CN204842969U - Silver - metal oxide electrical contact materials's preparation facilities and application - Google Patents
Silver - metal oxide electrical contact materials's preparation facilities and application Download PDFInfo
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- CN204842969U CN204842969U CN201420792532.9U CN201420792532U CN204842969U CN 204842969 U CN204842969 U CN 204842969U CN 201420792532 U CN201420792532 U CN 201420792532U CN 204842969 U CN204842969 U CN 204842969U
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Abstract
The embodiment of the utility model relates to a silver - metal oxide electrical contact materials's preparation facilities, including mixing reaction unit for mix argentiferous precursor solution and metal oxide's precursor solution, and react reductant and the mixed solution that obtains, with the wrap -around silver powder of precursor that obtains metal oxide, and heat treatment device, be used for with silver powder carries out thermal treatment under non - reducing atmosphere to make silver - metal oxide electrical contact materials, the utility model discloses still relate to an utilization silver - metal oxide electrical contact materials and an utilization of preparation facilities preparation the electrical contact that silver - metal oxide electrical contact materials made.
Description
Technical field
Embodiment of the present utility model relates to electrical contact field, and particularly, relates to a kind of preparation facilities and application of silver-metallic oxide electrical contact material.
Background technology
Electrical contact is the key element of electric switch, instrument and meter etc., carries connection, carrying and the task of disjunction normal current and fault current.In the electrical contact material manufacturing electrical contact, Ag-based electrical contact material is most important, that consumption is maximum and the most cheap electrical contact material, especially silver-base metal oxide is because of its good resistance to electrical wear, resistance fusion welding and electric conductivity, and is widely used in low tension contact material.Silver-base metal oxide electrical contact material is generally containing two components, and component is the simple metal Ag that can provide high electrical conductivity, good anti-oxidant, nitrogenize performance, and another component is metal oxide, and major decision electric arc interrupting performance, as SnO
2, ZnO etc., they add the electrical contact performance that can significantly improve electrical contact material, the electrical contact material developed mainly contains Ag-ZnO, Ag-CuO, Ag-NiO, Ag-SnO
2deng.At present, alloy inner oxidation method and powder metallurgic method are the preparation technologies of industrial applications Ag-MeO electrical contact material comparatively widely.With regard to powder metallurgical technique, at material powder preparatory phase, main employing mechanical mixture, such as mechanical alloying method, adopt this blending processes of powders, equipment is simple, Addition ofelements is easy to control, the composition of alloy can be adjusted in a big way, even tissue can be prepared, the contact that volume is larger, if but the mixed powder time (mixed vermicelli part) controls bad, powder surface situation or distribution of particles is easily made to change, cause component segregation, work hardening etc., the density of material of final preparation is lower, oxide particle is thicker, cause that resistance to arc erosion is poor affects electrical contact endurance.And the feature of internal oxidation to be alloy density high, contact electrical wear is little, the life-span is long, be convenient to produce in enormous quantities, but shortcoming is also clearly, and namely product size should not be too thick, and tissue easily occurs that " oxygen-depleted zone " causes inhomogeneities, thus properties of product are degenerated.
Utility model content
In view of the defect that above-mentioned prior art exists, embodiment of the present utility model provides a kind of silver-metallic oxide electrical contact material preparation method and preparation facilities, thus acquisition intensity and hardness significantly strengthen, processing characteristics, electric conductivity, electric erosion resistance energy and resistance fusion welding can significantly improve, the electrical contact material of especially electric life prolongation.
According to first aspect of the present utility model, provide a kind of preparation facilities of silver-metallic oxide electrical contact material, comprise;
Mixed reactor, for being mixed by the precursor solution of the precursor solution of argentiferous and metal oxide, and reacts reducing agent and the mixed solution obtained, with the silver powder that the presoma obtaining metal oxide is coated; And
Annealing device, for being heat-treated under non-reducing atmosphere by described silver powder, with obtained silver-metallic oxide electrical contact material.
In an embodiment of the present utility model, described preparation facilities also comprises filter, for filtering the suspended substance be obtained by reacting in described mixed reactor, and drying device, for filtering the sediment obtained in the described filter of drying.
In another embodiment of the present utility model, the precursor solution of described argentiferous is the silver ammino solution of silver concentration 10 ~ 1000ppm.
