CN103695682A - Sliver oxide contact material with base body performance-strengthening additives as well as preparation method and product thereof - Google Patents

Sliver oxide contact material with base body performance-strengthening additives as well as preparation method and product thereof Download PDF

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Publication number
CN103695682A
CN103695682A CN201310700969.5A CN201310700969A CN103695682A CN 103695682 A CN103695682 A CN 103695682A CN 201310700969 A CN201310700969 A CN 201310700969A CN 103695682 A CN103695682 A CN 103695682A
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powder
oxide
additive
silver
substrate performance
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CN103695682B (en
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刘立强
颜小芳
鲁香粉
翁桅
柏小平
林万焕
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Zhejiang Fuda Alloy Materials Technology Co Ltd
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Fuda Alloy Materials Co Ltd
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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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • C22C1/0466—Alloys based on noble metals
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
    • B22F2009/0828—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid with water
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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

Abstract

The invention discloses a preparation method of a sliver oxide contact material with base body performance-strengthening additives and a product thereof. The preparation method comprises the following steps: preparing an additive alloy with strengthening performance, oxide powder, other additive powder and a sliver ingot which are used as raw materials into powder by water atomization, mixing powder, pressing an ingot, sintering, extruding and finally drawing or rolling to prepare a contact material finished product. The sliver oxide contact material disclosed by the invention has a sliver base body with good electrical performance and mechanical performance, oxide particles and other additive materials are uniformly dispersed in the sliver base body, so that the contact material is ensured to have the characteristics of being uniform and stable in electrical performance, good in processing performance, and the like. Compared with the conventional sliver oxide contact material, the material prepared by the process in the invention has higher burning loss resistance, electro-transfer resistance and fusion welding resistance, can satisfy volume miniaturization and performance optimization needs of a low-voltage electrical appliance. Moreover, the process disclosed by the invention is simple and suitable for mass production. The prepared silver oxide product can be widely applied to a relay, a contact and a circuit breaker.

