CN111663087B - Preparation method of whisker reinforced silver tin oxide electric contact alloy - Google Patents
Preparation method of whisker reinforced silver tin oxide electric contact alloy Download PDFInfo
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- CN111663087B CN111663087B CN202010468778.0A CN202010468778A CN111663087B CN 111663087 B CN111663087 B CN 111663087B CN 202010468778 A CN202010468778 A CN 202010468778A CN 111663087 B CN111663087 B CN 111663087B
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- IVQODXYTQYNJFI-UHFFFAOYSA-N oxotin;silver Chemical compound [Ag].[Sn]=O IVQODXYTQYNJFI-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000000956 alloy Substances 0.000 title claims abstract description 38
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 39
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 24
- 229910052709 silver Inorganic materials 0.000 claims abstract description 23
- 239000004332 silver Substances 0.000 claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000011259 mixed solution Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 31
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 27
- 238000000137 annealing Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- 239000002243 precursor Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 17
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000006260 foam Substances 0.000 claims description 6
- 230000002431 foraging effect Effects 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 abstract description 6
- 230000003628 erosive effect Effects 0.000 abstract description 5
- 230000000704 physical effect Effects 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 239000000654 additive Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- KKHJTSPUUIRIOP-UHFFFAOYSA-J tetrachlorostannane;hydrate Chemical compound O.Cl[Sn](Cl)(Cl)Cl KKHJTSPUUIRIOP-UHFFFAOYSA-J 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
-
- 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
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
- H01H1/02376—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component SnO2
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Powder Metallurgy (AREA)
- Contacts (AREA)
Abstract
The invention discloses a preparation method of a whisker reinforced silver tin oxide electric contact alloy, which is implemented according to the following steps: step 1, preparing tin oxide whiskers; step 2, preparing whisker reinforced silver-tin oxide composite powder by using tin oxide whiskers; and 3, preparing the whisker reinforced silver-based electric contact alloy by using the whisker reinforced silver-tin oxide composite powder. The form of tin oxide in the silver matrix can be controlled, the dispersibility of second-phase tin oxide in the silver matrix is improved, and the second-phase oxide in the alloy is uniformly distributed; the tin oxide whisker has the characteristics of high strength, high modulus, good heat resistance, good compatibility and the like, and the mechanical property and the physical property of the silver-based electric contact alloy can be effectively improved by reinforcing the tin oxide whisker; the special structure of tin oxide whisker can maintain the uniformity of the second phase under the action of arc erosion, greatly improve the performance of the silver tin oxide electric contact alloy and prolong the service life of the silver tin oxide electric contact alloy.
Description
Technical Field
The invention belongs to the technical field of alloy material preparation, and particularly relates to a preparation method of a whisker reinforced silver tin oxide electric contact alloy.
Background
AgSnO2The AgCdO-based electric contact material is an environment-friendly electric contact material with great development prospect and can be widely applied to various relays and circuit breakers because the AgCdO-based electric contact material has excellent fusion welding resistance and arc erosion resistance. As a metal matrix composite, second phase SnO2In an Ag matrixThe distribution state of (a) directly affects the properties of the electrical contact material.
In recent years, researchers at home and abroad often add trace additives and second-phase oxide SnO2The performance of the silver tin oxide is improved by means of nanocrystallization and the like. 1. The product performance of the silver tin oxide is improved by adding trace additives to improve the wettability between the silver matrix and the second phase tin oxide. For example: 1) patent "a method for processing silver tin oxide electrical contact material containing additive" (application No. CN201410840392.2, publication No. CN104498762A, published as 2015.04.08); 2) the patent "preparation method of composite silver tin oxide electric contact material" (application No. CN201310078942.7, publication No. CN103184384A, published as 2013.07.03). 2. By adding a second phase oxide SnO2Nano-sizing and increasing SnO2The contact area of the particles and the matrix Ag is increased, and SnO under the action of electric arc is enhanced2The product performance of the silver tin oxide can be improved by the adhesion between the silver tin oxide and liquid Ag. For example: 1) patent "preparation method of micron composite tin dioxide powder for silver tin oxide electric contact material" (application No. CN201911068517.3, publication No. CN111036928A, published as 2020.04.21); 2) the patent "preparation process of micron tin dioxide powder for silver tin oxide electric contact material" (application No. CN201911068542.1, publication No. CN110902712A, published as 2020.03.24). However, whether additives are used or the second phase oxide SnO2The refinement of (2) can not avoid the agglomeration of the second phase oxide, and the second phase oxide SnO is easy to appear2The tin oxide floats on the surface of a silver molten pool under the action of electric arc for many times, and is re-enriched to generate segregation, so that the contact resistance of the contact material is increased, the temperature rise is higher, and the service performance and the service life of the contact material are seriously influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a whisker reinforced silver tin oxide electric contact alloy, which can improve the arc erosion resistance and the service life of the silver tin oxide electric contact alloy.
