CN116607044A - AgWCGr contact material and preparation method thereof - Google Patents
AgWCGr contact material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 48
- 229910021389 graphene Inorganic materials 0.000 claims description 43
- 239000000843 powder Substances 0.000 claims description 43
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 26
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 20
- 229910052709 silver Inorganic materials 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 101710134784 Agnoprotein Proteins 0.000 claims description 6
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920000084 Gum arabic Polymers 0.000 claims description 6
- 241000978776 Senegalia senegal Species 0.000 claims description 6
- 235000010489 acacia gum Nutrition 0.000 claims description 6
- 239000000205 acacia gum Substances 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000001788 irregular Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 12
- 238000003466 welding Methods 0.000 abstract description 9
- 230000004927 fusion Effects 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
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- 238000001132 ultrasonic dispersion Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 11
- 239000004332 silver Substances 0.000 description 10
- 239000000306 component Substances 0.000 description 8
- 230000001965 increasing effect Effects 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 230000006872 improvement Effects 0.000 description 4
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- 230000003247 decreasing effect Effects 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
- 229910017727 AgNi Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
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- 230000002776 aggregation Effects 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QEKREONBSFPWTQ-UHFFFAOYSA-N disilver dioxido(dioxo)tungsten Chemical compound [Ag+].[Ag+].[O-][W]([O-])(=O)=O QEKREONBSFPWTQ-UHFFFAOYSA-N 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
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- 238000004154 testing of material Methods 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/059—Making alloys comprising less than 5% by weight of dispersed reinforcing phases
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
-
- 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
-
- 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
- H01H1/027—Composite material containing carbon particles or fibres
-
- 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 an AgWCGr contact material and a preparation method thereof. And after coating, adding silver powder, uniformly mixing the components in the solution under the action of mechanical stirring, and re-pressing and re-sintering the dried mixed powder to obtain the AgWCGr contact material. The AgWCGr mixed powder is prepared by adopting a method combining ultrasonic dispersion, chemical coating and wet mixing, and the AgWCGr contact material is obtained after sintering, so that the dispersion distribution of each component is realized, the interface combination among the components is improved, the erosion of electric arcs to the contact material is reduced, the fusion welding resistance of the contact material is enhanced, and the AgWCGr contact material has small and stable contact resistance and good machining performance.
Description
Technical Field
The invention belongs to the technical field of low-voltage contact materials, and particularly relates to an AgWCGr contact material and a preparation method thereof.
Background
The silver-based contact is used as a core component of the low-voltage electrical appliance, bears the task of carrying and breaking current, and the performance of the silver-based contact directly influences the service life and the reliability of the electrical equipment. With the increasing load, miniaturization and multifunction of electrical appliances, existing silver-based contact materials are difficult to meet these requirements, such as AgSnO 2 The contact resistance is increased, the temperature is increased and the machining property is poor in the service process of the contact material; the AgNi contact material has poor fusion welding resistance when in service under a large-level current service environment; agG (graphite) contact materials have poor arc erosion resistance and the like, and the stability, reliability and service life of electrical equipment are obviously affected. WC (tungsten carbide) has a high melting point and a high hardness. However, WC has weak oxidation resistance, and nonconductive tungsten oxide and silver tungstate are easy to generate on the surface of the AgWC contact under the action of high-temperature electric arc, so that the contact resistance of the contact surface is increased and the temperature is increased. The unique two-dimensional structure of the graphene (Gr) ensures that the graphene has excellent electric conduction, thermal conductivity, mechanical property and wear resistance, is an ideal reinforcement of silver-based contact materials, and is expected to improveAnd the problems of reduced mechanical property, serious material loss, unstable contact resistance and the like caused by arc ablation in the closing and breaking processes are solved. In addition, graphene as a component of the silver-based contact material can also improve the machinability of the contact material. However, the common powder mixing method is difficult to realize uniform dispersion of components, and has poor affinity among Ag, WC and Gr, so that good interface combination is difficult to obtain, and the physical property, mechanical property and electrical property of the material are obviously affected. Therefore, development of the AgWCGr contact material with excellent comprehensive performance and the preparation method thereof have important engineering significance and practical value.