Description

A kind of silver oxide contact material with enhancing substrate performance additive and preparation method and products thereof
Technical field
The present invention relates to a kind of contact material and preparation method, especially a kind of silver oxide contact material with enhancing substrate performance additive and preparation method and products thereof.
Background technology
Silver oxide contact material is applied in low-voltage apparatus the most extensive, especially in the contactor, rly. of large current class.Conventional silver oxide contact material is that simple silver and " pseudoalloy " mode of oxide compound exist, and oxide compound is dispersed in around fine silver matrix.The preparation method of comparatively common silver oxide contact material is internal oxidation process, blending processes of powders, powder pre-oxidation process and cladding process etc.These techniques all adopt adds oxide compound mode and improves the wetting situation between silver matrix and stannic oxide, as following patent:
CN201210335376.9 composite silver silver-tin oxide electric contact material and manufacture method thereof, cardinal principle is to prepare stannic oxide and the dispersed mixture that adds oxide compound, more fully mixes with silver-colored solution, prepares composite silver stannic oxide materials.
The preparation method of a CN201210439786.8 siller tin oxide, cardinal principle is to add oxidizing atmosphere in silver-colored stannum alloy powder atomization process, realizes the oxidation of powder.
The preparation method of CN201110331046.8 silver-stannic oxide by using physical metallurgical coating method, cardinal principle is at the coated one deck alloy layer in granules of stannic oxide surface by physical metallurgy method, then in oxidation conversion, become to add the coated granules of stannic oxide of oxide compound, mix with silver powder again, thereby obtain silver tin oxide material.
This type of patent is all that silver is body material above, by adding additive, improve electrical property or improve the dispersed electrical property that improves of oxide particle, these patents or technology all cannot improve the electrical property of silver matrix, and in the working process of contact, loaded current and arcing maximum be silver matrix.Because silver matrix performance does not have larger lifting, thus greatly limited the high current impulse withstanding capability of contact material, anti-DC condition under material transfer performance and the performance of anti-contact melted etc.
At China, along with the raising day by day of people's living standard, various electrical equipment is also more and more, and electrical equipment is also developing to miniaturization.This just requires low-voltage apparatus need to adapt to more loadtype, adapts to higher current class etc., and this just requires contact material can meet higher rush of current performance, larger electric arc supporting capacity and less welding tendency.Conventional silver oxide contact material is not solving under the prerequisite of silver matrix performance, just relies on the change of type or the variation of composition of oxide compound, is difficult to meet the demands.
Summary of the invention
The object of the invention is the shortcoming and defect existing in order to overcome prior art, and a kind of preparation method with strengthening the silver oxide contact material of substrate performance additive is provided, by the method can provide the high current impulse withstanding capability of matrix, anti-DC condition under material transfer performance and the performance of anti-contact melted.
For achieving the above object, technical scheme of the present invention is that raw material is oxidate powder, strengthen substrate performance additive, the second additive powder, surplus is silver, the second additive can be one or more combinations in Tungsten oxide 99.999, oxide compound molybdenum, rare earth oxide, Indium sesquioxide, nickel oxide, tellurium oxide, cupric oxide, bismuth oxide, strengthen substrate performance additive and be bismuth, copper, indium, rare earth element, magnesium and zinc etc. any or several arbitrarily, it is characterized in that making step is as follows successively:
(1) water atomization pulverization
By silver and the melting of enhancing substrate performance additive alloy process, water atomization, be prepared into the silver powder that increases substrate performance
(2) mixed powder
Silver powder and oxidate powder, the second additive powder with strengthening substrate performance additive are prepared into powder mix by blending processes of powders
(3) isostatic cool pressing
The powder mix of preparation is carried out to isostatic cool pressing, be pressed into ingot;
(4) sintering
To be pressed into ingot and carry out sintering;
(5) hot extrusion molding
By spindle heating extrusion molding.
(6) forming materials processing
The wire rod of extruding or Strip are passed through to drawing or be rolled into the finished product.
Further arranging is that in described step (1), smelting temperature is at 1100-1300 ℃, and atomization temperature is at 1000-1200 ℃, and atomized water is pressed in 20-60MPa; The content that increases the additive alloy of substrate performance is 0.01-1% scope with respect to silver-colored mass ratio; Increase substrate performance additive and be bismuth, copper, indium, rare earth element, magnesium, nickel and zinc etc. any or several arbitrarily, when containing multiple element, total content is no more than 1%.
Further arrange is in described step (2), to mix in powder: the silver powder of band enhancing substrate performance additive and the ratio of oxide compound are between 92:8 to 78:28; Additive powder ratio accounts for gross weight than being 0.01-6%; Silver powder granularity is-200 orders, and oxide compound degree is < 15 μ m, and additive Powder Particle Size is < 30 μ m; Blending processes of powders is the blending processes of powders arbitrarily such as the mixed powder of dry-type mechanical, wet type powder mixing machine, the mixed powder of ball milling, the mixed powder of high-energy ball milling.
