CN101135011A - New method for preparing AgSnO2 electrical contact material - Google Patents
New method for preparing AgSnO2 electrical contact material Download PDFInfo
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- CN101135011A CN101135011A CNA2007100661409A CN200710066140A CN101135011A CN 101135011 A CN101135011 A CN 101135011A CN A2007100661409 A CNA2007100661409 A CN A2007100661409A CN 200710066140 A CN200710066140 A CN 200710066140A CN 101135011 A CN101135011 A CN 101135011A
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Abstract
The process of preparing electric contact AgSnO2 material includes the following technological steps: vacuum preparing intermediate AgY alloy and Sn material, preparing AgSnY alloy powder in chilled atomizing powder preparing equipment and in atmospheric state, inner oxidizing treatment to convert Sn and Y in the alloy into SnO2 and Y2O3 separately, modifying the inner oxidized powder, powder metallurgic steps to form cog, hot extruding to obtain semi-finished filament or sheet, hot working, and cold machining to obtain product. The present invention has the key technology of powder pre-oxidization and modification, and indirectly improved material machining performance.
Description
Technical field
The present invention relates to the manufacturing process of tin-oxygen-silver electric contact material, oxide treatment and powder is carried out the manufacturing process of modification Processing of Preparation tin-oxygen-silver electric contact material in particularly relating to.
Background technology
The quality and the manufacture craft of tin-oxygen-silver electric contact material performance are closely related, and manufacturing process difference, its contact material performance are also different.Its manufacturing process mainly contains four kinds of alloy inner oxidation method, powder metallurgic method, powdered alloy preoxidation and chemical coprecipitations.
The alloy inner oxidation method: the alloy inner oxidation method once was widely adopted in Japan, it is a kind of more sophisticated processing method, tiny, the anti-arc erosion performance of contact material densification, oxide particle that makes with this method is good, electric life is long, but material surface and internal structure are inhomogeneous, have poor zone of oxidation, the contact size is accurate inadequately.But this method is being produced AgSnO
2But run into the not saturating problem of oxidation when Sn content is higher than 6% during contact.Mainly be by adding In and adopting hyperbaric oxygen to solve at present.The primary condition of alloy inner oxidation is: under oxidation temperature, alloying element and oxygen should be able to be dissolved in the matrix metal, and the oxide compound of alloying element then should be insoluble; It is big that the solubleness of oxygen in matrix metal is wanted; Oxygen and matrix can not form stable oxide, should stablize with the oxide compound that alloying element forms; The velocity of diffusion of alloying element in matrix metal is lower than the velocity of diffusion of oxygen in matrix.
Powder metallurgic method: powder metallurgic method is adopted in West Europe more.Powder metallurgical technique is not subjected to the restriction of constituent element composition, and the material disperse of preparation is even, has avoided barren district, and weave construction is even, and technology is simple, but contact density is lower than the internal oxidation process, and hardness is lower, SnO
2Particle is thicker, and contact resistance is big, temperature rise, and anti-arc erosion is poor, and preparation time is long, and powder is easily contaminated, in addition, prepared Ag-SnO
2The plasticity and the ductility of material are very poor, are difficult for making the product that rivet or this class of sheet material need gross distortion.The technical process of powder metallurgic method comprises: with Ag and SnO
2Fines is thorough mixing in ball mill, and moulding then, presintering improve density, improves for making the goods final densities, and secondary processing is very important as multiple pressure, sintering and extruding etc.
The powdered alloy preoxidation: investigator's analysis and summary such as India Amitabh Vermac powdered alloy preoxidation (P/O) technology has been proposed after the relative merits of alloy inner oxidation technology and powder metallurgical technique.This technology can be regarded as the comprehensive of alloy inner oxidation technology and powder metallurgical technique, this technology utilization the advantage of rapid solidification, make the refinement of product grain, the microtexture of material segregation not occur, avoided the shortcoming of conventional alloy inner oxidation technology process, make the material internal even structure, can not produce barren district.People such as Amitabh Verma find, dispersed oxide with Sn and In in the contact material of this novel process preparation is distributed among the Ag, and oxidation particle all links to each other with rich Ag in each, has increased flowability, it is easier that electric current flows, thereby improved conductivity of electrolyte materials.Find the hardness of gained material, the height that density but is not so good as alloy inner oxidation technology process material simultaneously.
Chemical coprecipitation: its second-phase dispersion of contact material of chemical coprecipitation preparation is even, electrical property is good, but powder cost height, and owing to relate to the wet chemistry reaction process, the difficult control of the stability of each batch powder quality, so its popularization does not have other method so extensive.
