CN1477219A - 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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- CN1477219A CN1477219A CNA021327912A CN02132791A CN1477219A CN 1477219 A CN1477219 A CN 1477219A CN A021327912 A CNA021327912 A CN A021327912A CN 02132791 A CN02132791 A CN 02132791A CN 1477219 A CN1477219 A CN 1477219A
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Abstract
The preparation method of silver metal oxide electric contact material is characterized by that it adopts high-energy ball-grinding process to prepare silver-containing alloyed or intermetallic compound or obviously-fined powder, then utilizes the processes of internal oxidation and forming treatment so as to obtain the invented electric contact. It utilizes the control of partial pressure and temp. of oxygen in the course of internal oxidation of can obtain dispersed distribution of nano-grade or micrometer-grade metal oxide in silver base body. There is a self-formed interface between the oxide and silver base body.
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 add the hopcalite powder, then 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.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.
Embodiment 1
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 (6)
1, a kind of preparation method of siluer metal oxide electric contact material is characterized in that: at first prepare the powder of 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.
2, according to the preparation method of the described siluer metal oxide electric contact material of claim 1, it is characterized in that: the raw material of described high-energy ball milling is an 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.
3, according to the preparation method of the described siluer metal oxide electric contact material of claim 2, it is characterized in that: the oxide powder that adds Sn, Zn, In, Cu, Cd, Bi, W, Mo, Al, Ti, Mg, Mn, Zr, Ca, Ce, Cr, Fe, Ni, Co, Sb, Sr, Th, Pb in the raw material.
4, 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.
5, 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.
6, according to the preparation method of claim 4 or 5 described siluer metal oxide electric contact materials, it is characterized in that: wherein, densification processing is meant processing such as extruding, rolling, hot re-pressing, drawing, punching press or rammer system.
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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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| CN1230566C CN1230566C (en) | 2005-12-07 |
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| CN102312119A (en) * | 2010-06-29 | 2012-01-11 | 福达合金材料股份有限公司 | Preparation method for silver tin oxide electrical contact material |
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