CN109128213A - A kind of preparation method of silver oxidation of coal tin contact alloy - Google Patents
A kind of preparation method of silver oxidation of coal tin contact alloy Download PDFInfo
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- CN109128213A CN109128213A CN201810936274.XA CN201810936274A CN109128213A CN 109128213 A CN109128213 A CN 109128213A CN 201810936274 A CN201810936274 A CN 201810936274A CN 109128213 A CN109128213 A CN 109128213A
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- silver
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 29
- 239000000956 alloy Substances 0.000 title claims abstract description 29
- 239000003245 coal Substances 0.000 title claims abstract description 29
- 230000003647 oxidation Effects 0.000 title claims abstract description 29
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 8
- 239000004332 silver Substances 0.000 title claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims description 7
- 239000002131 composite material Substances 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 41
- 239000008187 granular material Substances 0.000 claims abstract description 36
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 28
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 23
- 238000000137 annealing Methods 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- -1 silver-carbon-tin oxide Chemical compound 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 10
- 229910001128 Sn alloy Inorganic materials 0.000 claims abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011812 mixed powder Substances 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 8
- 101710134784 Agnoprotein Proteins 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- 238000003701 mechanical milling Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- AOVKLNZJIJAUBS-UHFFFAOYSA-N [C].[O].[Sn] Chemical compound [C].[O].[Sn] AOVKLNZJIJAUBS-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 229910001339 C alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- RRKGBEPNZRCDAP-UHFFFAOYSA-N [C].[Ag] Chemical compound [C].[Ag] RRKGBEPNZRCDAP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- UYKQQBUWKSHMIM-UHFFFAOYSA-N silver tungsten Chemical compound [Ag][W][W] UYKQQBUWKSHMIM-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- C22C32/0084—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 carbon or graphite as the main non-metallic constituent
-
- 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
-
- 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
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/027—Composite material containing carbon particles or fibres
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
- Contacts (AREA)
Abstract
A kind of preparation method of silver-colored oxidation of coal tin contact alloy disclosed by the invention, comprising the following steps: preparation Sn (NO3)4And AgNO3Mixed solution A, successively polyvinylpyrrolidonesolution solution, sodium borohydride solution are added in mixed solution A, and it stirs evenly, obtain mixed solution B, ammonium hydroxide is added dropwise into mixed solution B and adjusts pH value, obtain precipitated product, siller tin oxide composite granule is prepared using precipitated product, siller tin oxide composite granule and graphite composite powder are put into proportion in ball mill and carry out the mixed powder of ball milling, uniformly mixed silver-carbon-tin oxide composite granule is obtained after annealing, and silver-carbon-tin oxide composite granule is prepared into silver-colored oxidation of coal tin alloy as electric contact material.Silver consuming amount can be saved, product cost is reduced, technical process is simple.
Description
Technical field
The invention belongs to alloy preparation method technical fields, are related to a kind of preparation method of silver-colored oxidation of coal tin contact alloy.
Background technique
AgC contact material is common in low voltage equipment such as breaker, relay, change-over switch and contactor
Contact material.
Currently, known silver carbon contact material patent has: 1) patent " a kind of silver/graphite/graphene sliding electrical contact material
The preparation method of material " (application number CN201710759776.5, publication number CN107695356A, publication date 2018.02.16)；2)
Patent " a kind of preparation method of silvering graphite alkene enhancing copper-based electric contact material " (application number CN201610527507.1, it is open
Number CN105950904A, publication date 2016.09.21)；3) patent " a kind of method for preparing silver-graphite electrical contact belt " (application number
CN200910153565.2, publication number CN101693955A, publication date 2010.04.14)；4) patent " a kind of silver-tungsten carbide-carbon
The manufacturing method of electrical contact material " (application number 200510024287.2, publication number CN1658346, publication date 2005.8.24).
Although silver-colored carbon alloy as electric contact material is with good resistance fusion welding energy, good electric conductivity and has good temperature rise
Performance, but alloy anti electric arc corrosion performance under the medium above current conditions is poor.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of silver-colored oxidation of coal tin contact alloy, the raising arc resistants of energy alloy
Erosion performance.