Summary of the invention
The technology used in the present invention mainly is based on powdered alloy preoxidation development and comes.Its basic ideas are to prepare silver-colored tin alloy powder earlier, after the oxide treatment, powder is carried out modification handle in it is carried out, and make the silk material or the sheet material of desired size then with powder metallurgy technology and pressure processing technology.
Design of alloy: remove SnO
2Add Y outward,
2O
3As the oxide compound constituent element, Ag is an alloy substrate.Add Y
2O
3Can improve the ablative and wear resistance of its anti-electric-arc, improve its electric life.Three kinds of designed alloying constituents are: (1) SnO
2-6%, Y
2O
3-2%, Ag is a surplus; (2) SnO
2-7%, Y
2O
3-3%, Ag is a surplus; (3) SnO
2-8%, Y
2O
3-4%, Ag is a surplus.
Operational path: obtain AgSnY powdered alloy → interior oxide treatment with own air water chilling powder by atomization technology and equipment under preparation AgY master alloy+Sn raw material → atmospheric condition under the vacuum and make Sn and Y in the alloy be transformed into SnO
2And Y
2O
3→ internal oxide powder carries out modification processing → powder metallurgy operation (shaping+sintering → multiple pressure+resintering → CIP+ sintering) and makes shaping base → hot extrusion acquisition silk material or sheet material work in-process base → hot-work acquisition work in-process → cold working acquisition finished product.
Gordian technique of the present invention is powder pre-oxidation technology and modification treatment technology.When having avoided alloy inner oxidation, the former is difficult to an oxidation difficult problem completely during high tin content.The latter has improved the bonding state between Ag matrix and oxide compound constituent element, thereby has improved Drawing abillity indirectly.
The AgSnO of the present invention's preparation
2The tissue of contact material and performance can be found out SnO in the microstructure from its microstructure such as accompanying drawing 1
2And Y
2O
3With graininess exist, distribution disperse and evenly, do not have obvious segregation, grain spacing is smaller; There is cavity to a certain degree in the material.
And density of material is 9.96gcm
-3, a spot of cavity makes the density of sample a little less than theoretical density 10.08gcm in the material
-3Specific conductivity is 42Msm
-1, corresponding its resistivity is 3.38 μ Ω cm; Hardness is HV98.The anti-electric-arc ablation property is good, long service life.
The drawing explanation
Fig. 1 is an AgSnO2 contact material micro-organization chart.SnO in the microstructure
2And Y
2O
3With graininess exist, distribution disperse and evenly, do not have obvious segregation, grain spacing is smaller; There is cavity to a certain degree in the material.
Embodiment:
(1) AgY master alloy preparation: under the vacuum with the induction melting Ag (purity is more than 99.95%) of plumbago crucible elder generation, charge into inert atmosphere Ar after the degasification, add raw material Y (purity is more than 99.5%), the intensification refining is fully fused in the Ag molten metal Rare Earth Y, after leaving standstill 5 minutes, be poured in the graphite casting die, fully vacuum is destroyed in the cooling back, takes out AgY master alloy ingot casting.(2) chilling atomizing preparation AgSnY powdered alloy: first induction melting AgY master alloy under the atmospheric condition, suitably reduce temperature, adding Sn raw material (purity〉99.95%), the intensification refining also makes its abundant alloying, be incubated that (the alloy liquid temp is controlled at 1000-1180 ℃) at the uniform velocity pours into hot funnel (ideal temperature is 1050-1100 ℃) after 3-8 minute, (atomizing medium is pure N to the alloy liquid by funnel through inert atmosphere
2, atomizing pressure is 0.6-1.2MPa) impact and crushing effect, water is as heat-eliminating medium, and the alloying pellet after the atomizing is cooled off fast.Cooled powdered alloy is crossed 100 mesh standard sieves (size＜150 μ m), and-100 purpose powdered alloys are stand-by, and meal (+100 order) then can melt down powder process again.(3) AgSnY powdered alloy preoxidation: earlier AgSnY alloy powder sample presentation is carried out thermogravimetric analysis, measure the interior oxidizing temperature scope (620-750 ℃) of alloy.Selecting proper interior oxidizing temperature is 650-720 ℃, heaps thickness according to powdered alloy and work out interior oxidization time (being approximately 8hours/cm) and mode (can carry out) under atmospheric condition.(4) the oxide powder modification is handled: interior oxide powder is moistening with pure water, add a small amount of rare HNO
