CN102350502B - Preparation method of silver-stannic oxide by using physical metallurgical coating method - Google Patents

Preparation method of silver-stannic oxide by using physical metallurgical coating method Download PDF

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CN102350502B
CN102350502B CN 201110331046 CN201110331046A CN102350502B CN 102350502 B CN102350502 B CN 102350502B CN 201110331046 CN201110331046 CN 201110331046 CN 201110331046 A CN201110331046 A CN 201110331046A CN 102350502 B CN102350502 B CN 102350502B
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powder
silver
stannic oxide
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sintering
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CN102350502A (en
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刘立强
颜小芳
翁桅
林万焕
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Zhejiang Fuda Alloy Materials Technology Co Ltd
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Abstract

The invention discloses a preparation method of silver-stannic oxide by using a physical metallurgical coating method. According to the preparation method, silver powder, stannic oxide powder and additive alloy powder are as raw materials. The preparation method comprises the following steps: preparing additive-coated stannic oxide powder through powder mixing, calcining and oxidizing processes; mixing the additive-coated stannic oxide powder with the silver powder to prepare silver-stannic oxide powder; and compressing, calcining, extruding, and drawing or rolling to finally obtain a contact material finished product. The silver-stannic oxide has the characteristics of uniform additive distribution, uniform and stable stannic oxide particles, uniform and stable electric performance of contact material, excellent processing performance and the like. The preparation method is simple and suitable for batch production, and the prepared silver-stannic oxide product can be widely used in relays, contactors and breakers.

Description

The preparation method of silver-stannic oxide by using physical metallurgical coating method
Technical field
The present invention relates to a kind of preparation method of contact material, especially a kind of preparation method of siller tin oxide slider material.
Background technology
AgSnO 2Slider material has more and more replaced the AgCdO contact application in electrical equipment, and has tentatively finished AgSnO at west european developed country owing to its good resistance fusion welding energy and high electric life performance and environmental-protecting performance 2Replace AgCdO work.Domestic and international AgSnO 2The contact main production is divided into three kinds of techniques: powder mixing method, internal oxidation, chemical method.Wherein powder mixing method is Ag powder, SnO 2And additive powder powder fully mixes, and then material extruding, mold pressing are prepared into AgSnO 2Slider material; Internal oxidation is by being divided into preoxidation and internal oxidation, and wherein preoxidation mainly refers to prepare the AgSn alloy powder, then is prepared into AgSnO by the powder oxidation 2Material is prepared into highdensity AgSnO by extruding or press moulding mode at last 2Slider material, this method, for example Chinese disclosure of the invention number is the preparation method of a kind of silver tin oxide material of CN1425790A, internal oxidation refers to that AgSn is prepared into alloy wire or sheet material, then is prepared into AgSnO by internal oxidation process 2Slider material; Chemical method mainly refers to prepare AgSnO by hydrometallurgical processes 2Slider material, the most representative is exactly that liquor argenti nitratis ophthalmicus adds the tin oxide powder, and then reduction silver realizes that chemistry coats AgSnO in the solution 2Contact method, the method are called again Chemical coating method.
Because AgSnO 2Contact resistance own is higher, and behind the arcing, SnO 2Easily be gathered in working face, so the AgSnO2 material all passes through the additive method basically, increase the wetting of SnO2 and Ag, thus SnO after reducing about electric arc 2Clustering phenomena reduces the contact resistance between the course of work contact, further reduces the splash phenomenon of Ag behind the large arcing, thereby improves the electric life of contact.So AgSnO 2All researchs of electric contact material are all around changing SnO by additive 2And the wetting problem between the Ag uses maximum additives to be Bi in domestic and foreign literature and the patent 2O 3, CuO, In 2O 3, these additives all can increase SnO 2Wetting performance between particle and the Ag matrix.Conventional powder mixing method additive adding method is powder mixing machine, and the method is difficult to realize the additive full and uniform dispersion, thereby can not guarantees each SnO 2There is additive between particle and the Ag matrix.The alloy powder pre-oxidation process has fully solved SnO 2The uniform and stable problem of additive between particle and the Ag matrix, but AgSn alloy powder preoxidation process is easy to occur SnO 2The problem of assembling, thus cause the powder uniformity to have very large fluctuation, cause the electrical property fluctuation larger; Chemical coating method can solve the problem of additive dispersiveness equally, but there is environmental issue in chemical powdering technique, does not also recommend to carry out industrial mass and carries out.There is the poor problem of analysing of material internal oxide equally in the material internal oxidation process, causes the fluctuation of material electrical property larger.