The invention adopts the technical scheme that a preparation method of a whisker reinforced silver tin oxide electric contact alloy is implemented according to the following steps:
step 1, preparing tin oxide whiskers;
step 2, preparing whisker reinforced silver-tin oxide composite powder by using tin oxide whiskers;
and 3, preparing the whisker reinforced silver-based electric contact alloy by using the whisker reinforced silver-tin oxide composite powder.
The invention is also characterized in that:
the specific process of the step 1 is as follows:
step 1.1, dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol, and dropwise adding a sodium hydroxide solution with the concentration of 0.8-1mol/L into the mixed solution of tin chloride under the condition of magnetic stirring to obtain a mixed solution A;
step 1.2, adding hexadecyl trimethyl ammonium bromide into the mixed solution A and fully stirring to obtain precursor solution;
step 1.3, transferring the precursor liquid into a ground conical flask, and placing the ground conical flask into a constant-temperature water bath kettle for aging to obtain a mixed liquid B;
and step 1.4, carrying out suction filtration on the mixed solution B for multiple times, taking out a filter cake after the solution is clear and has no foam, and drying the filter cake in a vacuum oven to constant weight to obtain the tin oxide whisker.
Step 1.1, dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol to obtain a solution, wherein the content of tin chloride in the obtained solution is 0.2-0.3mol/L, and the molar ratio of the hydrated tin chloride to sodium hydroxide is 1: 6-8; the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 0.8-1.0.
In the step 1.2, the concentration of hexadecyl trimethyl ammonium bromide in the precursor solution is 0.1-0.2 mol/L.
In the step 1.3, the aging temperature is 80-90 ℃, and the aging time is 4-6 h.
In step 1.4 the temperature in the vacuum oven was set to 80 ℃.
The specific process of the step 2 is as follows: putting the silver powder and the tin oxide whisker in a mass ratio of 85-92:8-15 into a horizontal planetary ball mill for full mixing, and annealing in a vacuum atmosphere to obtain the uniformly mixed whisker reinforced silver-tin oxide composite powder.
The ball milling process of the horizontal planetary ball mill has the following relevant parameters: the grinding balls are alumina grinding balls, the diameters of the grinding balls are respectively 12mm, 8mm and 5mm, the quantity ratio is 1:3:2, the ball-material ratio is 6-12:1, the ball-milling rotating speed is 300-600r/min, and the ball-milling time is 2-5 h.
Parameters relevant to the annealing treatment: the annealing temperature is 400-600 ℃, and the annealing time is 2-4 h.
The specific process of the step 3 is as follows: and pressing, sintering and extruding the whisker reinforced silver-tin oxide composite powder to obtain the whisker reinforced silver-based electric contact alloy.
The invention has the beneficial effects that:
the invention relates to a preparation method of a whisker reinforced silver tin oxide electric contact alloy, which takes tin chloride hydrate as a tin source and Cetyl Trimethyl Ammonium Bromide (CTAB) as a surfactant, obtains tin oxide whiskers after aging, suction filtration and vacuum drying, obtains whisker reinforced silver tin oxide composite powder through high-energy ball milling, and further prepares the whisker reinforced silver-based electric contact alloy. The tin oxide whisker has the characteristics of high strength, high modulus, good heat resistance, good compatibility and the like, and the mechanical property and the physical property of the silver-based electric contact alloy can be effectively improved by reinforcing the tin oxide whisker. In addition, the tin oxide whisker with a special structure prepared by a hydrothermal method is used for replacing the traditional tin oxide particles, and the obtained whisker reinforced silver-based electric contact material can effectively avoid the situation that second-phase tin oxide is difficult to suspend in a liquid silver molten pool and is separated from a silver matrix and enriched on the surface of a contact, so that the uniformity of the second phase can be maintained under the action of arc erosion, and the performance and the service life of the silver-tin oxide electric contact alloy are greatly improved.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a whisker reinforced silver tin oxide electric contact alloy, which is implemented according to the following steps:
step 1, preparing tin oxide whiskers; the specific process is as follows:
step 1.1, dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol, and dropwise adding a sodium hydroxide solution with the concentration of 0.8-1mol/L into the mixed solution of tin chloride under the condition of magnetic stirring to obtain a mixed solution A;
dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol to obtain a solution, wherein the content of tin chloride in the obtained solution is 0.2-0.3mol/L, and the molar ratio of the hydrated tin chloride to sodium hydroxide is 1: 6-8; the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 0.8-1.0.