In another embodiment of the present utility model, the precursor solution of described metal oxide is acetate or the nitrate solution of metal, and wherein said metal is one or more in Zn, Cu, In, Ni, W, Mo.
In another embodiment of the present utility model, described metal oxide is ZnO, CuO, In
2o
3, Ni
2o, WO
3, MoO
3in one or more.
In another embodiment of the present utility model, described reducing agent is the one in hydrazine hydrate, ascorbic acid, sodium borohydride.
In another embodiment of the present utility model, described non-reducing atmosphere is inert atmosphere or oxidizing atmosphere.
In another embodiment of the present utility model, described inert atmosphere is nitrogen and/or rare gas, and wherein said rare gas is one or more in argon gas, helium, neon.
In another embodiment of the present utility model, described heat treatment is calcine 1 ~ 12h at 150 ~ 800 DEG C.
In another embodiment of the present utility model, in described silver-metallic oxide electrical contact material, the mass percent of silver is 65 ~ 99%.
In another embodiment of the present utility model, in described silver-metallic oxide electrical contact material, Argent grain and/or metal oxide particle are nanoscale.
According to another aspect of the present utility model, provide the silver-metallic oxide electrical contact material obtained by preparation facilities of the silver-metallic oxide electrical contact material of a kind of utilization according to first aspect of the present utility model, wherein said silver-metallic oxide electrical contact material is nanoscale.
According to another aspect of the present utility model, provide the electrical contact that a kind of utilization is obtained according to described silver-metallic oxide electrical contact material of the present utility model, wherein said silver-metallic oxide electrical contact material is nanoscale.
Fabricated in situ liquid phase reduction is adopted to carry out mixed powder reaction according to the preparation facilities of the silver-metallic oxide electrical contact material of embodiment of the present utility model, then by heat treatments such as drying, calcinings, presoma is made to change the nano-scale powders of oxide into, and at nanoscale silver powder surface relevant position growth forming core, thus clad nano yardstick silver powder particles; Wherein nano-metal-oxide provides strong dispersion-strengthened effect, improves the quality of electrical contact, reduces the arc erosion of electrical contact; Metal oxide and the nano level even composite refining particle of Argent grain, greatly increase the wellability between silver and metal oxide, the electric life of significant prolongation electrical contact material, electric life reaches and is greater than 1000,000 time.
Accompanying drawing explanation
Present general will only be described embodiment of the present utility model by example with reference to accompanying drawing, and wherein similar parts represent with identical Reference numeral, in accompanying drawing:
Fig. 1 is the flow chart of the preparation method of silver-metallic oxide electrical contact material according to an embodiment of the present utility model
Fig. 2 is the SEM photo figure of the silver-ZnO sample obtained according to an embodiment of preparation method of the present utility model;
Fig. 3 is the TEM photo figure of the silver-ZnO sample of Fig. 1;
Fig. 4 is the X ray diffracting spectrum of the silver-cupric oxide sample obtained according to another embodiment of preparation method of the present utility model;
Fig. 5 is the SEM photo figure of the silver-cupric oxide sample of Fig. 4;
Fig. 6 is the TEM photo figure of the silver-cupric oxide sample of Fig. 4;
Fig. 7 is the schematic diagram of the preparation facilities of silver-metallic oxide electrical contact material according to an embodiment of the present utility model;
Fig. 8 is the schematic diagram of the preparation facilities of silver-metallic oxide electrical contact material according to another embodiment of the present utility model; And
Fig. 9 is the schematic diagram of the preparation facilities of silver-metallic oxide electrical contact material according to exemplary embodiment of the present utility model.
Detailed description of the invention
Below with reference to exemplary embodiment, principle of the present utility model and spirit are described.Should be appreciated that describing these embodiments is only used to enable those skilled in the art understand better and then realize the utility model, and not limit scope of the present utility model by any way.
The preparation method of the silver-metallic oxide electrical contact material of embodiment of the present utility model is briefly adopt fabricated in situ liquid-phase reduction, filtration, drying, calcining to obtain the micro/nano level silver powder that Surface coating has nanosize metal oxide.Particularly, described preparation method comprises step: mixed by the precursor solution of the precursor solution of argentiferous and metal oxide; Reducing agent and the mixed solution obtained are reacted, to obtain the coated silver powder of metal oxide precursor; Obtained silver powder is heat-treated under non-reducing atmosphere, obtained silver-metallic oxide electrical contact material.