Along with AgSnO 2Slider material increases at the consumption of low-voltage electrical apparatus, more need to seek a kind of processing characteristics better, the distribute production technology of the more stable siller tin oxide slider material of even dispersion more, electrical property of additive.
Summary of the invention
The problem to be solved in the present invention is to improve the shortcomings such as the disperse of additive skewness, the electrical property of siller tin oxide slider material production technology in the background technology be unstable.
For achieving the above object, the invention provides a kind of preparation method of Physical Metallurgy coated with silver tin oxide slider material, raw material is SnO 2, additive, surplus is Ag, wherein additive be among Bi, Cu, In and the Zn any or several arbitrarily, it is characterized in that making step is as follows successively:
(1) powder mixing machine
With SnO 2Powder, the mixing of additive powder mechanical uniform also form the first mixture;
(2) powder sintering
With the first mixture sintering under non-oxidizing atmosphere;
(3) powder oxidation
The first mixture that sintering is finished carries out oxidation under aerobic environment;
(4) powder is broken
The first mixture that oxidation is finished carries out fragmentation;
(5) powder mixing machine
The first mixture powder after Ag powder, the fragmentation is carried out powder mixing machine and forms the second mixture;
(6) isostatic cool pressing
The second mixture is carried out isostatic cool pressing, be pressed into ingot;
(7) sintering
The second mixture that is pressed into ingot is carried out sintering;
(8) hot extrusion molding
With spindle heating and extrusion molding.
SnO in the described step (2) 2The powder particle mean size is at 1 μ m-5 μ m, and described additive powder mean particle sizes is at 1 μ m-25 μ m.
Sintering temperature in the described step (2) is 300 ℃-850 ℃, and sintering time is 1h-4h, and non-oxidizing atmosphere is vacuum environment or hydrogen or nitrogen environment or ar gas environment.
Described step (3) aerobic environment is air ambient or pure oxygen environment, oxidization time 0.5 h-4h, and oxidizing temperature is at 300 ℃-750 ℃, and pressure is 0.1 Mpa-0.9Mpa.
Particle mean size in the described step (4) after the first mixture fragmentation≤10 μ m.
Ag powder particle mean size is at≤15 μ m described in the described step (5).
The pressure of isostatic cool pressing is at 60MPa-250Mpa in the described step (6),
Described step (7) sintering, wherein sintering temperature is 750 ℃-920 ℃, the time is 2h-5h, under the air conditions or under the vacuum condition.
The heating-up temperature of described step (8) is 750 ℃-900 ℃, and extrusion speed is wire rod or band or sheet material after the extrusion modling at 1mm/s-15mm/s.
Wherein the main component of additive alloy powder can for: Bi, BiCu, In, BiIn, ZnCu, ZnBi etc. any or appoint several, the common feature of this type of alloy be fusing point below 800 ℃, purpose is can not allow SnO in additive alloy melting temperature 2The particle sintering strength is larger, to the broken adverse influence that produces of follow-up powder.