Disclosure of Invention
The AgWCGr contact material has excellent arc erosion resistance and fusion welding resistance, small and stable contact resistance, good mechanical property and machining property.
The invention also aims to provide a preparation method of the AgWCGr contact material, which realizes the dispersion distribution of WC and Gr in a matrix and good combination with a silver matrix, and can effectively avoid the introduction of impurities while obtaining the AgWCGr contact material with uniform structure and good interface combination.
In order to solve the problems in the prior art, the invention adopts the following technical scheme:
the AgWCGr contact material comprises the following components in percentage by mass: 87.5 to 91.9 percent of Ag, 8 to 12 percent of WC, 0.1 to 0.5 percent of graphene (Gr) and 100 percent of the sum of the mass percentages of the components.
The preparation method of the AgWCGr contact material comprises the following steps:
step 1, respectively weighing the following materials in percentage by mass: 85% -90% of Ag powder, 8% -12% of WC powder and 0.1% -0.5% of graphene;
step 2, according to the mass fraction of 1 percent AgNO 3 Preparing silver nitrate solution by the proportion of 0.5% ammonia water, 0.1% PVP, 0.1% gum arabic and 98.3% deionized water;
step 3, adding the graphene weighed in the step 1 into the silver nitrate solution prepared in the step 2, uniformly stirring, and then placing the mixture into an ultrasonic machine for ultrasonic treatment for 60-200 min to obtain graphene suspension after the ultrasonic treatment is completed;
step 4, adding the WC powder weighed in the step 1 into the graphene suspension obtained in the step 3, carrying out mechanical stirring and oil bath heating, simultaneously adding glycol serving as a reducing agent, reacting for 30-60 min, adding the Ag powder weighed in the step 1, continuing mechanical stirring at 500rpm for 4-6 h, standing for 20-30 min after stirring is completed, pouring out supernatant, sequentially adopting deionized water and absolute ethyl alcohol for cleaning, repeating the cleaning operation for 3-5 times until the pH=7 of the mixed solution, and drying the cleaned mixed powder in a 60 ℃ oven for 6-8 h;
step 5, loading the completely dried mixed powder into a steel mould for pressing, sintering in a tubular furnace under argon atmosphere, wherein the initial pressure is 200MPa-300MPa, the dwell time is 1min-2min, the sintering temperature is 800-900 ℃, and the heat preservation is carried out for 2h-3h; the re-pressing pressure is 900MPa-1200MPa, the dwell time is 3min-5min, the sintering temperature is 600-700 ℃, the heat preservation is carried out for 1h-2h, and the AgWCGr contact material is obtained after cooling to room temperature along with the furnace.
As improvement, the particle size of the Ag powder in the step 1 is 1-10 mu m, the morphology is similar to sphere, the particle size of the WC powder is 1-10 mu m, the morphology is irregular polyhedron, the thickness of the graphene is 2nm, the sheet diameter is 2-3 mu m, and the purity of raw materials is more than 99.9%.
As an improvement, the mass ratio of the silver nitrate solution in the step 2 to the WC powder in the step 1 is 20-40:1.
As an improvement, the mass ratio of the silver nitrate solution to the ethylene glycol in the step 4 is 1:2-4.
As an improvement, the mechanical stirring speed and the oil bath temperature in the step 4 are respectively 100rpm-200rpm and 120-150 ℃.
Advantageous effects
Compared with the prior art, the AgWCGr contact material with excellent comprehensive performance and the preparation method thereof are characterized in that graphene is added into silver nitrate solution, and then agglomeration of the graphene is weakened by utilizing ultrasonic cavitation. And then carrying out Ag coating on WC and graphene in the WC-graphene-silver nitrate mixed solution by adopting a solvothermal method, so as to improve the interface combination between the component and the silver matrix. After coating, silver powder is added, uniform mixing of each component is realized in the solution under the action of mechanical stirring, and the dried mixed powder is subjected to re-pressing and re-sintering to obtain the AgWCGr contact material. The AgWCGr mixed powder is prepared by adopting a method combining ultrasonic dispersion, chemical coating and wet mixing, and the AgWCGr contact material is obtained after sintering. According to the AgWCGr contact material with excellent comprehensive performance, the dispersed WC and graphene are beneficial to alleviating corrosion of electric arcs on the contact material and enhancing fusion welding resistance of the contact material, and the contact material has small and stable contact resistance and good machining performance.