In an embodiment of the present utility model, as shown in Figure 1, preparation condition and processing step are:
A) preparation of mixed solution
First prepare respectively the precursor solution of argentiferous and the precursor solution of metal oxide: such as, in liquor argenti nitratis ophthalmicus, drip ammoniacal liquor to make the precursor solution that silver-colored ammonia (complexing) solution is used as argentiferous, wherein silver concentration 10 ~ 1000ppm; In the acid such as acetic acid, nitric acid, add metal hydroxides is used as metal oxide presoma with the acetic acid or nitrate of making metal, wherein metal is one or more in Zn, Cu, In, Ni, W, Mo.
Then the precursor solution of the precursor solution of argentiferous and metal oxide is mixed, particularly, in the precursor solution of argentiferous, add the precursor solution of metal oxide, such as, in silver ammino solution, add acetic acid or the nitrate solution of the metal of such as Schweinfurt green, copper nitrate and so on.
B) precipitate reduction reaction
By such as hydrazine hydrate (N
2h
4h
2o), ascorbic acid (C
6h
8o
6), the reducing agent of sodium borohydride and so on joins in the mixed solution of the presoma (such as zinc acetate) containing silver-colored ammonium ion, metal oxide and carries out precipitate reduction reaction, reaction time is 0.5 ~ 24h, be preferably 0.5h, silver ion reduction in silver-colored ammonium ion become elemental silver and is precipitated out, thus obtaining the mixture suspended substance containing argent.
C) filtration and drying
Adopt the mixture suspended substance that the filter method of such as plate compression, centrifugal or negative pressure leaching and so on is obtained by reacting to filter precipitate reduction, carry out drying obtain the coated silver powder of metal oxide precursor by filtering the sediment obtained.
D) heat treatment
Silver powder coated for the metal oxide precursor of acquisition is heat-treated under non-reducing atmosphere, namely (roasting) is calcined, heat treatment temperature is 150 ~ 800 DEG C, described non-reducing atmosphere comprises inert atmosphere or oxidizing atmosphere, thus ensure reduction reaction to occur, inert atmosphere comprises nitrogen and/or rare gas, such as argon gas, helium, one or more in neon, through calcining, metal oxide precursor changes into metal oxide, such as ZnO, CuO, In2O3, Ni2O, WO3, one or more in MoO3, thus obtain silver-metallic oxide electrical contact material (powder).
Method production process of the present utility model is simple, cost is low, is suitable for suitability for industrialized production; Obtained silver-metallic oxide powder reaches nanoscale, has strong dispersion-strengthened effect, improves performance and the life-span of electrical contact material.
Below in conjunction with specific embodiment, explain the utility model further.Should be understood that these embodiments are only not used in restriction scope of the present utility model for illustration of the utility model.
Embodiment 1
(1) prepare silver-colored ammonia complexing solution and zinc acetate solution respectively, both ratios are 1:1, wherein silver concentration 10 ~ 1000ppm;
(2) in silver-colored ammonia complexing solution, add zinc acetate solution, mix;
(3) in the mixed solution obtained in step (2), add a certain amount of hydrazine hydrate, mix, in mixed solution, silver ion and hydrazine hydrate ratio are 4:3, after question response 0.5h, filter, drying obtains the coated silver powder of zinc oxide precursor;
(4) silver powder step (3) obtained in 300 DEG C of calcining 12h, prepares Ag-ZnO electrical contact material under pure nitrogen gas atmosphere.
The sample being prepared by embodiment 1 to gained carries out test analysis, and concrete outcome is as follows:
First the content about about 30.13% that ICP-MS mass spectral analysis obtains element Zn in gained sample has been carried out, illustrate in nanometer mixed powder except silver element also comprises a large amount of Zn elements, and the compound of Zn accounts for larger proportion wherein, the mixed powder of the oxide of silver powder and Zn should be belonged in theory, and can infer that the oxide of Argent grain and Zn in this powder is commonplace, have good covered effect.