The present invention is SnO at first 2Powder fully mixes with the additive alloy powder, then carries out sintering more than the fusing point of alloy powder, makes alloy form liquid state, fully is wrapped in SnO 2Around the particle, then to being wrapped in SnO 2Circumgranular alloy carries out oxidation, makes it to change into alloyed oxide, finishes SnO 2The Physical Metallurgy of particle coats process, subsequently to SnO 2Powder carries out fragmentation, and all are oxide ceramics mutually owing to powder inside, so in Physical Metallurgy coating process, SnO 2Particle can not produce serious adhesion clustering phenomena, and is follow-up by the i.e. SnO of simple Mechanical Crushing 2Particle reverts to the primary granule size again.The AgSnO of the present invention's preparation 2The slider material even tissue is stable, and homogeneous chemical composition is stable, and can guarantee every SnO 2Surface parcel one deck additive alloy oxidation layer has solved traditional powder mixing machine and can't reach the additive decentralization, has fully guaranteed stability and the uniformity of material electrical property, and because SnO 2Uniform particles is stable, thus the AgSnO of preparation 2Materials processing is functional.This method combines the kinds of processes such as powder mixing machine, Physical Metallurgy coating, powder oxidation, and whole preparation process produces without waste gas, waste liquid, and working (machining) efficiency also can satisfy industrialized mass.
The present invention has overcome all drawbacks that existing technique exists, and combine that the mixed powder of powder, chemistry coat, the advantage of powder oxidation three class techniques, proposed that a kind of density of material is high, homogeneous chemical composition stable, metallographic structure evenly, the center is without the preparation method of poor Sn layer, processing characteristics is good, oxidation rate is fast tin-oxygen-silver electric contact material.
Description of drawings
Fig. 1 process chart of the present invention.
The specific embodiment
Embodiment 1
With AgSnO 2Bi 2O 3(10) material is prepared as example
1, SnO 2Powder 1.7kg, Bi powder 0.269kg put into three-dimensional mixed powder machine and mix powder and form the first mixture; SnO wherein 2The powder particle mean size is at 5 μ m, and the Bi average particle size is at 10 μ m.Mixed powder time 1h;
2, SnO 2The first mixture that+Bi powder forms carries out sintering under the hydrogen condition, 300 ℃ of temperature, and the time is 1h; Generate the SnO that Bi coats 2The SnO of particle 2The Bi material;
3, SnO 2The Bi material carries out oxidation under air conditions, 500 ℃ of oxidizing temperatures, and the time is 1h; Generate Bi 2O 3Coat SnO 2The SnO of particle 2Bi 2O 3Material;
4, with SnO 2Bi 2O 3Powder is placed on and carries out ball mill crushing in the ball mill, the particle mean size 10 μ m of particle behind the ball mill crushing;
5, Ag powder and the SnO of 18kg 2Bi 2O 3Powder mixes powder and forms the second mixture AgSnO in the mixed powder machine of three-dimensional 2Bi 2O 3(10) powder, wherein the particle mean size of Ag powder is 15 μ m;
6, AgSnO 2Bi 2O 3(10) powder is at the first-class static pressure of 300MPa isostatic pressing machine, and hydrostatic pressure is 250MPa, and the spindle diameter is between 85-88mm;
7, AgSnO 2Bi 2O 3(10) spindle at air conditions at sintering, 920 ℃ of sintering temperatures, the time is 5h;
8, AgSnO 2Bi 2O 3(10) spindle pushes under the 15mm/s condition at 800 ℃, extrusion speed, and the extruding specification is the sheet material in 40mmX5mm cross section.
The AgSnO of this example preparation 2Bi 2O 3(10) the strip-form contacts physical property is as follows: density 10.03 g/cm 3, resistivity 2.21 μ Ω .cm, hardness (HV0.3) 75(annealed state).
The AgSnO of this example preparation 2Bi 2O 3(10) the strip-form contacts physical property is as follows: density 10.03 g/cm 3, resistivity 2.21 μ Ω .cm, hardness (HV0.3) 75(annealed state).
Embodiment 2
With AgSnO 2In 2O 3Bi 2O 3(12) material is prepared as example.
