CN112151285B - Silver-based electric contact material with two-dimensional lamellar phase enhancement and preparation method thereof - Google Patents
Silver-based electric contact material with two-dimensional lamellar phase enhancement and preparation method thereof Download PDFInfo
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- CN112151285B CN112151285B CN202010922256.3A CN202010922256A CN112151285B CN 112151285 B CN112151285 B CN 112151285B CN 202010922256 A CN202010922256 A CN 202010922256A CN 112151285 B CN112151285 B CN 112151285B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0233—Composite material having a noble metal as the basic material and containing carbides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Abstract
The invention discloses a silver-based electric contact material with enhanced two-dimensional lamellar phase and a preparation method thereof, and relates to the technical field of metal-based composite materials. Compared with metallic silver, the silver-based electric contact material obtained by the method has the advantages that the hardness is improved, and meanwhile, the resistivity change is small.
Description
Technical field:
the invention relates to the technical field of metal matrix composite materials, in particular to a two-dimensional lamellar phase enhanced silver-based electric contact material and a preparation method thereof.
The background technology is as follows:
based on relevant statistics, the global electrical contact material market size in 2017 reaches $36.3 billion, and it is expected that $59.38 billion will reach $2025, and the annual composite growth rate (CAGR) is 6.34%, i.e., the electrical contact material has great market demand and a bright future. The working environment of the electric contact material determines that the electric contact material has good electric conduction and thermal conduction, good processability and certain strength and other properties, and the metallic silver has excellent electric conduction and thermal conduction, processability and oxidation resistance, so that the electric contact material is widely applied to the preparation of various electric contact materials such as relays, contactors and load switches. Although the metallic silver has extremely low contact resistance, the performance defects (such as low hardness, poor wear resistance and the like) of the metallic silver cause the metallic silver to be compounded with other materials, so that the performance of the metallic silver is improved.
Two-dimensional materials have been of interest since the advent of special structures that give them superior properties. Graphene and a metal carbide or nitride material (Mxene material) with a two-dimensional layered structure are taken as typical two-dimensional materials, have excellent mechanical properties, can be added into metal to optimize normal-temperature mechanical properties and high-temperature properties such as strength, hardness and the like of a matrix, and can be used as a reinforcing phase of an electric contact material.
Patent CN 105575684A discloses a silver-based electrical contact composite material, which is prepared by mixing graphene with silver powder through ball milling and then sintering. Patent CN 107146650a discloses an Ag-MXene contact material, which is sintered to a contact material after mixing silver and MXene by wet mixing. Although the above patents all improve the hardness of silver through the introduction of a two-dimensional lamellar reinforcing phase, the interface of a matrix and the reinforcing phase cannot be uniformly and tightly combined due to direct mixing, and the improvement on the comprehensive performance of the composite material is limited, for example, the conductivity of a contact material in CN 105575684A can be maintained, but the maximum hardness value is only 52HB. The resistivity of the contact material of CN 107146650A is 16 multiplied by 10 -3 mu.OMEGA.m is increased to (27-33). Times.10 -3 Mu omega.m, which is increased by 69-106%.
In order to improve the interface bonding effect of a matrix and an enhanced phase, patent CN 102385938A discloses a metal-based graphene composite electrical contact material and a preparation method thereof, wherein a metal precipitation layer is formed on the surface of graphene by adopting a precipitation method, and then graphene containing the precipitation layer is mixed with metal powder. Although the interface bonding effect of the graphene and the metal powder is improved to a certain extent, due to the fact that the graphene and the metal precipitation layer are poorly wetted, the heat conducting performance of the obtained composite electric contact material is still insufficient, so that heat of an electric contact cannot be timely transmitted, and larger burning loss is generated in a small breaking frequency in a rapid switching test. And because hydrazine hydrate is used in the precipitation process, the substance has high toxicity and is not beneficial to industrial production.