By TEM and SEM electromicroscopic photograph, phenetic analysis is carried out to the microscopic appearance of this powder, covered effect.Fig. 2 is the SEM photo figure of silver-ZnO sample prepared by embodiment 1, show the pattern photo under 5 μm and 1 μm of yardstick, can to find out in sample microstructure that disperse is compared in silver powder distribution even, connected by some solid matter glue, as can be seen from the figure some silver powder particles superficial growth goes out some solid particulate matters, and this phenomenon is analyzed further by TEM photo (Fig. 3).From the TEM photo of this sample, see that some silver powder particles surfaces form homogeneous transparent rete, and there is a large amount of granular adsorption thing in some silver powder particles surface, in uneven thickness, the direction of growth is mutually vertical with silver powder surface, judge in conjunction with analysis above, infer that particulate material is the oxide that rete forms rear adsorbent solution and separates out separately, and this rete and particulate material should be zinc oxide.
Embodiment 2
(1) prepare silver-colored ammonia complexing solution and Schweinfurt green solution respectively, both ratios are 1:1, wherein silver concentration 10 ~ 1000ppm;
(2) in silver-colored ammonia complexing solution, add Schweinfurt green solution, mix;
(3) in the mixed solution obtained in step (2), add a certain amount of hydrazine hydrate, in mixed solution, silver ion and hydrazine hydrate ratio are 4:3, mix, and after question response 0.5h, filter, drying obtains the coated silver powder of cupric oxide presoma;
(4) silver powder step (3) obtained in 300 DEG C of calcining 12h, prepares Ag-CuO electrical contact material under pure nitrogen gas atmosphere.
Embodiment 3
(1) silver-colored ammonia complexing solution and Schweinfurt green solution is prepared respectively, wherein silver concentration 10 ~ 1000ppm;
(2) in silver-colored ammonia complexing solution, add Schweinfurt green solution, both ratios are 1:1, mix;
(3) in the mixed solution obtained in step (2), add a certain amount of ascorbic acid, in mixed solution, silver ion and ascorbic acid ratio are 2:1, mix, after question response 0.5h, filtration, drying obtain the coated silver powder of cupric oxide presoma;
(4) silver powder step (3) obtained in 150 DEG C of calcining 12h, prepares Ag-CuO electrical contact material under air atmosphere.
The sample being prepared by embodiment 3 to gained carries out test analysis, and concrete outcome is as follows:
The content about about 13.06% of element Cu in gained sample is obtained by ICP-MS mass spectral analysis, illustrate in this sample and comprise the more Cu element of content, then this sample should belong to the mixed powder of the oxide of silver powder and Cu in theory, and the oxide mixing can knowing Argent grain and Cu in this powder by inference is commonplace.
By the Fig. 4 of X-ray diffractogram showing silver-cupric oxide sample, test this powder sample by XRD material phase analysis.Analyzed by the corresponding XRD software database of comparison, then this sample known contains the angle of diffraction corresponding to the corresponding crystal face of substance oxidation copper, then contain cupric oxide in this nanometer mixed powder provable, the result meeting ICP-MS mass spectral analysis and obtain also is compared in this analysis.
By TEM and SEM electromicroscopic photograph, phenetic analysis is carried out to the microscopic appearance of this powder, covered effect.Fig. 5 is the SEM photo figure of silver-cupric oxide sample prepared by embodiment 3, show the pattern photo of sample under 2 μm of yardsticks, can find out in sample microstructure, silver powder has gathering adhesion phenomenon more, and obviously can find out that silver powder particles table is coated with the thick solid matter of one deck, can judge that these clads should be solid oxidation copper by analyzing above, but covered effect also need carry out analysis and summary under larger multiplication factor, analyze further by TEM photo (Fig. 6), can observation and analysis from the TEM photo of this sample, this sample silver powder particles superficial film is formed relatively good, and it is more continuous, but the thickness low LCL of some position film is even, also there is the solid matter that on part Argent grain, upper existence is adsorbed in granular form in addition, judge in conjunction with analysis above, coated rete material should be cupric oxide, and cupric oxide coated silver powder effect is comparatively good.