The technical scheme adopted by the invention is that a kind of preparation method of silver oxidation of coal tin contact alloy, including following step
It is rapid:
Step 1, preparation Sn (NO3)4And AgNO3Mixed solution A；
Successively polyvinylpyrrolidonesolution solution, sodium borohydride solution is added in step 2 in mixed solution A, and stirs equal
It is even, obtain mixed solution B；
Ammonium hydroxide is added dropwise into mixed solution B and adjusts pH value for step 3, obtains precipitated product；
Step 4 prepares siller tin oxide composite granule using precipitated product；
Siller tin oxide composite granule and graphite composite powder are put into the mixed powder of progress ball milling, annealing in ball mill by step 5 in proportion
Uniformly mixed silver-carbon-tin oxide composite granule is obtained after processing；
Silver-carbon-tin oxide composite granule is prepared into silver-colored oxidation of coal tin alloy as electric contact material by step 6.
The features of the present invention also characterized in that
The specific steps of step 1 are as follows: tin grain is first added to the HNO that mass fraction is 60%~80%3In solution sufficiently
Sn (the NO of 2mol/L is made in dissolution3)4Solution；Then by Sn (NO3)4Solution is slowly added into the AgNO of 2mol/L3Aqueous solution
In, obtain mixed solution A.
In step 2: the concentration of polyvinylpyrrolidonesolution solution is 0.6~1mol/L, the concentration of sodium borohydride is 2~
3mol/L。
Step 3 specifically: mixed solution B is carried out to ultrasonic wave at 60 DEG C and stirs 2~3h, and passes through drop in this process
Add ammonium hydroxide to adjust solution ph to 2~4, is stirred for 1~3h after being added dropwise to complete, until precipitating is completely, obtains precipitated product.
Step 4 specifically: first precipitated product is put into vacuum oven, obtains dry powder after dry at 70~90 DEG C
End；Then dry powder is put into Muffle furnace, 2~4h is calcined at 500~650 DEG C；The powder that will finally be obtained after calcining
Grinding refinement is taken out at end, obtains siller tin oxide composite granule.
In step 5: the mass fraction of siller tin oxide composite granule is 60%~80%, and the mass fraction of graphite composite powder is
20%~40%, the sum of mass fraction of the two is 100%.
In step 5 mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 10mm, 5mm, and presses 2:3:
1 quantitative proportion, ratio of grinding media to material are 15~20:1, and rotational speed of ball-mill 400r/min, Ball-milling Time is 8~12h.
In step 5: annealing temperature is 500 DEG C, annealing time 2h.
In step 6 specifically: prepare silver-carbon-tin oxide composite granule using traditional compacting-sintering-extrusion process
Obtain silver-colored oxidation of coal tin alloy as electric contact material.
The beneficial effects of the present invention are:
The preparation method of silver-colored oxidation of coal tin contact alloy of the invention uses sol gel process with polyvinyl alcohol for dispersion
Agent to control the size and dispersibility that generate colloid, while preparing siller tin oxide powder as reducing agent using sodium borohydride
Body；The advantages of two kinds of contact materials of silver-colored carbon and siluer metal oxide can be had both simultaneously, it both can guarantee that contact material was with higher
Anti- melting welding, anti electric arc corrosion performance, while contact alloy can be made to reach higher conductive, heating conduction again；Silver-colored carbon of the invention
The preparation method of tin oxide contact alloy can save silver consuming amount, reduce product cost, and technical process is simple.
Detailed description of the invention
Fig. 1 is a kind of electron microscope of the embodiment of the preparation method of silver-colored oxidation of coal tin contact alloy of the present invention.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of silver-colored oxidation of coal tin contact alloy of the present invention, is specifically implemented according to the following steps:
Step 1, preparation Sn (NO3)4And AgNO3Mixed solution A；
First tin grain is added in the HNO3 solution that mass fraction is 60%~80% and is sufficiently dissolved, the Sn of 2mol/L is made
(NO3)4Solution；Then by Sn (NO3)4Solution is slowly added into the AgNO of 2mol/L3In aqueous solution, mixed solution A is obtained.