Step 1.2, adding hexadecyl trimethyl ammonium bromide into the mixed solution A and fully stirring to obtain precursor solution; the concentration of hexadecyl trimethyl ammonium bromide in the precursor liquid is 0.1-0.2 mol/L.
Step 1.3, transferring the precursor liquid into a ground conical flask, and placing the ground conical flask into a constant-temperature water bath kettle for aging to obtain a mixed liquid B; the aging temperature is 80-90 ℃, and the aging time is 4-6 h.
And step 1.4, carrying out suction filtration on the mixed solution B for multiple times, taking out a filter cake after the solution is clear and has no foam, putting the filter cake in a vacuum oven, setting the temperature in the vacuum oven to be 80 ℃, and drying to constant weight to obtain the tin oxide whisker.
Step 2, preparing whisker reinforced silver-tin oxide composite powder by using tin oxide whiskers; the specific process is as follows: putting the silver powder and the tin oxide whisker in a mass ratio of 85-92:8-15 into a horizontal planetary ball mill for full mixing, and annealing in a vacuum atmosphere to obtain the uniformly mixed whisker reinforced silver-tin oxide composite powder.
The ball milling process of the horizontal planetary ball mill has the following relevant parameters: the grinding balls are alumina grinding balls, the diameters of the grinding balls are respectively 12mm, 8mm and 5mm, the quantity ratio is 1:3:2, the ball-material ratio is 6-12:1, the ball-milling rotating speed is 300-600r/min, and the ball-milling time is 2-5 h.
Parameters relevant to the annealing treatment: the annealing temperature is 400-600 ℃, and the annealing time is 2-4 h.
Step 3, preparing a whisker reinforced silver-based electric contact alloy by using the whisker reinforced silver-tin oxide composite powder; the specific process is as follows:
and pressing, sintering and extruding the whisker reinforced silver-tin oxide composite powder to obtain the whisker reinforced silver-based electric contact alloy.
Example 1
A preparation method of a whisker reinforced silver tin oxide electric contact alloy is implemented according to the following steps:
dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol to obtain a solution with the tin chloride content of 0.2mol/L, and dropwise adding a sodium hydroxide solution with the concentration of 0.8mol/L into the mixed solution of tin chloride under the condition of magnetic stirring to obtain a mixed solution A; wherein the molar ratio of the hydrated tin chloride to the sodium hydroxide is 1: 6; the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 0.8. adding hexadecyl trimethyl ammonium bromide into the mixed solution A and fully stirring to obtain precursor solution; the concentration of hexadecyl trimethyl ammonium bromide in the precursor solution is 0.1 mol/L. Transferring the precursor liquid into a ground conical flask, and placing the ground conical flask into a constant-temperature water bath kettle for aging to obtain a mixed liquid B; the aging temperature is 80 ℃, and the aging time is 4 h. And (3) carrying out suction filtration on the mixed solution B for many times, taking out a filter cake after the solution is clear and has no foam, putting the filter cake into a vacuum oven, setting the temperature in the vacuum oven to be 80 ℃, and drying to constant weight to obtain the tin oxide whisker.
Putting the silver powder and the tin oxide whisker into a horizontal planetary ball mill according to the mass ratio of 92:8 for full mixing, and carrying out annealing treatment in a vacuum atmosphere to obtain the uniformly mixed whisker reinforced silver-tin oxide composite powder.
The ball milling process of the horizontal planetary ball mill has the following relevant parameters: the grinding balls are alumina grinding balls, the diameters of the grinding balls are 12mm, 8mm and 5mm respectively, the grinding balls are proportioned according to the quantity ratio of 1:3:2, the ball-material ratio is 6:1, the ball-milling rotating speed is 300r/min, and the ball-milling time is 2 hours.
Parameters relevant to the annealing treatment: the annealing temperature is 400 ℃, and the annealing time is 2 h.
Pressing, sintering and extruding the whisker reinforced silver-tin oxide composite powder to obtain Ag92 SnO2The whisker of 8 reinforces the silver-based electrical contact alloy.