3Remove foreign matter, with the rare AgNO for preparing in advance
3Solution (AgNO
3Amount is the 2-12wt% of the powdered alloy amount of required modification) progressively add, fully stir with glass stick and make it become uniform suspension.Add dilute ammonia solution (NH by amount
4OH, industrial concentration), and fully stir, when treating that whole solution is rendered as white colloidal mixture, add a small amount of hydration hydrazine reductant, stir fast, make the simple substance silver that restores be deposited in the surface (can judge whether that silver covers powder surface) of powder with the particulate matter of superfine size according to the color of powder before and after the reaction.Composite powder appearance after the modification is Ag, and inside is SnO
2, Y
2O
3With the mixture of Ag, thereby improved the distribution of oxide particle.(5) shaping and sintering process: when powdered mixture was shaped, compacting pressure should not be too big, gets final product about 180-200MPa, and soaking time is slightly long, is 4-6min.During sintering, for avoiding be shaped base cracking and nonaffine deformation, heat-up rate is unsuitable too fast, preferably heats up holding time long (1h) stage by stage first: room temperature-300 ℃ intensification 1h, insulation 1.5h; 300-600 ℃ of intensification 1h fills inert atmosphere and reduces vacuum tightness to reduce volatilization, insulation 1.5h; 600-900 ℃ of intensification 1h, insulation 2-6h; Be cooled to below 100 ℃ and can come out of the stove with stove.Better, the dwell time is 2-4min to pressure between 250-300MPa when pressing again.Room temperature during resintering-600 ℃ intensification 1h fills inert atmosphere and reduces vacuum tightness to reduce volatilization, insulation 1.5h; 600-900 ℃ of intensification 1h, insulation 2-6h; Be cooled to below 100 ℃ and can come out of the stove with stove.CIP (isostatic cool pressing system), compacting pressure is 300-350MPa, dwell time 5-12min, CIP technology can improve the density and the homogeneity thereof of shaping blank, with resintering technology it is carried out sintering subsequently.(6) shaping base hot extrusion: under the air atmosphere, more than the 640-800 ℃ of insulation 4h, moderate speed under the 180-250MPa, large extrusion ratio (〉 100: 1) it is squeezed into band or silk material.Hot extrusion can improve density, improves tissue, can improve its processing characteristics simultaneously.(7) complete processing: extrusion billet can carry out the hot-work (AgSnO of large deformation
2The hot workability of contact material is good), stay less deflection and carry out cold working (preferably making the passage amount of finish) less than 5%, increase scrap rate in order to avoid ftracture.Here it is AgSnO
2The whole detailed process rules of contact material preparation.
Embodiment 1 SnO
2-6%, Y
2O
3-2%, Ag is a surplus, and concrete steps are described in detail as in the embodiment.
Embodiment 2 SnO
2-7%, Y
2O
3-3%, Ag is a surplus, and concrete steps are described in detail as in the embodiment.
Embodiment 3 SnO
2-8%, Y
2O
3-4%, Ag is a surplus, and concrete steps are described in detail as in the embodiment.
Claims (4)
1. AgSnO
2The contact material novel preparation method is characterized in that comprising following steps:
(1) preparation AgY master alloy under the vacuum;
(2) chilling atomizing preparation AgSnY powdered alloy;
(3) interior oxide treatment makes Sn and Y in the alloy be transformed into SnO
2And Y
2O
3
(4) internally oxide powder carries out the modification processing;
(5) the powder metallurgy operation makes the shaping base;
(6) hot extrusion obtains silk material or sheet material work in-process base;
(7) hot-work obtains work in-process;
(8) cold working obtains finished product.
2. according to the described AgSnO of claim
2The contact material novel preparation method is characterized in that the temperature of the interior oxide treatment of described step (3) is 650～750 ℃.
3. according to the described AgSnO of claim
2The contact material novel preparation method is characterized in that the internal oxide powder of described step (4) carries out the modification processing and is: interior oxide powder is moistening with pure water, add the rare AgNO for preparing in advance
3Solution fully stirs, and adds dilute ammonia solution (NH by amount
4OH), and fully stir, treat to present in the solution a large amount of white colloidal thing amounts, after the agent of adding hydrazine hydrate reduction, stir fast, make the simple substance silver that restores be deposited in the surface (can judge whether that silver covers powder surface) of powder according to the color of powder before and after the reaction.