Drawings
FIG. 1 is a process flow diagram of a method for preparing AgWCGr contact material according to the present invention;
FIG. 2 is a scanning electron micrograph of a mixed powder coated with Ag of WC and Gr prepared in example 1 of the present invention;
FIG. 3 is a metallographic photograph of AgWCGr contact material prepared using 2 μmWC in example 2 of the present invention;
FIG. 4 is an anode morphology of AgWCGr contact material prepared using 10 μmWC according to example 1 of the present invention after 5000 electrical contacts at 36V/16A;
FIG. 5 is a cathode morphology of AgWCGr contact material prepared using 10 μmWC according to example 1 of the present invention after 5000 electrical contacts at 36V/16A.
Detailed Description
The AgWCGr contact material comprises the following components in percentage by mass: 87.5 to 91.9 percent of Ag, 8 to 12 percent of WC, 0.1 to 0.5 percent of graphene (Gr) and 100 percent of the sum of the mass percentages of the components.
The preparation method of the AgWCGr contact material is shown in a process flow chart as shown in figure 1, and comprises the following specific steps:
step 1, respectively weighing the following materials in percentage by mass: 85% -90% of Ag powder, 8% -12% of WC powder and 0.1% -0.5% of graphene, wherein the particle size of the Ag powder is 1-10 mu m, the morphology is similar to a sphere, the particle size of the WC powder is 1-10 mu m, the morphology is irregular polyhedron, the thickness of the graphene is about 2nm, the sheet diameter is 2-3 mu m, and the purity of raw materials is greater than 99.9%.
Step 2, according to the mass fraction of 1 percent AgNO 3 Preparing a silver nitrate solution by the proportion of 0.5% ammonia water, 0.1% PVP, 0.1% gum arabic and 98.3% deionized water, wherein the mass ratio of the silver nitrate solution to the WC powder in the step 1 is 20-40:1.
And 3, adding the graphene weighed in the step 1 into the silver nitrate solution prepared in the step 2, uniformly stirring, and then placing into an ultrasonic machine for ultrasonic treatment for 60-200 min to obtain graphene suspension after the ultrasonic treatment is completed.
And 4, adding the WC powder weighed in the step 1 into the graphene suspension obtained in the step 3, and then mechanically stirring and heating in an oil bath, wherein the rotating speed is 100rpm-200rpm, and the heating temperature is 120-150 ℃. Simultaneously adding reducer glycol, wherein the mass ratio of the silver nitrate solution to the glycol is 1:2-4. And (3) after reacting for 30-60 min, adding the Ag powder weighed in the step (1), and continuing to mechanically stir at 500rpm for 4-6 h. Standing for 20min-30min after stirring, pouring out supernatant, washing with deionized water and absolute ethanol for 3-5 times until the pH=7 of the mixed solution, and drying the washed mixed powder in a 60 ℃ oven for 6-8 h.
Step 5, loading the completely dried mixed powder into a steel mould for pressing, sintering in a tubular furnace under argon atmosphere, wherein the initial pressure is 200MPa-300MPa, the dwell time is 1min-2min, the sintering temperature is 800-900 ℃, and the heat preservation is carried out for 2h-3h; the re-pressing pressure is 900MPa-1200MPa, the dwell time is 3min-5min, the sintering temperature is 600-700 ℃, the heat preservation is carried out for 1h-2h, and the AgWCGr contact material is obtained after cooling to room temperature along with the furnace.
The present invention will be described in detail with reference to specific examples.
Example 1
And step 1, 86% of Ag powder, 12% of WC powder and 0.1% of graphene are respectively weighed according to mass percentages. Wherein the grain diameter of the Ag powder is 1-10 mu m, the appearance is similar to sphere, the grain diameter of the WC powder is 10 mu m, the appearance is irregular polyhedron, the thickness of the graphene is about 2nm, the sheet diameter is 2-3 mu m, and the purity of the raw materials is more than 99.9%.