Embodiment 4
(1) silver-colored ammonia complexing solution and zinc acetate solution is prepared respectively, wherein silver concentration 10 ~ 1000ppm;
(2) in silver-colored ammonia complexing solution, add zinc acetate solution, both ratios are 1:1, mix;
(3) in the mixed solution obtained in step (2), add a certain amount of hydrazine hydrate, in mixed solution, silver ion and hydrazine hydrate ratio are 4:3, mix, and after question response 0.5h, filter, drying obtains the coated silver powder of zinc oxide precursor;
(4) silver powder step (3) obtained in 600 DEG C of calcining 2h, prepares Ag-ZnO electrical contact material under pure argon atmosphere.
Embodiment 5
(1) silver-colored ammonia complexing solution and nickel acetate solution is prepared respectively, wherein silver concentration 10 ~ 1000ppm;
(2) in silver-colored ammonia complexing solution, add nickel acetate solution, both ratios are 1:1, mix;
(3) in the mixed solution obtained in step (2), add a certain amount of sodium borohydride, in mixed liquor, the ratio of silver ion and sodium borohydride is 1:1, mixes, after question response 0.5h, filtration, drying obtain the coated silver powder of nickel oxide precursor;
(4) silver powder step (3) obtained in 800 DEG C of calcining 12h, prepares Ag-Ni under pure nitrogen gas atmosphere
2o electrical contact material.
Embodiment 6
(1) silver-colored ammonia complexing solution and nickel acetate solution is prepared respectively, wherein silver concentration 10 ~ 1000ppm;
(2) in silver-colored ammonia complexing solution, add nickel acetate solution, both ratios are 1:1, mix;
(3) in the mixed solution obtained in step (2), add a certain amount of sodium borohydride, in mixed liquor, the ratio of silver ion and sodium borohydride is 1:1, mixes, after question response 24h, filtration, drying obtain the coated silver powder of nickel oxide precursor;
(4) silver powder step (3) obtained in 800 DEG C of calcining 1h, prepares Ag-Ni under pure nitrogen gas atmosphere
2o electrical contact material.
Fig. 7 shows the preparation facilities of the silver-metallic oxide electrical contact material according to an embodiment of the present utility model, comprises;
Mixed reactor 1, for making the precursor solution of argentiferous, the precursor solution mixing of metal oxide, and makes obtained mixed solution and reducing agent react, to obtain the coated silver powder of metal oxide precursor;
Annealing device 4, the silver powder obtained for heat treatment under non-reducing atmosphere is with obtained silver-metallic oxide electrical contact material.
In one embodiment, as shown in Figure 8, described preparation facilities also comprises:
Filter 2, for filtering the suspended substance be obtained by reacting in mixed reactor 1; And drying device 3, for filtering the sediment obtained in dry filtrating equipment 2.
In an embodiment of the present utility model, as shown in Figure 9, in above-mentioned preparation facilities, mixed reactor can be mixing channel 10, such as, in groove, silver ammino solution mixes with Schweinfurt green, then add hydrazine hydrate mixing and carry out precipitate reduction reaction, generate the mixture suspended substance containing elemental silver, mixture suspended substance is poured into such as plate and frame filter press 20 (or negative pressure leaching machine, filter centrifugal) and so on filter filter, the drying device that the coated sediment of silver-metallic oxide presoma that filtration obtains puts into such as vacuum drying oven 30 and so on is carried out drying, thus obtain the coated silver powder of metal oxide precursor (such as Schweinfurt green), finally silver powder is put into such as Muffle furnace 40 (or tunnel cave, meshbeltfurnace, rotary furnace and so on) annealing device in heat-treat (calcining), final obtained silver-metallic oxide (such as cupric oxide) electrical contact material.
In addition, the preparation method of the silver-metallic oxide electrical contact material of embodiment of the present utility model can also be utilized to obtain silver-metallic oxide electrical contact material.Further, the silver-metallic oxide electrical contact material of embodiment of the present utility model is utilized to obtain electrical contact.
Through giving description of the present utility model for the object illustrated and describe, but it is not intended to be exhaustive or be limited to the utility model of disclosed form.It may occur to persons skilled in the art that a lot of amendment and variant.