The invention comprises the following steps:
the invention aims to provide a two-dimensional lamellar phase reinforced silver-based electric contact material and a preparation method thereof, wherein the electric contact material is obtained by taking graphene or MXene with a surface rich in functional groups as a reinforcing phase and depositing silver on the surface, and has high hardness and small resistivity, and because hydrazine hydrate is not used in the preparation process, the electric contact material has low relative danger.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
the silver-based electric contact material with the enhanced two-dimensional lamellar phase comprises a matrix phase and an enhanced phase, wherein the matrix phase is silver, the enhanced phase is a two-dimensional lamellar structure with the surface rich in functional groups, and silver precipitates are coated on the surface of the enhanced phase.
The functional group includes an oxygen-containing functional group.
The reinforcement phase includes reduced graphene oxide (rGO) and/or MXene.
The MXene comprises Ti 3 C 2 、Ti 2 C、Ta 4 C 3 、(Ti 0.5 Nb 0.5 ) 2 C、Ti 3 CN and Mo 2 C, one or more of C.
The mass fraction of the matrix phase in the silver-based electric contact material is 90-99.9%, and the mass fraction of the reinforcing phase is 0.1-10%.
The preparation method of the silver-based electric contact material with the two-dimensional lamellar phase enhancement comprises the following specific steps:
(1) Mixing a two-dimensional lamellar material with a surface rich in functional groups with silver salt to obtain a solution A;
(2) Adding a precipitant into the solution A to form precipitation of silver ions, and coating the precipitation on the surface of the two-dimensional lamellar material;
(3) Washing, drying and carrying out heat treatment in an oxygen-free atmosphere to obtain the silver-based electric contact material.
The two-dimensional platelet material comprises graphene oxide suspensions rich in a large number of functional groups and/or MXene suspensions rich in a large number of functional groups.
The graphene oxide suspension is prepared by strong acid oxidation treatment by a Brodie method or a Staudenmailer method or a Hummers method.
The MXene suspension is prepared by acid liquor etching or acid liquor and lithium fluoride intercalation etching.
The silver salt is soluble salt, preferably one or more of silver nitrate and silver sulfate solution, and the concentration of the silver salt solution is 0.01-0.5 mol/L.
In order to provide better adsorption self-assembly of the plurality of functional groups carried on the two-dimensional lamellar reinforcing phase with silver ions, the mixing of step (1) includes, but is not limited to, one or more of magnetic stirring, mechanical stirring and ultrasonic mixing.
To facilitate the removal of impurities, the precipitants include, but are not limited to, one or more of sodium carbonate, sodium hydroxide, at a concentration of 0.01 to 0.5 moles per liter, and sufficient precipitant is added to complete precipitation of silver ions. To make precipitation more uniform, the precipitant drop rate was < 5mL/min.
The washing liquid adopted in the washing is deionized water and absolute ethyl alcohol, and the washing times are 2-3 times; the drying condition is that the vacuum is 30-80 ℃ for 2-24h.
The heat treatment comprises one or more of powder metallurgy, plasma electric spark sintering and microwave sintering, wherein the sintering atmosphere comprises vacuum or at least one of nitrogen, hydrogen and argon gas, the sintering temperature is 650-900 ℃, and the sintering time is 2-5h.
For ease of testing or use, the dried powder in step (3) may be pressed into a tablet by post-tablet heat treatment under the following conditions: tabletting at 400-600MPa, maintaining pressure for 60-180s, and molding.
The beneficial effects of the invention are as follows:
(1) According to the invention, the two-dimensional lamellar layer with the surface rich in functional groups is used as the reinforcing phase, and because the surface functional groups have polarity, silver ions are coated on the matrix in a static adsorption self-assembly and precipitation mode, so that the matrix and the reinforcing phase achieve molecular level mixing, and the interface two-phase wetting effect is better. Compared with metallic silver, the silver-based electric contact material obtained by the method has the advantages that the hardness and the heat conduction performance are improved, and meanwhile, the resistivity change is small.
(2) The invention realizes coating by means of metal ion precipitation, and does not involve substances with high toxicity such as hydrazine hydrate in the reaction, thus being beneficial to industrial production.
Description of the drawings:
FIG. 1 is a sediment electron microscope image of example 1 of the present invention;
FIG. 2 is a sediment electron microscope image of example 4 of the present invention;
FIG. 3 is a sediment electron microscope image of a comparative example of the present invention.