Step 2, according to the mass fraction of 1 percent AgNO 3 Preparation of silver nitrate solution in proportion of 0.5% Ammonia Water, 0.1% PVP, 0.1% gum arabic and 98.3% deionized WaterThe mass ratio of the liquid, silver nitrate solution and WC powder in the step 1 is 20:1.
And 3, adding the graphene weighed in the step 1 into the silver nitrate solution prepared in the step 2, uniformly stirring, and then placing the mixture into an ultrasonic machine for ultrasonic treatment for 120min to obtain graphene suspension after the ultrasonic treatment is completed.
And 4, adding the WC powder weighed in the step 1 into the graphene suspension obtained in the step 3, and then mechanically stirring and heating in an oil bath, wherein the rotating speed is 100rpm, and the heating temperature is 150 ℃. Simultaneously adding reducer glycol, wherein the mass ratio of the silver nitrate solution to the glycol is 1:2. After 30min of reaction, the Ag powder weighed in the step 1 is added, and mechanical stirring is continued for 4h at the rotating speed of 500 rpm. Standing for 30min after stirring, pouring out the supernatant, washing with deionized water and absolute ethyl alcohol for 3 times until the pH value of the mixed solution is=7, and drying the washed mixed powder in a 60 ℃ oven for 8h.
Step 5, loading the completely dried mixed powder into a steel mould for pressing, sintering in a tubular furnace under argon atmosphere, wherein the initial pressure is 200MPa, the dwell time is 2min, the sintering temperature is 900 ℃, and the heat preservation is carried out for 3h; the re-pressing pressure is 1200MPa, the dwell time is 5min, the sintering temperature is 600 ℃, the heat preservation is carried out for 1h, and the AgWCGr contact material is obtained after cooling to room temperature along with the furnace.
Example 2
And step 1, respectively weighing 85% of Ag powder, 12% of WC powder and 0.1% of graphene according to mass percentages. Wherein the grain diameter of the Ag powder is 1-10 mu m, the appearance is similar to sphere, the grain diameter of the WC powder is 2 mu m, the appearance is irregular polyhedron, the thickness of the graphene is about 2nm, the sheet diameter is 2-3 mu m, and the purity of the raw materials is more than 99.9%.
Step 2, according to the mass fraction of 1 percent AgNO 3 Preparing a silver nitrate solution by the proportion of 0.5% ammonia water, 0.1% PVP, 0.1% gum arabic and 98.3% deionized water, wherein the mass ratio of the silver nitrate solution to the WC powder in the step 1 is 30:1.
And 3, adding the graphene weighed in the step 1 into the silver nitrate solution prepared in the step 2, uniformly stirring, and then placing the mixture into an ultrasonic machine for ultrasonic treatment for 120min to obtain graphene suspension after the ultrasonic treatment is completed.
And 4, adding the WC powder weighed in the step 1 into the graphene suspension obtained in the step 3, and then mechanically stirring and heating in an oil bath, wherein the rotating speed is 100rpm, and the heating temperature is 150 ℃. Simultaneously adding reducer glycol, wherein the mass ratio of the silver nitrate solution to the glycol is 1:3. And (3) after reacting for 45min, adding the Ag powder weighed in the step (1), and continuing to mechanically stir at 500rpm for 4h. Standing for 30min after stirring, pouring out the supernatant, washing with deionized water and absolute ethyl alcohol for 5 times until the pH value of the mixed solution is=7, and drying the washed mixed powder in a 60 ℃ oven for 8h.
Step 5, loading the completely dried mixed powder into a steel mould for pressing, sintering in a tubular furnace under argon atmosphere, wherein the initial pressure is 200MPa, the dwell time is 2min, the sintering temperature is 900 ℃, and the heat preservation is carried out for 3h; the re-pressing pressure is 1200MPa, the dwell time is 5min, the sintering temperature is 600 ℃, the heat preservation is carried out for 1h, and the AgWCGr contact material is obtained after cooling to room temperature along with the furnace.
Example 3
And step 1, respectively weighing 85% of Ag powder, 12% of WC powder and 0.5% of graphene according to mass percentages. Wherein the grain diameter of the Ag powder is 1-10 mu m, the appearance is similar to sphere, the grain diameter of the WC powder is 2 mu m, the appearance is irregular polyhedron, the thickness of the graphene is about 2nm, the sheet diameter is 2-3 mu m, and the purity of the raw materials is more than 99.9%.
