CN1230566C - Preparation method of siluer metal oxide electric contact material - Google Patents
Preparation method of siluer metal oxide electric contact material Download PDFInfo
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- CN1230566C CN1230566C CN 02132791 CN02132791A CN1230566C CN 1230566 C CN1230566 C CN 1230566C CN 02132791 CN02132791 CN 02132791 CN 02132791 A CN02132791 A CN 02132791A CN 1230566 C CN1230566 C CN 1230566C
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- 239000000463 material Substances 0.000 title claims abstract description 26
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 16
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 21
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 11
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 10
- 238000000280 densification Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- 238000005275 alloying Methods 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 description 13
- 229910045601 alloy Inorganic materials 0.000 description 12
- 239000002245 particle Substances 0.000 description 8
- 239000000470 constituent Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910052684 Cerium Inorganic materials 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 229910017944 Ag—Cu Inorganic materials 0.000 description 3
- 229910006404 SnO 2 Inorganic materials 0.000 description 3
- 229910052776 Thorium Inorganic materials 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052712 strontium Inorganic materials 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- 229910017980 Ag—Sn Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910005793 GeO 2 Inorganic materials 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000001146 hypoxic effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- HYHSBSXUHZOYLX-WDSKDSINSA-N S-nitrosoglutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CSN=O)C(=O)NCC(O)=O HYHSBSXUHZOYLX-WDSKDSINSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- WZSWPMDIARCYDN-UHFFFAOYSA-N copper;oxosilver Chemical compound [Ag].[Cu]=O WZSWPMDIARCYDN-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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Abstract
The present invention relates to a preparation method of a silver metal oxide electric contact material, which is characterized in that a silver-containing alloyed or intermetallic compound or obviously-fined powders are prepared firstly via a high energy ball milling method; internal oxidation and forming treatment are carried out; accordingly, an electrical contact is prepared. The internal oxidation of the present invention is obviously lowered and time is greatly reduced, and also, production cost is obviously lowered. The present invention can respectively obtain disperse distribution of a nano-grade or a micrometer-grade metal oxide in a silver base body via the oxygen partial pressure and the temperature of the internal oxidation process. Self-formed interfaces are arranged between the oxide and the silver base body of the present invention. The combination of the interfaces is good, and material processing performance is enhanced. Additionally, the present invention can realize that added elements are uniformly distributed near Ag and MeO, and consequently, the functions that the added elements improve the wettability of the Ag and the MeO and enhance the performance of the electrical contact are fully exerted.
Description
Technical field:
The invention belongs to electric field of functional materials, is a kind of manufacture method of Ag-based electrical contact material.
Background technology:
Electrical contact material is the core parts and the critical material of electric power, electron device, bears the task of connection, breaking circuits and load current, has determined the connecting-disconnecting function and the contact reliability of switch.At present, people's main Agcdo (AgCdO) alloy that uses in the mesolow appliance contact.Yet the AgCdO alloy can discharge in production and use poison vapors, has the serious environmental pollution problem.And, along with electric switch proposes harsh performance requriements such as miniaturization, high reliability, long lifetime to electrical contact, the AgCdO alloy has manifested deficiency on performance index such as anti-melting welding, anti-arc erosion, development can replace the novel siluer metal oxide of AgCdO contact and further improve the important trend that alloy property is the development of mesolow electrical contact material.
Developed in the world and several nontoxic AgMeO electrical contact materials, as siller tin oxide (AgSnO
2), Ag-ZnO (AgZnO), silver copper oxide (AgCuO) etc.These AgMeO compare with AgCdO, show more good anti-melting welding and anti-arc erosion performance, successful Application on some device for switching, but still there is wretched insufficiency on its production technology and the use properties.
Powder metallurgy and two kinds of processing methodes of interior oxidation are mainly adopted in the production of AgMeO contact material.Wherein, powder metallurgy technology is with silver powder and oxidate powder mechanically mixing, through cold pressing, sintering and following process be shaped.This method is the control material composition easily, but because oxide compound and silver matrix are difficult to form the good interface combination, oxide compound hardness is higher again, make the moulding of silver oxide matrix material difficult unusually (moulding process comprises the extruding, rolling of sheet material, the rammer system of extruding, drawing and the rivet of silk material etc.).And, owing to be easy to occur the powder mixes non-uniform phenomenon, have a strong impact on quality product.
Internal oxidation is that the Ag/Me alloy is heated in oxygen-enriched environment, by the diffusion of oxygen in α-Ag, generates oxide particle at material internal.This method can obtain meticulous oxide particle and distribute, but often has the component gradient of oxide compound in the product, and the surface is many, and is middle few, has poor oxide region, and poly oxide is partially gone back easily in the crystal boundary zone, has a strong impact on the contact performance.And the interior oxidation required time of block alloy material is long, and consumes energy is many, and oxidation in some alloy (as Ag-Sn) system is difficult to has to add noble element (as typical A gSnO
2In
2O
3Alloy) promotes interior oxidising process.For addressing these problems, people's development in recent years with Ag/Me alloy atomization powdered then in the technology of oxidation, but, be difficult in industrial sizable application because the facility investment of this method is big, cost is higher.