The specific embodiment is as follows:
the invention is further described below with reference to specific embodiments and illustrations in order to make the technical means, the creation features, the achievement of the purpose and the effect of the implementation of the invention easy to understand.
Example 1
(1) The flaky graphite is used as a raw material, graphite oxide is prepared by utilizing a Hummers method, and then the graphene oxide solution with good dispersion is obtained after ultrasonic treatment for 10 hours by using an ultrasonic machine.
(2) 3.3974g of silver nitrate is taken, 9.31mL of graphene oxide solution is added, deionized water is added to 100mL, ultrasonic mixing is carried out at low temperature, mechanical stirring is carried out for 30min, and electrostatic adsorption self-assembly is completed.
(3) Taking 0.88g of sodium hydroxide, adding 100mL of water, uniformly stirring, dripping the mixed salt solution at the dripping speed of 3mL/min, and mechanically stirring at the whole process with 800 r/min.
(4) And (3) washing and filtering the precipitate for 3 times, drying the precipitate for 12 hours at the temperature of 50 ℃ in vacuum, grinding the composite material powder, maintaining the pressure for 90 seconds under 550MPa, tabletting, and sintering in a vacuum furnace, wherein the sintering parameter is 750 ℃ and the temperature is kept for 3 hours, so as to obtain the silver-based electric contact material.
Example 2
(1) The method comprises the steps of preparing graphite oxide by using flaky graphite as a raw material through a Hummers method, and then performing ultrasonic treatment for 10 hours through an ultrasonic machine to obtain a well-dispersed 5mg/mL graphene oxide solution.
(2) 3.3974g of silver nitrate is taken, 37.52mL of graphene oxide solution is added, deionized water is added to 100mL, ultrasonic mixing is carried out at low temperature, mechanical stirring is carried out for 30min, and electrostatic adsorption self-assembly is completed.
(3) Taking 0.88g of sodium hydroxide, adding 100mL of water, uniformly stirring, dripping the mixed salt solution at the dripping speed of 4mL/min, and mechanically stirring with 750r/min as an auxiliary process.
(4) And washing and suction-filtering the precipitate for 3 times, drying at the temperature of 50 ℃ in vacuum for 12 hours, grinding the composite material powder, maintaining the pressure at 550MPa for 90 seconds, tabletting, sintering in a nitrogen atmosphere, and preserving the temperature for 3 hours at the sintering parameter of 850 ℃ to obtain the silver-based electric contact material.
Example 3
(1) The method comprises the steps of preparing graphite oxide by using flaky graphite as a raw material through a Hummers method, and then performing ultrasonic treatment for 10 hours through an ultrasonic machine to obtain a well-dispersed 5mg/mL graphene oxide solution.
(2) 1.6987g of silver nitrate is taken, 6.62mL of graphene oxide solution is added, deionized water is added to 100mL, ultrasonic mixing is carried out at low temperature, mechanical stirring is carried out for 30min, and electrostatic adsorption self-assembly is completed.
(3) Taking 0.44g of sodium hydroxide, adding 100mL of water, uniformly stirring, dripping the mixed salt solution at the dripping speed of 3mL/min, and mechanically stirring with 750r/min as an auxiliary process.
(4) Washing and suction-filtering the precipitate for 3 times, drying at 50 ℃ for 12 hours in vacuum, grinding the composite material powder, maintaining the pressure for 90 seconds under 550MPa, tabletting, sintering in a vacuum furnace, and preserving the temperature for 3 hours at 750 ℃ as sintering parameters to obtain the silver-based electric contact material.
Example 4
(1) Etching Ti using LiF and HF 3 AlC 2 Centrifugally washing to neutrality to obtain Ti with great amount of functional groups 3 C 2 1mg/mL Ti with good dispersion is obtained after argon protection ultrasonic treatment 3 C 2 A solution.
(2) 3.3974g of silver nitrate was added to 20.20mL of Ti 3 C 2 And adding deionized water to 100mL after the solution, carrying out ultrasonic mixing and mechanical stirring for 30min, and completing electrostatic adsorption self-assembly.