Example 2
A preparation method of a whisker reinforced silver tin oxide electric contact alloy is implemented according to the following steps:
dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol to obtain a solution with the tin chloride content of 0.25mol/L, and dropwise adding a sodium hydroxide solution with the concentration of 0.9mol/L into the mixed solution of tin chloride under the condition of magnetic stirring to obtain a mixed solution A; wherein the molar ratio of the hydrated tin chloride to the sodium hydroxide is 1: 7; the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 0.9. adding hexadecyl trimethyl ammonium bromide into the mixed solution A and fully stirring to obtain precursor solution; the concentration of hexadecyl trimethyl ammonium bromide in the precursor solution is 0.15 mol/L. Transferring the precursor liquid into a ground conical flask, and placing the ground conical flask into a constant-temperature water bath kettle for aging to obtain a mixed liquid B; the aging temperature is 85 ℃, and the aging time is 5 h. And (3) carrying out suction filtration on the mixed solution B for many times, taking out a filter cake after the solution is clear and has no foam, putting the filter cake into a vacuum oven, setting the temperature in the vacuum oven to be 80 ℃, and drying to constant weight to obtain the tin oxide whisker.
And putting the silver powder and the tin oxide whisker in a mass ratio of 88:12 into a horizontal planetary ball mill for full mixing, and annealing in a vacuum atmosphere to obtain the uniformly mixed whisker reinforced silver-tin oxide composite powder.
The ball milling process of the horizontal planetary ball mill has the following relevant parameters: the grinding balls are alumina grinding balls, the diameters of the grinding balls are 12mm, 8mm and 5mm respectively, the grinding balls are proportioned according to the quantity ratio of 1:3:2, the ball-material ratio is 9:1, the ball-milling rotating speed is 450r/min, and the ball-milling time is 3.5 h.
Parameters relevant to the annealing treatment: the annealing temperature is 500 ℃, and the annealing time is 3 h.
Pressing, sintering and extruding the whisker reinforced silver-tin oxide composite powder to obtain Ag88 SnO2The whisker of 12 reinforces the silver-based electrical contact alloy.
Example 3
A preparation method of a whisker reinforced silver tin oxide electric contact alloy is implemented according to the following steps:
dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol to obtain a solution with the tin chloride content of 0.3mol/L, and dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the mixed solution of tin chloride under the condition of magnetic stirring to obtain a mixed solution A; wherein the molar ratio of the hydrated tin chloride to the sodium hydroxide is 1: 8; the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 1.0. adding hexadecyl trimethyl ammonium bromide into the mixed solution A and fully stirring to obtain precursor solution; the concentration of hexadecyl trimethyl ammonium bromide in the precursor solution is 0.2 mol/L. Transferring the precursor liquid into a ground conical flask, and placing the ground conical flask into a constant-temperature water bath kettle for aging to obtain a mixed liquid B; the aging temperature is 90 ℃, and the aging time is 6 h. And (3) carrying out suction filtration on the mixed solution B for many times, taking out a filter cake after the solution is clear and has no foam, putting the filter cake into a vacuum oven, setting the temperature in the vacuum oven to be 80 ℃, and drying to constant weight to obtain the tin oxide whisker.
And putting the silver powder and the tin oxide whisker in a mass ratio of 85:15 into a horizontal planetary ball mill for full mixing, and annealing in a vacuum atmosphere to obtain the uniformly mixed whisker reinforced silver-tin oxide composite powder.
The ball milling process of the horizontal planetary ball mill has the following relevant parameters: the grinding balls are alumina grinding balls, the diameters of the grinding balls are respectively 12mm, 8mm and 5mm, the ball-material ratio is 12:1 according to the quantity ratio of 1:3:2, the ball-milling rotating speed is 600r/min, and the ball-milling time is 5 hours.
Parameters relevant to the annealing treatment: the annealing temperature is 600 ℃, and the annealing time is 4 h.
Pressing, sintering and extruding the whisker reinforced silver-tin oxide composite powder to obtain Ag85 SnO215 the whisker reinforced silver-based electrical contact alloy.
According to the preparation method of the whisker reinforced silver tin oxide electric contact alloy, tin chloride hydrate is used as a tin source by a hydrothermal method, Cetyl Trimethyl Ammonium Bromide (CTAB) is used as a surfactant, tin oxide whiskers are obtained after aging, suction filtration and vacuum drying, whisker reinforced silver tin oxide composite powder is obtained through high-energy ball milling, and then the whisker reinforced silver-based electric contact alloy is prepared. The tin oxide whisker has the characteristics of high strength, high modulus, good heat resistance, good compatibility and the like, and the mechanical property and the physical property of the silver-based electric contact alloy can be effectively improved by reinforcing the tin oxide whisker. In addition, the tin oxide whisker with a special structure prepared by a hydrothermal method is used for replacing the traditional tin oxide particles, and the obtained whisker reinforced silver-based electric contact material can effectively avoid the situation that second-phase tin oxide is difficult to suspend in a liquid silver molten pool and is separated from a silver matrix and enriched on the surface of a contact, so that the uniformity of the second phase can be maintained under the action of arc erosion, and the performance and the service life of the silver-tin oxide electric contact alloy are greatly improved.
