotang Road, Changshu, Suzhou, Jiangsu Province Patentee after: Changshu intellectual property operation center Co.,Ltd. Address before: Room 3a12, building A1, 1983 creative Town, No.29 Nanxin street, Nanling village community, Nanwan street, Longgang District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Chengze Information Technology Co.,Ltd. Effective date of registration: 20201116 Address after: Room 3a12, building A1, 1983 creative Town, No.29 Nanxin street, Nanling village community, Nanwan street, Longgang District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Chengze Information Technology Co.,Ltd. Address before: 518118 Pingshan Road, Pingshan Town, Shenzhen, Guangdong, No. 3001, No. Patentee before: BYD Co.,Ltd. |
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Denomination of invention: A preparation method of silver tungsten composite Effective date of registration: 20211111 Granted publication date: 20110817 Pledgee: Jiangsu Changshu Rural Commercial Bank Co.,Ltd. Fushan sub branch Pledgor: Changshu Huayu Environmental Technology Co.,Ltd. Registration number: Y2021320010464 |