At present, adopt the AgMeO contact of method for preparing on use propertieies such as contact resistance, still to be not so good as the AgCdO alloy, major cause is that the wetting property of these MeO and Ag is poor, and MeO separates with silver easily and gathers partially in contact surface during arcing, has influenced the stability of performances such as contact resistance.The better method that addresses this problem is to add second and third kind oxide compound constituent element, as at AgSnO
2Add In in the alloy
2O
3, Bi
2O
3, CuO, MoO
3, WO
3, GeO
2Deng.But owing to interpolation constituent element and former MeO particle in the conventional powder metallurgical technique are discrete distribution, promptly MeO particle neighbour does not add constituent element (maybe can not form composite oxides), thereby can not give full play to and improve Ag and the infiltrating effect of MeO.For this reason, DODUCO company has developed spray pyrolysis and has prepared SnO
2With Bi
2O
3, CuO, GeO
2Deng adding the hopcalite powder, with the uniform mixture (or composite oxides) of oxide compound and the powder metallurgy technology shaping of adopting routine after silver powder mixes again, electrical contact material AC3 life-span and the over-all properties prepared significantly improve then.Yet this method prepares the complex procedures of oxide mixture, and still exists conventional powder metallurgy technology to mix the problem that powder is irregular, the following process difficulty is big.
Summary of the invention:
The invention provides a kind of preparation method of siluer metal oxide electric contact material, it is characterized in that: the powder of at first preparing argentiferous alloying or intermetallic compound or remarkable refinement with high energy ball mill method; Be prepared into electrical contact through interior oxidation and forming processes again.
Among the preparation method of siluer metal oxide electric contact material of the present invention, the raw material of high-energy ball milling is at least a powder mix among Ag powder and Sn, Zn, In, Cu, Cd, Bi, W, Mo, Al, Ti, Mg, Mn, Zr, Ca, Ce, Cr, Fe, Ni, Co, Sb, Sr, Th, the Pb, and the weight percentage of Ag is 75～95% in the powder mix.
Among the preparation method of siluer metal oxide electric contact material of the present invention, can also when high-energy ball milling, in raw material, add the oxide powder of Sn, Zn, In, Cu, Cd, Bi, W, Mo, Al, Ti, Mg, Mn, Zr, Ca, Ce, Cr, Fe, Ni, Co, Sb, Sr, Th, Pb.
Among the preparation method of siluer metal oxide electric contact material of the present invention, can with the powder behind the high-energy ball milling through pre-treatment, cold pressing, sintering and densification shape, again with the shaping contact at inter process or after interior oxide treatment.Perhaps high-energy ball milling powder is at first generated the Ag-MeO composite powder through interior oxidation, then through cold pressing, sintering and densification shape.Wherein, densification processing is meant processing such as extruding, rolling, hot re-pressing, drawing, punching press or rammer system.
The present invention is applicable to various siluer metal oxide contacts, as AgSnO
2, AgZnO, AgCuO, AgCdO and the series A gMeO electrical contact material that adds other constituent element on this basis.
The invention has the beneficial effects as follows:
First: the invention provides a kind of novel preparation process, realize the preparation of contact material by the method for high-energy ball milling and interior oxidation.Compare with traditional production technique, interior oxidizing temperature significantly reduces (reducing to 400～800 ℃ from 600～900 ℃), and the time reduces (reducing to 0.1～10 hour from 10～30 hours) significantly, and production cost is significantly reduced;
Second: the powder grain size reduces significantly behind the high-energy ball milling, and can reach mutual alloying (or generating intermetallic compound).By the oxygen partial pressure and the temperature of oxidising process in controlling, the disperse of metal oxide in silver matrix that can obtain nanometer scale or micron dimension respectively distributes;
The 3rd: be the self-generating interface between oxide compound and silver matrix, interface junction gets togather, and has improved the materials processing performance;
The the 4th: can realize adding the uniform distribution of constituent element, add the effect that constituent element improves Ag and MeO wetting property and raising electrical contact performance thereby give full play to Ag, MeO neighbour.
Description of drawings:
Fig. 1 is the X-ray result after Ag-Cu powder mix and high-energy ball milling, interior oxidation, the thermoforming.
Embodiment:
(1) Ag powder and at least a metal-powder Me (among Sn, Zn, In, Cu, Cd, Bi, W, Mo, Al, Ti, Mg, Mn, Zr, Ca, Ce, Cr, Fe, Ni, Co, Sb, Sr, Th, the Pb at least a) are mixed, wherein add the oxide powder of (also can not adding) above-mentioned metallic element, the weight percentage of silver is 75～95% in the powder mix.Mixed powder is carried out high-energy ball milling make mutual alloying (or generating intermetallic compound) and refinement significantly, reach the uniform mixing of each constituent element on atom or nanoscale;
(2) with the powder behind the high-energy ball milling through pre-treatment, cold pressing, sintering and densification be shaped, with the shaping contact at inter process or after interior oxide treatment; Perhaps high-energy ball milling powder is at first generated the Ag-MeO composite powder through interior oxidation, then through cold pressing, sintering and densification shape.Wherein, densification processing is meant processing such as extruding, rolling, hot re-pressing, drawing, punching press or rammer system.