1, SnO 2Powder 2.00kg, In powder 0.166kg, Bi powder 0.180kg put into three-dimensional mixed powder machine and mix powder and form the first mixture; SnO wherein 2The powder particle mean size is at 1 μ m, and the In Powder Particle Size is at 5 μ m, and the Bi average particle size is at 10 μ m.Mixed powder time 4h;
2, SnO 2+ Bi+In powder carries out sintering under the hydrogen condition, 400 ℃ of temperature, and the time is 2h, generates the SnO that Bi, In coat 2The SnO of particle 2The BiIn material;
3, SnO 2The BiIn material carries out oxidation under air conditions, 500 ℃ of oxidizing temperatures, and the time is 2h; Generate Bi 2O 3In 2O 3Coat SnO 2The SnO of particle 2Bi 2O 3In 2O 3Material;
4, SnO 2Bi 2O 3In 2O 3Material carries out ball mill crushing in ball mill, particle mean size 8 μ m
5, Ag powder and the SnO of 17.6kg 2In 2O 3Bi 2O 3Powder mixes powder and forms the second mixture AgSnO in the mixed powder machine of three-dimensional 2In 2O 3Bi 2O 3(12) powder, wherein the particle mean size of Ag powder is 10 μ m;
6, AgSnO 2In 2O 3Bi 2O 3(12) powder is at the first-class static pressure of 300MPa isostatic pressing machine, and hydrostatic pressure is 250MPa, and the spindle diameter is between 85-88mm;
7, AgSnO 2Spindle at air conditions at sintering, 880 ℃ of sintering temperatures, the time is 3h;
8, AgSnO 2In 2O 3Bi 2O 3(12) spindle pushes under the 5mm/s condition at 850 ℃, extrusion speed, and the extruding specification is the silk thread material of Φ 6mm.
The AgSnO of this example preparation 2In 2O 3Bi 2O 3(12) silk material contact physical property is as follows: density 9.91g/cm 3, resistivity 2.30 μ Ω .cm, hardness (HV0.3) 80(annealed state), tensile strength 307MPa.
Embodiment 3
With AgSnO 2Bi 2O 3CuO (14) material is prepared as example.
1, SnO 2Powder 2.00kg, BiCu alloyed powder (wherein Cu accounts for percentage by weight 2.3) 0.36kg put into three-dimensional mixed powder machine and mix powder and form the first mixture; SnO wherein 2The powder particle mean size is at 1 μ m, and BiCu powder particle mean size is at 10 μ m.Mixed powder time 4h;
2, SnO 2+ BiCu powder carries out sintering under the hydrogen condition, 800 ℃ of temperature, and the time is 2h, generates the SnO that Bi, Cu coat 2The SnO of particle 2The BiCu material;
3, SnO 2The BiCu material carries out oxidation under air conditions, 500 ℃ of oxidizing temperatures, and the time is 2h; Generate Bi 2O 3+CuO coats SnO 2The SnO of particle 2Bi 2O 3The CuO material;
4, SnO 2Bi 2O 3The CuO material carries out ball mill crushing in ball mill, particle mean size 8 μ m
5, Ag powder and the SnO of 17.6kg 2Bi 2O 3The CuO powder mixes powder and forms the second mixture AgSnO in the mixed powder machine of three-dimensional 2Bi 2O 3CuO (14) powder, wherein the particle mean size of Ag powder is 10 μ m;
6, AgSnO 2Bi 2O 3CuO (14) powder is at the first-class static pressure of 300MPa isostatic pressing machine, and hydrostatic pressure is 250MPa, and the spindle diameter is between 85-88mm;
7, AgSnO 2Bi 2O 3CuO (14) spindle at air conditions at sintering, 880 ℃ of sintering temperatures, the time is 3h;
8, AgSnO 2Bi 2O 3CuO (14) spindle pushes under the 3mm/s condition at 880 ℃, extrusion speed, and the extruding specification is the silk thread material of Φ 6mm.
The AgSnO of this example preparation 2Bi 2O 3CuO (14) contact silk material physical property is as follows: density 9.81g/cm 3, resistivity 2.41 μ Ω .cm, hardness (HV0.3) 84(annealed state), even tiny, the tensile strength 310MPa(annealed state of oxide particle), percentage elongation 19%(annealed state).
The technique of the relative prior art of technique of the present invention has advantage, and the comparison is as follows shows:
Figure 2011103310468100002DEST_PATH_IMAGE001
The invention is not restricted to above embodiment.