4. according to the described AgSnO of claim
2The contact material novel preparation method is characterized in that described step (5) powder metallurgy operation is: shaping+sintering → multiple pressure+resintering → CIP+ sintering.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268583A (en) * | 2011-08-09 | 2011-12-07 | 福达合金材料股份有限公司 | Method for preparing silver tin oxide electrical contact material |
| CN103194658A (en) * | 2013-04-09 | 2013-07-10 | 温州宏丰电工合金股份有限公司 | Preparation method of superfine SnO2 particle-reinforced electric contact material |
| CN104148661A (en) * | 2014-09-03 | 2014-11-19 | 湖北鄂信钻石科技股份有限公司 | Method for preparing aluminum oxide dispersion pre-alloyed powder |
| CN104313364A (en) * | 2014-10-10 | 2015-01-28 | 福达合金材料股份有限公司 | Process for preparing fine oxide particle reinforced silver-based electric contact material by oxidization-reduction method |
| CN104498763A (en) * | 2014-12-30 | 2015-04-08 | 桂林电器科学研究院有限公司 | Method for processing silver tin oxide-oxide electrical contact material |
| CN104532049A (en) * | 2014-11-25 | 2015-04-22 | 宁波科扬贵金属合金科技有限公司 | Silver tin oxide (AgSnO2) contact material making method |
| CN105215351A (en) * | 2015-10-09 | 2016-01-06 | 中国船舶重工集团公司第七一二研究所 | A kind of silver-colored coated fin oxide condutire powder and preparation method thereof |
| CN105788891A (en) * | 2016-04-29 | 2016-07-20 | 河南省豫星华晶微钻有限公司 | High-wearing-resistance high-heat-conductivity electrical contact based on 3D printing technology and preparation process thereof |
| CN110499435A (en) * | 2019-09-20 | 2019-11-26 | 昆明贵金属研究所 | A kind of silver-based electric contact material and preparation method thereof |
-
2007
- 2007-08-28 CN CNA2007100661409A patent/CN101135011A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268583B (en) * | 2011-08-09 | 2013-06-12 | 福达合金材料股份有限公司 | Method for preparing silver tin oxide electrical contact material |
| CN102268583A (en) * | 2011-08-09 | 2011-12-07 | 福达合金材料股份有限公司 | Method for preparing silver tin oxide electrical contact material |
| CN103194658B (en) * | 2013-04-09 | 2016-02-03 | 温州宏丰电工合金股份有限公司 | A kind of ultra-fine SnO 2the preparation method of the electric contact composite material of particle reinforce |
| CN103194658A (en) * | 2013-04-09 | 2013-07-10 | 温州宏丰电工合金股份有限公司 | Preparation method of superfine SnO2 particle-reinforced electric contact material |
| CN104148661A (en) * | 2014-09-03 | 2014-11-19 | 湖北鄂信钻石科技股份有限公司 | Method for preparing aluminum oxide dispersion pre-alloyed powder |
| CN104148661B (en) * | 2014-09-03 | 2016-01-06 | 湖北鄂信钻石科技股份有限公司 | A kind of preparation method of aluminum oxide dispersion prealloy powder |
| CN104313364A (en) * | 2014-10-10 | 2015-01-28 | 福达合金材料股份有限公司 | Process for preparing fine oxide particle reinforced silver-based electric contact material by oxidization-reduction method |
| CN104313364B (en) * | 2014-10-10 | 2016-05-25 | 福达合金材料股份有限公司 | A kind of oxidation-method of reducing is alternately prepared the technique of the particle reinforced Ag-based contact material of fine oxide |
| CN104532049A (en) * | 2014-11-25 | 2015-04-22 | 宁波科扬贵金属合金科技有限公司 | Silver tin oxide (AgSnO2) contact material making method |
| CN104498763A (en) * | 2014-12-30 | 2015-04-08 | 桂林电器科学研究院有限公司 | Method for processing silver tin oxide-oxide electrical contact material |
| CN105215351A (en) * | 2015-10-09 | 2016-01-06 | 中国船舶重工集团公司第七一二研究所 | A kind of silver-colored coated fin oxide condutire powder and preparation method thereof |
| CN105788891A (en) * | 2016-04-29 | 2016-07-20 | 河南省豫星华晶微钻有限公司 | High-wearing-resistance high-heat-conductivity electrical contact based on 3D printing technology and preparation process thereof |
| CN110499435A (en) * | 2019-09-20 | 2019-11-26 | 昆明贵金属研究所 | A kind of silver-based electric contact material and preparation method thereof |
| CN110499435B (en) * | 2019-09-20 | 2021-07-09 | 昆明贵金属研究所 | Silver-based electric contact material and preparation method thereof |
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