The pressure that further setting is isostatic cool pressing in described step (3) is at 100MPa-250Mpa.
Further arranging is described step (4) sintering, and wherein sintering temperature is 750 ℃-920 ℃, and the time is 2h-5h, under condition of nitrogen gas or under vacuum condition or under argon gas condition.
Further setting is that the Heating temperature of described step (5) is 700 ℃-900 ℃, and extrusion speed, at 1-15mm/s, is wire rod or band or sheet material after extrusion molding.
Another object of the present invention provides a kind of silver oxide contact material with strengthening substrate performance additive, its technical scheme is to comprise following component: oxidate powder, strengthen substrate performance additive, the second additive powder, surplus is silver, the second additive can be Tungsten oxide 99.999, oxide compound molybdenum, rare earth oxide, Indium sesquioxide, nickel oxide, tellurium oxide, cupric oxide, bismuth oxide, strengthen substrate performance additive and be bismuth, copper, indium, rare earth element, magnesium, nickel and zinc etc. any or several arbitrarily.
The feature of maximum of the present invention is the silver powder adopting with strengthening the additive of substrate performance, thereby solved silver matrix in conventional silver oxide material, is fine silver matrix, and its anti-current impact, arc erosion, resistance fusion welding can be all poor; Improve wetting situation between silver and oxide compound simultaneously, oxide material is enclosed in all the time with in the silver matrix of strengthening the property, reduced the gathering of oxide compound, floating trend, further improved the anti-electric-arc ablation ability of contact material; Simultaneously, owing to increasing additive alloy overall control lower of substrate performance, substantially can not reduce the conductivity of silver matrix, even can further improve its conductivity, so this material contact performance also can guarantee.Silver powder water atomization technology of preparing, contact material with strengthening the additive of substrate performance that the present invention adopts mix powder technology of preparing, and all technique is very simple, is applicable to industrialized mass.
Below in conjunction with specification drawings and specific embodiments, the present invention is described further.
Accompanying drawing explanation
Fig. 1 process flow sheet of the present invention.
Embodiment
Below by embodiment, the present invention is specifically described; only be used to further illustrate the present invention; can not be interpreted as limiting the scope of the present invention, the technician in this field can make some nonessential improvement and adjustment to the present invention according to the content of foregoing invention.
embodiment 1
With AgLa-SnO 210 materials are prepared as example
1,19.98kg Ag ingot, 0.02kgMg melting under 1300 ℃ of conditions, then at 1250 ℃ of Water Under powder by atomizations, water atomization pressure is 38MPa, last powder is crossed 200 mesh sieves, thereby obtains AgLa alloy powder;
2, the SnO of the AgLa powder of 9kg and the 3 μ m of 1kg 2powder machinery is dry mixed powder and prepares AgLa-SnO 210 powder;
3, AgLa-SnO 210 powder ingot processed under 180MPa pressure on cold isostatic press, spindle diameter 85mm.
4, AgLa-SnO 210 spindles are sintering 4h under vacuum condition, 850 ℃ of sintering temperatures.
5, AgLa-SnO 210 spindles push under 800 ℃ of conditions, and extruding specification is Φ 6.
6, AgLa-SnO 210 wire rods are through cold drawing machine, and cold drawing is to the diameter dimension needing.
AgLa-SnO prepared by this example 210 physicalies are as follows: density 10.1g/cm 3, resistivity 2.2 μ Ω .cm, hardness (HV0.3) 91(half-hard state), tensile strength 331MPa.
embodiment 2
With AgMgNi-SnO 2in 2o 312 materials are prepared as example
1, the Ag ingot of 19.98kg is, the Ni sheet of 0.01kg, the melting under 1200 ℃ of conditions of 0.01kgMg ingot, and then at 1150 Water Under powder by atomizations, water atomization pressure is 42MPa, and last powder is crossed 200 mesh sieves, thereby obtains AgMgNi alloy powder;
2, the SnO of the AgMgNi powder of 8.8kg and the 4 μ m of 1.0kg 2the In of the 5 μ m of powder, 0.2kg 2o 3powder machinery is dry mixed powder and prepares AgMgNi-SnO 2in 2o 312 powder;
3, AgMgNi-SnO 2in 2o 312 powder ingot processed under 220MPa pressure on cold isostatic press, spindle diameter 86mm.
4, AgMgNi-SnO 2in 2o 312 spindles are sintering 4h under vacuum, 860 ℃ of sintering temperatures.
5, AgMgNi-SnO 2in 2o 312 spindles push under 820 ℃ of conditions, and extruding specification is Φ 6.
6, AgMgNi-SnO 2in 2o 312 wire rods are through cold drawing machine, and cold drawing is to the diameter dimension needing.
AgMgNi-SnO prepared by this example 2in 2o 312 material contact physicalies are as follows: density 9.91g/cm 3, resistivity 2.38 μ Ω .cm, hardness (HV0.3) 102, tensile strength 354MPa.
embodiment 3
With AgCuNi-ZnO10 material, be prepared as example
1, the Ag ingot of 19.98kg is, the Cu of 0.01kg is excellent, the Ni sheet of 0.01kg, melting under 1300 ℃ of conditions, and then at 1250 ℃ of Water Under powder by atomizations, water atomization pressure is 60MPa, last powder is crossed 200 mesh sieves, thereby obtains AgCuNi alloy powder;
2, the ZnO powder machinery of the 7 μ m of the AgCuNi powder of 9kg and 1kg is dry mixed powder and prepares AgCuNi-ZnO10 powder;
3, AgCuNi-ZnO10 powder ingot processed under 180MPa pressure on cold isostatic press, spindle diameter 83mm.
4, AgCuNi-ZnO10 spindle sintering 4h under vacuum condition, 800 ℃ of sintering temperatures.
5, AgCuNi-ZnO10 spindle pushes under 780 ℃ of conditions, and extruding specification is 40X4.
6, the specification that AgCuNi-ZnO10 band extremely needs through cold-rolling mill rolling, punching.
AgCuNi-ZnO10 sheet point physicals prepared by this example is as follows: density 9.68g/cm 3, resistivity 2.29 μ Ω .cm, hardness (HV0.3) 87.