Claims (11)
1. a preparation facilities for silver-metallic oxide electrical contact material, is characterized in that, comprising:
Mixed reactor, for being mixed by the precursor solution of the precursor solution of argentiferous and metal oxide, and reacts reducing agent and the mixed solution obtained, with the silver powder that the presoma obtaining metal oxide is coated; And
Annealing device, for being heat-treated under non-reducing atmosphere by described silver powder, with obtained silver-metallic oxide electrical contact material.
2. preparation facilities according to claim 1, is characterized in that, also comprises:
Filter, for filtering the suspended substance be obtained by reacting in described mixed reactor; And
Drying device, for filtering the sediment obtained in the described filter of drying.
3. preparation facilities according to claim 1, is characterized in that, the precursor solution of described argentiferous is the silver ammino solution of silver concentration 10 ~ 1000ppm.
4. preparation facilities according to claim 1, is characterized in that, the precursor solution of described metal oxide is acetate or the nitrate solution of metal, and wherein said metal is the one in Zn, Cu, In, Ni, W, Mo.
5. preparation facilities according to claim 4, is characterized in that, described metal oxide is ZnO, CuO, In
2o
3, Ni
2o, WO
3, MoO
3in one.
6. preparation facilities according to claim 1, is characterized in that, described reducing agent is the one in hydrazine hydrate, ascorbic acid, sodium borohydride.
7. preparation facilities according to claim 1, is characterized in that, described non-reducing atmosphere is inert atmosphere or oxidizing atmosphere.
8. preparation facilities according to claim 7, is characterized in that, described inert atmosphere is nitrogen and/or rare gas, and wherein said rare gas is the one in argon gas, helium, neon.
9. preparation facilities according to claim 1, is characterized in that, the Argent grain in described silver-metallic oxide electrical contact material and/or metal oxide particle are nanoscale.
10. a silver-metallic oxide electrical contact material, is characterized in that, utilize the device according to any one in claim 1-9 to prepare, wherein said silver-metallic oxide electrical contact material is nanoscale.
11. 1 kinds of electrical contacts, is characterized in that, utilize silver-metallic oxide electrical contact material according to claim 10 to obtain, wherein said silver-metallic oxide electrical contact material is nanoscale.
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| WO2016091216A1 (en) * | 2014-12-12 | 2016-06-16 | 施耐德电气工业公司 | Silver-metal oxide electrical contact tip material preparation method, device and application |
| CN106903325A (en) * | 2015-12-23 | 2017-06-30 | 施耐德电器工业公司 | The preparation method of silver-tin contact material and its contact material being made |
| CN107400819A (en) * | 2017-06-15 | 2017-11-28 | 昆明理工大学 | A kind of preparation method of nano-metal-oxide enhancing Ag-based electrical contact material |
| CN109128212A (en) * | 2018-08-16 | 2019-01-04 | 西安工程大学 | A kind of preparation method of silver nickel zinc oxide alloy as electric contact material |
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| WO2016091216A1 (en) * | 2014-12-12 | 2016-06-16 | 施耐德电气工业公司 | Silver-metal oxide electrical contact tip material preparation method, device and application |
| CN105728714A (en) * | 2014-12-12 | 2016-07-06 | 施耐德电气工业公司 | Preparation method of silver-metal oxide electrical contact materials as well as device and application thereof |
| CN105728714B (en) * | 2014-12-12 | 2018-12-04 | 施耐德电气工业公司 | Preparation method, device and the application of silver-metallic oxide electrical contact material |
| US10639722B2 (en) | 2014-12-12 | 2020-05-05 | Schneider Electric Industries Sas | Preparation method and preparation device for silver-metal oxide electrical contact material and application of the material |
| CN106903325A (en) * | 2015-12-23 | 2017-06-30 | 施耐德电器工业公司 | The preparation method of silver-tin contact material and its contact material being made |
| CN106903325B (en) * | 2015-12-23 | 2021-01-26 | 施耐德电器工业公司 | Preparation method of silver-tin oxide electric contact material and electric contact material prepared by same |
| CN107400819A (en) * | 2017-06-15 | 2017-11-28 | 昆明理工大学 | A kind of preparation method of nano-metal-oxide enhancing Ag-based electrical contact material |
| CN109128212A (en) * | 2018-08-16 | 2019-01-04 | 西安工程大学 | A kind of preparation method of silver nickel zinc oxide alloy as electric contact material |
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