(3) Taking 0.88g of sodium hydroxide, adding 100mL of water, uniformly stirring, dripping the mixed salt solution at the dripping speed of 3mL/min, and mechanically stirring at the whole process with 800 r/min.
(4) Washing and suction-filtering the precipitate for 3 times, drying at the temperature of 50 ℃ for 12 hours in vacuum, grinding the composite material powder, maintaining the pressure for 90 seconds under 550MPa, tabletting, sintering in a vacuum furnace, and preserving the temperature for 3 hours at the temperature of 700 ℃ to obtain the silver-based electric contact material.
Comparative example 1
(1) 3.3974g of silver nitrate and 0.88g of sodium hydroxide are respectively added into 100mL of deionized water and stirred uniformly, the sodium hydroxide is dripped into the silver nitrate solution at the dripping speed of 3mL/min, and the whole process is assisted with 800r/min mechanical stirring.
(2) Washing and suction-filtering the precipitate for 3 times, drying at the temperature of 50 ℃ for 12 hours in vacuum, grinding the composite material powder, maintaining the pressure at 550MPa for 90 seconds, tabletting, sintering in a vacuum furnace, and preserving the temperature for 1 hour at the sintering parameter of 400 ℃ and then preserving the temperature for 3 hours at the temperature of 750 ℃ to obtain the silver-based electric contact material.
Comparative example 2
As comparative example 2, example 2 of CN 102385938A was used, and the electrical contact material obtained in comparative example 2 had a conductivity of 38.2MS/m, which was converted to a resistivity of 2.84X 10 7 μΩ·m。
As can be seen by comparing fig. 1, 2 and 3, when a two-dimensional lamellar reinforcing phase is introduced, silver ions in fig. 1 and 2 each form precipitates around the lamellar reinforcing phase.
Table 1 hardness, resistivity, thermal conductivity of the materials prepared in examples and comparative examples
The hardness and resistivity data in Table 1 were measured with reference to the standard GB/T5586-2016 electrical contact material basic Performance test method. As can be seen from table 1, when the two-dimensional lamellar reinforcing phase is introduced, the hardness of the base metal silver is improved, which is beneficial to prolonging the service life of the base metal silver, and compared with the prior art, the base metal silver has more hardness while maintaining the same level of conductivity. The enhanced phase is introduced by the method, so that the loss of electrical properties is small, and the resistivity of the silver is close to that of pure silver. As can be seen from the thermal conductivity coefficients of example 3 and comparative example 2, the thermal conductivity coefficient of example 3 is greater than that of comparative example 2 at the same graphene content.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (13)
1. A two-dimensional lamellar phase enhanced silver-based electrical contact material characterized by: comprises a matrix phase and a reinforcing phase, wherein the matrix phase is silver, the reinforcing phase is of a two-dimensional lamellar structure with a functional group-rich surface, and silver precipitates are coated on the surface of the reinforcing phase;
the preparation method comprises the following specific steps:
(1) Mixing a two-dimensional lamellar material with a surface rich in functional groups with silver salt to obtain a solution A;
(2) Adding a precipitant into the solution A to form precipitation of silver ions, and coating the precipitation on the surface of the two-dimensional lamellar material;
(3) Washing, drying and carrying out heat treatment in an oxygen-free atmosphere to obtain the silver-based electric contact material.
2. The two-dimensional lamellar phase enhanced silver-based electrical contact material in accordance with claim 1, characterized in that: the functional group includes an oxygen-containing functional group.
3. The two-dimensional lamellar phase enhanced silver-based electrical contact material in accordance with claim 1, characterized in that: the reinforcement phase includes reduced graphene oxide (rGO) and/or MXene.
4. A two-dimensional lamellar phase enhanced silver-based electrical contact material in accordance with claim 3, characterized in that: the MXene comprises Ti 3 C 2 、Ti 2 C、Ta 4 C 3 、(Ti 0.5 Nb 0.5 ) 2 C、Ti 3 CN and Mo 2 C, one or more of C.