Claims (9)

1. the preparation method of a silver-stannic oxide by using physical metallurgical coating method, raw material is SnO 2, additive, surplus is Ag, wherein additive be among Bi, Cu, In and the Zn any or several arbitrarily, it is characterized in that making step is as follows successively:
(1) powder mixing machine
With SnO 2Powder, the mixing of additive powder mechanical uniform also form the first mixture;
(2) powder sintering
With the first mixture sintering under non-oxidizing atmosphere;
(3) powder oxidation
The first mixture that sintering is finished carries out oxidation under aerobic environment;
(4) powder is broken
The first mixture that oxidation is finished carries out fragmentation;
(5) powder mixing machine
The first mixture powder after Ag powder, the fragmentation is carried out powder mixing machine and forms the second mixture;
(6) isostatic cool pressing
The second mixture is carried out isostatic cool pressing, be pressed into ingot;
(7) sintering
The second mixture that is pressed into ingot is carried out sintering;
(8) hot extrusion molding
With spindle heating and extrusion molding.
2. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1 is characterized in that: the SnO in the described step (1) 2The powder particle mean size is at 1 μ m-5 μ m, and described additive powder mean particle sizes is at 1 μ m-25 μ m.
3. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1, it is characterized in that: the sintering temperature in the described step (2) is 300 ℃-850 ℃, sintering time is 1h-4h, and non-oxidizing atmosphere is vacuum environment or hydrogen or nitrogen environment or ar gas environment.
4. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1, it is characterized in that: described step (3) aerobic environment is air ambient or pure oxygen environment, oxidization time 0.5h-4h, oxidizing temperature is at 300 ℃-750 ℃, and pressure is 0.1 Mpa-0.9Mpa.
5. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1 is characterized in that: the particle mean size in the described step (4) after the first mixture fragmentation≤10 μ m.
6. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1, it is characterized in that: Ag powder particle mean size is at≤15 μ m described in the described step (5).
7. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1 is characterized in that: the pressure of isostatic cool pressing is at 60MPa-250Mpa in the described step (6).
8. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1 is characterized in that: described step (7) sintering, and wherein sintering temperature is 750 ℃-920 ℃, the time is 2h-5h, under the air conditions or under the vacuum condition.
9. the preparation method of a kind of silver-stannic oxide by using physical metallurgical coating method according to claim 1, it is characterized in that: the heating-up temperature of described step (8) is 750 ℃-900 ℃, extrusion speed is wire rod or band or sheet material after the extrusion modling at 1mm/s-15mm/s.
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CN103014395B (en) * 2012-12-09 2014-12-24 温州聚星电接触科技有限公司 Method for preparing efficient aerated mixed powder
CN103695682B (en) * 2013-12-18 2016-03-23 福达合金材料股份有限公司 A kind of silver oxide contact material and preparation method and products thereof with strengthening substrate performance additive
CN104269296B (en) * 2014-09-05 2017-01-25 重庆川仪自动化股份有限公司 Preparation method of silver tin oxide electric contact material
CN104493178B (en) * 2014-12-30 2016-09-14 桂林电器科学研究院有限公司 A kind of processing method of the silver zinc oxide electrical contact material containing additive
CN105880609B (en) * 2016-04-11 2018-06-26 哈尔滨建成集团有限公司 The moulding technique and molding die of a kind of engine jet pipe
CN106653410B (en) * 2016-10-14 2019-04-19 佛山市诺普材料科技有限公司 A kind of high-performance environment protection type siller tin oxide electric contact material and preparation method thereof
CN108330315B (en) * 2018-02-13 2019-12-06 浙江大学 Superplastic Ag/SnO2 alloy material and preparation method thereof

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CN101202169A (en) * 2007-10-23 2008-06-18 福达合金材料股份有限公司 Method of preparing novel silver tin oxide silk electrical contact material
CN101609755B (en) * 2009-07-08 2012-07-25 中南大学 Preparation method of silver-metallic oxide electrical contact material
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