Claims (4)
1. A preparation method of a whisker reinforced silver tin oxide electric contact alloy is characterized by comprising the following steps:
step 1, preparing tin oxide whiskers: the specific process of the step 1 is as follows:
step 1.1, dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol, and dropwise adding a sodium hydroxide solution with the concentration of 0.8-1mol/L into the mixed solution of tin chloride under the condition of magnetic stirring to obtain a mixed solution A;
step 1.1, dissolving hydrated tin chloride in a mixed solution of deionized water and absolute ethyl alcohol, wherein the content of tin chloride in the obtained solution is 0.2-0.3mol/L, and the molar ratio of the hydrated tin chloride to sodium hydroxide is 1:6-8, wherein the volume ratio of the deionized water to the absolute ethyl alcohol is 1: 0.8-1.0;
step 1.2, adding cetyl trimethyl ammonium bromide into the mixed solution A and fully stirring to obtain precursor solution, wherein the concentration of the cetyl trimethyl ammonium bromide in the precursor solution is 0.1-0.2mol/L;
step 1.3, transferring the precursor liquid into a ground conical flask, and placing the ground conical flask into a constant-temperature water bath kettle for aging to obtain a mixed liquid B;
step 1.4, carrying out suction filtration on the mixed solution B for multiple times, taking out a filter cake after the solution is clear and has no foam, and drying the filter cake in a vacuum oven to constant weight to obtain tin oxide whiskers;
step 2, preparing whisker reinforced silver-tin oxide composite powder by using tin oxide whiskers: the specific process of the step 2 is as follows: putting the silver powder and the tin oxide whisker into a horizontal planetary ball mill according to the mass ratio of 85-92:8-15 for full mixing, and annealing in a vacuum atmosphere to obtain uniformly mixed whisker reinforced silver-tin oxide composite powder;
the ball milling process related parameters of the horizontal planetary ball mill are as follows: the grinding balls are alumina grinding balls, the diameters of the grinding balls are respectively 12mm, 8mm and 5mm, the quantity ratio is 1:3:2, the ball-material ratio is 6-12:1, the ball-milling rotating speed is 300-;
the relevant parameters of the annealing treatment are as follows: the annealing temperature is 400-600 ℃, and the annealing time is 2-4h;
and 3, preparing the whisker reinforced silver-based electric contact alloy by using the whisker reinforced silver-tin oxide composite powder.
2. The method for preparing a whisker reinforced silver tin oxide electrical contact alloy as claimed in claim 1, wherein the aging temperature in step 1.3 is 80-90 ℃ and the aging time is 4-6 h.
3. The method for preparing a whisker reinforced silver tin oxide electrical contact alloy as claimed in claim 1, wherein the temperature in the vacuum oven is set to 80 ℃ in step 1.4.
4. The method for preparing the whisker reinforced silver tin oxide electrical contact alloy according to claim 1, wherein the specific process in the step 3 is as follows: and pressing, sintering and extruding the whisker reinforced silver-tin oxide composite powder to obtain the whisker reinforced silver-based electric contact alloy.
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| CN104528810A (en) * | 2015-01-20 | 2015-04-22 | 天津大学 | Preparation method for preparing stannic oxide nanorod cluster by using one-step hydrothermal method |
| CN105236471A (en) * | 2015-09-30 | 2016-01-13 | 上海工程技术大学 | Tin dioxide nanorod with controllable length/diameter ratio and preparation method thereof |
| CN105908108A (en) * | 2016-04-14 | 2016-08-31 | 西安工程大学 | Preparation method of tin oxide fiber reinforced silver-based electric contact alloy |
| CN110735094A (en) * | 2019-11-12 | 2020-01-31 | 西安工程大学 | Nano tin oxide fiber reinforced silver tin oxide low-voltage contact material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528810A (en) * | 2015-01-20 | 2015-04-22 | 天津大学 | Preparation method for preparing stannic oxide nanorod cluster by using one-step hydrothermal method |
| CN105236471A (en) * | 2015-09-30 | 2016-01-13 | 上海工程技术大学 | Tin dioxide nanorod with controllable length/diameter ratio and preparation method thereof |
| CN105908108A (en) * | 2016-04-14 | 2016-08-31 | 西安工程大学 | Preparation method of tin oxide fiber reinforced silver-based electric contact alloy |
| CN110735094A (en) * | 2019-11-12 | 2020-01-31 | 西安工程大学 | Nano tin oxide fiber reinforced silver tin oxide low-voltage contact material and preparation method thereof |
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