5. The two-dimensional lamellar phase enhanced silver-based electrical contact material in accordance with claim 1, characterized in that: the mass fraction of the reinforcing phase in the silver-based electric contact material is 90-99.9%, and the mass fraction of the matrix phase is 0.1-10%.
6. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 1, characterized in that: the two-dimensional platelet material comprises graphene oxide suspensions rich in a large number of functional groups and/or MXene suspensions rich in a large number of functional groups.
7. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 6, characterized in that: the graphene oxide suspension is prepared by strong acid oxidation treatment through a Brodie method or a Staudenmailer method or a Hummers method; the MXene suspension is prepared by acid liquor etching or acid liquor and lithium fluoride intercalation etching.
8. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 1, characterized in that: the silver salt is soluble salt, and the concentration of the silver salt solution is 0.01-0.5 mol/L.
9. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 8, characterized in that: the soluble salt is one or more of silver nitrate and silver sulfate solution.
10. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 1, characterized in that: the precipitant comprises one or more of sodium carbonate and sodium hydroxide, the concentration of the precipitant is 0.01-0.5 mol/L, and the dropping speed of the precipitant is less than 5mL/min.
11. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 1, characterized in that: the washing liquid adopted in the washing is deionized water and absolute ethyl alcohol, and the washing times are 2-3 times; the drying condition is that the vacuum is 30-80 ℃ for 2-24h.
12. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 1, characterized in that: the heat treatment comprises one or more of powder metallurgy, plasma electric spark sintering and microwave sintering, wherein the sintering atmosphere comprises vacuum or at least one of nitrogen, hydrogen and argon gas, the sintering temperature is 650-900 ℃, and the sintering time is 2-5h.
13. The method for preparing a two-dimensional lamellar phase enhanced silver-based electrical contact material according to claim 1, characterized in that: the dried powder in the step (3) can be pressed into tablets and then subjected to heat treatment, wherein the conditions of pressing into tablets are as follows: tabletting at 400-600MPa, maintaining pressure for 60-180s, and molding.
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Citations (6)
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| CN102385938A (en) * | 2011-11-10 | 2012-03-21 | 电子科技大学 | Metal matrix graphene composite electrical contact material and preparation method thereof |
| CN103233136A (en) * | 2013-04-26 | 2013-08-07 | 河北工业大学 | Technology for preparing silver rare earth oxide electric contact material for low voltage electric apparatus with liquid phase method |
| CN104148663A (en) * | 2014-07-15 | 2014-11-19 | 东南大学 | Method for efficiently preparing silver nano particle-graphene three-dimensional composite structure |
| CN104700961A (en) * | 2015-03-18 | 2015-06-10 | 上海和伍新材料科技有限公司 | Graphene/silver composite material and preparation method thereof |
| CN107761081A (en) * | 2017-09-27 | 2018-03-06 | 郴州博太超细石墨股份有限公司 | A kind of graphene/silver composite material of high-compactness and preparation method thereof |
| CN108677048A (en) * | 2018-04-20 | 2018-10-19 | 西安理工大学 | A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof |
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- 2020-09-04 CN CN202010922256.3A patent/CN112151285B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102385938A (en) * | 2011-11-10 | 2012-03-21 | 电子科技大学 | Metal matrix graphene composite electrical contact material and preparation method thereof |
| CN103233136A (en) * | 2013-04-26 | 2013-08-07 | 河北工业大学 | Technology for preparing silver rare earth oxide electric contact material for low voltage electric apparatus with liquid phase method |
| CN104148663A (en) * | 2014-07-15 | 2014-11-19 | 东南大学 | Method for efficiently preparing silver nano particle-graphene three-dimensional composite structure |
| CN104700961A (en) * | 2015-03-18 | 2015-06-10 | 上海和伍新材料科技有限公司 | Graphene/silver composite material and preparation method thereof |
| CN107761081A (en) * | 2017-09-27 | 2018-03-06 | 郴州博太超细石墨股份有限公司 | A kind of graphene/silver composite material of high-compactness and preparation method thereof |
| CN108677048A (en) * | 2018-04-20 | 2018-10-19 | 西安理工大学 | A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof |
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