Step 2, according to the mass fraction of 1 percent AgNO 3 Preparing a silver nitrate solution by the proportion of 0.5% ammonia water, 0.1% PVP, 0.1% gum arabic and 98.3% deionized water, wherein the mass ratio of the silver nitrate solution to the WC powder in the step 1 is 25:1.
And 3, adding the graphene weighed in the step 1 into the silver nitrate solution prepared in the step 2, uniformly stirring, and then placing into an ultrasonic machine for ultrasonic treatment for 180min to obtain graphene suspension after the ultrasonic treatment is completed.
And 4, adding the WC powder weighed in the step 1 into the graphene suspension obtained in the step 3, and then mechanically stirring and heating in an oil bath, wherein the rotating speed is 100rpm, and the heating temperature is 150 ℃. Simultaneously adding reducer glycol, wherein the mass ratio of the silver nitrate solution to the glycol is 1:3. And (3) after reacting for 45min, adding the Ag powder weighed in the step (1), and continuing to mechanically stir at 500rpm for 4h. Standing for 30min after stirring, pouring out the supernatant, washing with deionized water and absolute ethyl alcohol for 5 times until the pH value of the mixed solution is=7, and drying the washed mixed powder in a 60 ℃ oven for 8h.
Step 5, placing the dried mixed powder into a steel mould for pressing, placing the steel mould into a tubular furnace for sintering under argon atmosphere, wherein the initial pressure is 200MPa, the dwell time is 2min, the sintering temperature is 900 ℃, and the heat preservation is carried out for 3h; the re-pressing pressure is 1200MPa, the dwell time is 5min, the sintering temperature is 600 ℃, the heat preservation is carried out for 1h, and the AgWCGr contact material is obtained after cooling to room temperature along with the furnace.
Fig. 2 is a scanning electron microscope photograph of the mixed powder of WC and Gr coated with Ag prepared in step 3 of example 1 according to the present invention, and it can be seen that the Ag coating effect is good.
Fig. 3 is a metallographic photograph of an AgWCGr contact material prepared by using 2 μmWC in example 2 of the present invention, and it can be seen that WC and graphene are dispersed in a silver matrix.
FIGS. 4 and 5 are the anode and cathode morphologies, respectively, of the AgWCGr contact material prepared using 10 μmWC in example 1 of the present invention after 5000 electrical contacts at 36V/16A. It can be seen that shallow pits are formed after arc erosion of the anode of the contact material, and small protrusions are formed after arc erosion of the cathode of the contact material, indicating that the arc has low erosion degree on the anode and the cathode of the contact material.
The AgWCGr contact material prepared by the embodiment of the invention is tested by the following test method:
conductivity test: the conductivity Sigma (unit: S/m) of the material was measured using a Sigma2008 type digital eddy current metal conductivity meter and converted to international annealed copper standard units (%iacs) according to equation (1). The surface of the sample needs to be smooth and clean, no interference of oxide scale and the like, the surface is measured after calibration by using a standard sample, and the front side and the back side of each sample are respectively tested for 10 times and averaged.
(1)
Hardness testing: the hardness of the silver-based contact material was measured using an HV-1000 micro vickers durometer. And (3) carrying out coarse grinding on the sample before testing, removing surface impurities and oxide layers, and measuring after drying. The load at the time of measurement was 500g, the dwell time was 15s, the lengths of two diagonals of the indentation were measured after unloading the test force, and then the measured vickers hardness was calculated according to formula (2), 30 points (uniformly distributed over the entire sample surface) were measured on the front and back sides of each sample, respectively, and an average value was calculated.
(2)
Testing contact resistance, fusion welding force and quality loss, namely processing the prepared AgWCGr contact material into cathode and anode contacts with the diameter of 3mm by wire cutting, and testing in a JF04D electric contact material testing system, wherein the testing parameters are 36V/16A of direct current resistive load, 1Hz of contact frequency, 2mm of electrode spacing, 0.4N of contact pressure and 5000 times of operation. The contact test system automatically stores the test results of contact resistance and fusion welding force, and averages the test results, so that the overall average value can intuitively reflect the contact resistance and fusion welding force. The mass change of the contact materials before and after the electric contact test of the anode and the cathode is measured by adopting a TG382A type electronic balance.