Key of the present invention is to adopt high-energy ball-milling process to realize alloying, homogenizing and the super-refinement of Ag/Me powder, and combining powder is metallurgical prepares the AgMeO electrical contact with interior oxidation technology.
With the Ag powder of 92wt% and the Cu powder uniform mixing of 8wt%, see Fig. 1 curve a.With mixed powder high-energy ball milling 6 hours, at this moment Cu was solid-solubilized in the Ag-Cu powdered alloy (curve b) that forms super-refinement among the Ag fully; Powder behind the ball milling is through oxidation in 450～600 ℃ of air behind 200～350 ℃ of vacuum preannealings, and the generation dispersed oxide is distributed in the CuO particulate powder (curve c) in the Ag matrix; Powder after the oxidation is prepared AgCuO10 contact (curve d) through heat processing and forming.
Embodiment 2
To contain the Cu powder, surplus of 8wt%, make the powdered alloy of Ag-Cu for the mixed powder of Ag powder carries out high-energy ball milling (high-energy ball milling can carry out, ball milling 2～8 hours) in vacuum, argon gas or air.Powder behind the ball milling is through 200～350 ℃ of vacuum preannealings, then through colding pressing, sintering, rolling, wire drawing, making into rivet.With rivet contact oxide treatment in 700 ℃ of warps, generate the AgCuO10 contact.
Embodiment 3
Weight ratio is respectively 80～90% Ag powder, 10～20% Sn powder mixed powder high-energy ball milling 2～10 hours in hypoxic atmosphere, make Ag-Sn binary alloy powder, powder behind the ball milling 400～650 ℃ of oxide treatment, is generated the SnO that disperse distributes in silver matrix
2Particle, SnO
2Size of particles is not more than 5 μ m.With the powder after the interior oxidation through cold pressing, sintering, hot re-pressing prepare AgSnO
2Contact.
Embodiment 4
The mixed powder that weight ratio is respectively 80～90% Ag powder, 10～20% Sn powder, 0～2% Ce powder high-energy ball milling 2～10 hours in hypoxic atmosphere, make Ag-Sn-Ce ternary metal powder, powder behind the ball milling 400～650 ℃ of oxide treatment, is generated the SnO that disperse distributes in silver matrix
2, the CeO particle, SnO
2Be not more than 5 μ m with the CeO size of particles.With the powder after the interior oxidation through cold pressing, sintering, hot re-pressing prepare AgSnO
2The CeO contact.
Claims (5)
1, a kind of preparation method of siluer metal oxide electric contact material is characterized in that:
The Ag powder is mixed with metal-powder Me, and metal-powder Me is selected from Sn, Cu, Ce is at least a, and the weight percentage of silver is 75～95% in the powder mix, carries out the powder that high-energy ball milling is prepared argentiferous alloying or intermetallic compound or remarkable refinement;
Mixed powder behind the high-energy ball milling is prepared into electrical contact through interior oxidation and forming processes, 400～800 ℃ of interior oxidizing temperatures, 0.1～10 hour time.
2, according to the preparation method of the described siluer metal oxide electric contact material of claim 1, it is characterized in that: the oxide powder that adds described metal-powder Me in the raw material.
3, according to the preparation method of the described siluer metal oxide electric contact material of claim 1, it is characterized in that: with the powder behind the high-energy ball milling through pre-treatment, cold pressing, sintering and densification shape, again with the shaping contact at inter process or after interior oxide treatment.
4, according to the preparation method of the described siluer metal oxide electric contact material of claim 1, it is characterized in that: high-energy ball milling powder is at first generated the Ag-MeO composite powder through interior oxidation, then through cold pressing, sintering and densification shape.
5, according to the preparation method of claim 3 or 4 described siluer metal oxide electric contact materials, it is characterized in that: wherein, densification processing is meant that extruding, rolling, hot re-pressing, drawing, punching press or the system of upsetting process.
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|---|---|---|---|
| CN 02132791 CN1230566C (en) | 2002-08-21 | 2002-08-21 | Preparation method of siluer metal oxide electric contact material |
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|---|---|---|---|
| CN 02132791 CN1230566C (en) | 2002-08-21 | 2002-08-21 | Preparation method of siluer metal oxide electric contact material |
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| CN1477219A CN1477219A (en) | 2004-02-25 |
| CN1230566C true CN1230566C (en) | 2005-12-07 |
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- 2002-08-21 CN CN 02132791 patent/CN1230566C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1477219A (en) | 2004-02-25 |
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