Claims (7)

1. one kind with the silver oxide contact material preparation method who strengthens substrate performance additive, it is characterized in that: raw material is oxidate powder, strengthen substrate performance additive, the second additive powder, surplus is silver, the second additive can be any or any several combination in Tungsten oxide 99.999, oxide compound molybdenum, rare earth oxide, Indium sesquioxide, nickel oxide, tellurium oxide, cupric oxide, bismuth oxide, strengthen substrate performance additive and be in bismuth, copper, indium, rare earth element, magnesium and zinc any or several arbitrarily, it is characterized in that making step is as follows successively:
(1) water atomization pulverization
By silver and the melting of enhancing substrate performance additive alloy process, water atomization, be prepared into the silver powder that increases substrate performance
(2) mixed powder
Silver powder and oxidate powder, the second additive powder with strengthening substrate performance additive are prepared into powder mix by blending processes of powders
(3) isostatic cool pressing
The powder mix of preparation is carried out to isostatic cool pressing, be pressed into ingot;
(4) sintering
To be pressed into ingot and carry out sintering;
(5) hot extrusion molding
By spindle heating extrusion molding;
?(6) forming materials processing
The wire rod of extruding or Strip are passed through to drawing or be rolled into the finished product.
2. a kind of silver-colored nickel contact material preparation method with strengthening substrate performance additive according to claim 1, is characterized in that: in described step (1), smelting temperature is at 1100-1300 ℃, and atomization temperature is at 1000-1200 ℃, and atomized water is pressed in 20-60MPa; The content that increases the additive alloy of substrate performance is 0.01-1% scope with respect to silver-colored mass ratio; Increase substrate performance additive and be bismuth, copper, indium, rare earth element, magnesium, nickel and zinc etc. any or several arbitrarily, when containing multiple element, total content is no more than 1%.
3. a kind of silver oxide contact material preparation method with strengthening substrate performance additive according to claim 1, is characterized in that: in described step (2), mix in powder: the silver powder of band enhancing substrate performance additive and the ratio of oxide compound are between 92:8 to 78:28; Additive powder ratio accounts for gross weight than being 0.01-6%; Silver powder granularity is-200 orders, and oxide compound degree is < 15 μ m, and additive Powder Particle Size is < 30 μ m; Blending processes of powders is the blending processes of powders arbitrarily such as the mixed powder of dry-type mechanical, wet type powder mixing machine, the mixed powder of ball milling, the mixed powder of high-energy ball milling.
4. a kind of silver oxide contact material preparation method with strengthening substrate performance additive according to claim 1, is characterized in that: in described step (3), the pressure of isostatic cool pressing is at 100MPa-250Mpa.
5. a kind of silver oxide contact material preparation method with strengthening substrate performance additive according to claim 1, it is characterized in that: described step (4) sintering, wherein sintering temperature is 750 ℃-920 ℃, time is 2h-5h, under condition of nitrogen gas or under vacuum condition or under argon gas condition.
6. a kind of silver oxide contact material preparation method with strengthening substrate performance additive according to claim 1, it is characterized in that: the Heating temperature of described step (5) is 700 ℃-900 ℃, extrusion speed, at 1-15mm/s, is wire rod or band or sheet material after extrusion molding.
7. the band that prepared by a preparation method as claimed in claim 1 strengthens the silver oxide contact material of substrate performance additive, it is characterized in that comprising following component: oxidate powder, strengthen substrate performance additive, the second additive powder, surplus is silver, the second additive can be Tungsten oxide 99.999, oxide compound molybdenum, rare earth oxide, Indium sesquioxide, nickel oxide, tellurium oxide, cupric oxide, bismuth oxide etc. any or several arbitrarily, strengthening substrate performance additive is bismuth, copper, indium, rare earth element, magnesium, nickel and zinc etc. any or several arbitrarily, the silver powder of band enhancing substrate performance additive and the mass ratio of oxide compound are between 92:8 to 78:28, the second additive powder ratio accounts for gross weight than being 0.01-6%, strengthen the 0.01-1% that substrate performance additive accounts for total content.
CN201310700969.5A 2013-12-18 2013-12-18 A kind of silver oxide contact material and preparation method and products thereof with strengthening substrate performance additive Active CN103695682B (en)

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PCT/CN2014/072141 WO2015089940A1 (en) 2013-12-18 2014-02-17 Sliver oxide contact material with matrix performance-enhancing additive as well as preparation method and product thereof

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WO2017008719A1 (en) * 2015-07-13 2017-01-19 严利容 Ag-cuo low-voltage contact material and method for fabrication thereof
CN108015276A (en) * 2017-11-29 2018-05-11 温州宏丰电工合金股份有限公司 One kind enhancing phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof
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CN105374598A (en) * 2015-11-05 2016-03-02 福达合金材料股份有限公司 Manufacturing method for coarse oxide particle silver-based electric contact materials
CN108015276A (en) * 2017-11-29 2018-05-11 温州宏丰电工合金股份有限公司 One kind enhancing phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof
CN108015276B (en) * 2017-11-29 2019-08-23 温州宏丰电工合金股份有限公司 A kind of reinforced phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof
JP2019183268A (en) * 2018-04-11 2019-10-24 Ｄｏｗａエレクトロニクス株式会社 Silver powder and manufacturing method therefor
JP7272834B2 (en) 2018-04-11 2023-05-12 Ｄｏｗａエレクトロニクス株式会社 Silver powder and its manufacturing method
CN112475295A (en) * 2020-09-30 2021-03-12 福达合金材料股份有限公司 Silver iron oxide electric contact material with oxide particles dispersed and distributed and preparation method thereof
CN115896530A (en) * 2022-12-23 2023-04-04 贵研中希（上海）新材料科技有限公司 High-performance AgCuNi composite material and preparation method thereof

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