The test results are shown in table 1:
TABLE 1 AgWCGr contact material Performance data prepared in accordance with various embodiments of the invention
As can be seen from the data of examples 1 and 2, the AgWCGr contact materials prepared in examples 1 and 2 decreased in conductivity and contact resistance and increased in hardness, fusion welding force and mass loss as WC grain size decreased. As can be seen from the data of example 2 and example 3, as the graphene content increases, the AgWCGr contact materials prepared in example 2 and example 3 decrease in conductivity and welding force, and increase in contact resistance. In all examples, the AgWCGr contact material prepared in example 2 had the best overall properties.
In summary, WC and graphene are simultaneously introduced into a silver matrix, and the AgWCGr contact material with excellent comprehensive performance is prepared.
Claims (6)
1. The AgWCGr contact material is characterized by comprising the following components in percentage by mass: 87.5 to 91.9 percent of Ag, 8 to 12 percent of WC, 0.1 to 0.5 percent of graphene (Gr) and 100 percent of the sum of the mass percentages of the components.
2. A method for preparing AgWCGr contact material according to claim 1, characterized in that,
step 1, respectively weighing the following materials in percentage by mass: 85% -90% of Ag powder, 8% -12% of WC powder and 0.1% -0.5% of graphene;
step 2, according to the mass fraction of 1 percent AgNO 3 Preparing silver nitrate solution by the proportion of 0.5% of dilute ammonia water, 0.1% of PVP, 0.1% of gum arabic and 98.3% of deionized water;
step 3, adding the graphene weighed in the step 1 into the silver nitrate solution prepared in the step 2, uniformly stirring, and then placing the mixture into an ultrasonic machine for ultrasonic treatment for 60-200 min to obtain graphene suspension after the ultrasonic treatment is completed;
step 4, adding the WC powder weighed in the step 1 into the graphene suspension obtained in the step 3, carrying out mechanical stirring and oil bath heating, adding the reducing agent glycol at the same time, reacting for 30-60 min, adding the Ag powder weighed in the step 1, continuing to mechanically stir at 500rpm for 4-6 h, standing for 20-30 min after stirring is completed, pouring out the supernatant, sequentially adopting deionized water and absolute ethyl alcohol for cleaning, repeating the cleaning operation for 3-5 times until the pH value of the mixed solution is=7, and drying the cleaned mixed powder in a 60 ℃ oven for 6-8 h;
step 5, filling the completely dried mixed powder into a die steel die for pressing, sintering in a tubular furnace under argon atmosphere, wherein the initial pressure is 200MPa-300MPa, the dwell time is 1min-2min, the sintering temperature is 800-900 ℃, and the heat preservation is carried out for 2h-3h; the re-pressing pressure is 900MPa-1200MPa, the dwell time is 3min-5min, the sintering temperature is 600-700 ℃, the heat preservation is carried out for 1h-2h, and the AgWCGr contact material is obtained after cooling to room temperature along with the furnace.
3. The method for preparing the AgWCGr contact material according to claim 2, wherein the particle size of the Ag powder in the step 1 is 1-10 μm, the morphology is sphere-like, the particle size of the WC powder is 1-10 μm, the morphology is irregular polyhedron, the thickness of the graphene is 2nm, the sheet diameter is 2-3 μm, and the purity of raw materials is more than 99.9%.
4. The method for preparing the AgWCGr contact material according to claim 2, wherein the mass ratio of the silver nitrate solution in the step 2 to the WC powder in the step 1 is 20-40:1.
5. The method for preparing the AgWCGr contact material according to claim 2, wherein the mass ratio of the silver nitrate solution to the ethylene glycol in the step 4 is 1:2-4.
6. The method for preparing AgWCGr contact material according to claim 2, wherein the mechanical stirring speed and the oil bath temperature in step 4 are 100rpm to 200rpm and 120 ℃ to 150 ℃, respectively.
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