Step 2, in mixed solution A be added polyvinylpyrrolidonesolution solution as dispersing agent, after mixing evenly, then to its
Middle addition sodium borohydride solution is stirred evenly as reducing agent, and constantly, obtains mixed solution B；
The concentration of polyvinylpyrrolidonesolution solution is 0.6~1mol/L, and the concentration of sodium borohydride is 2~3mol/L.
Ammonium hydroxide is added dropwise into mixed solution B and adjusts pH value for step 3, obtains precipitated product；
Specifically: mixed solution B is carried out to ultrasonic wave at 50~70 DEG C and stirs 2~3h, and passes through drop in this process
Add ammonium hydroxide to adjust solution ph to 2~4, is stirred for 1~3h after being added dropwise to complete, until precipitating is completely, obtains precipitated product.
Step 4 prepares siller tin oxide composite granule using precipitated product；
Specifically: first precipitated product is put into vacuum oven, is obtained in 70~90 DEG C of dryings until moisture evaporation
Dry powder；Then dry powder is put into Muffle furnace, 2~4h is calcined at 500~600 DEG C；It will finally be obtained after calcining
The powder arrived takes out grinding refinement, obtains siller tin oxide composite granule.
Step 5, the siller tin oxide composite granule for being 60%~80% by mass fraction and mass fraction are 20%~40%
Graphite composite powder, the sum of mass fraction of the two be 100%；It is put into planetary ball mill in proportion and carries out the mixed powder of ball milling,
Uniformly mixed silver-carbon-tin oxide composite granule is obtained in vacuum atmosphere, after annealing, annealing temperature is 500 DEG C, annealing
Time is 2h.
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 10mm, 5mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material are 15~20:1, and rotational speed of ball-mill 400r/min, Ball-milling Time is 8~12h.
Silver-carbon-tin oxide composite granule is prepared into silver-colored oxidation of coal tin alloy as electric contact material by step 6.
Specifically: silver-colored carbon is prepared using traditional compacting-sintering-extrusion process in silver-carbon-tin oxide composite granule
Tin oxide alloy as electric contact material.
In the above manner, the preparation method of silver-colored oxidation of coal tin contact alloy of the invention, use sol gel process with
Polyvinyl alcohol is dispersing agent, to control the size and dispersibility that generate colloid, while using sodium borohydride as reducing agent, preparation
Siller tin oxide powder out；The advantages of two kinds of contact materials of silver-colored carbon and siluer metal oxide can be had both simultaneously, contact material was both can guarantee
Expect anti-melting welding with higher, anti electric arc corrosion performance, while contact alloy can be made to reach higher conductive, heating conduction again；
The preparation method of silver-colored oxidation of coal tin contact alloy of the invention can save silver consuming amount, reduce product cost, and technical process is simple.
As shown in Figure 1, the stannic oxide with the dotted pattern of black is evenly distributed in silver-colored carbon base body, it is thus possible to effectively
Improve Burning corrosion resistance energy and resistance fusion welding energy that arc erosion acts on lower alloy.
Embodiment 1
Step 1, first by tin grain be added to mass fraction be 80% HNO3It is sufficiently dissolved in solution, the Sn of 2mol/L is made
(NO3)4Solution；Then by Sn (NO3)4Solution is slowly added into the AgNO of 2mol/L3In aqueous solution, mixed solution A is obtained；
Step 2, addition concentration is 1mol/L polyvinylpyrrolidonesolution solution in mixed solution A, after mixing evenly, then to
The sodium borohydride solution of 3mol/L is wherein added, and constantly stirs evenly, obtains mixed solution B；
Step 3, mixed solution B is carried out at 70 DEG C ultrasonic wave stirring 3h, and in this process by be added dropwise ammonium hydroxide with
Solution ph is adjusted to 2,3h is stirred for after being added dropwise to complete, until precipitating is completely, obtains precipitated product；
Precipitated product is first put into vacuum oven by step 4, in 70 DEG C of dryings, until moisture evaporates, is obtained dry
Powder；Then dry powder is put into Muffle furnace, calcines 4h at 600 DEG C；Finally the powder obtained after calcining taking-up is ground
Levigateization obtains siller tin oxide composite granule；
The graphite composite powder that step 5, the siller tin oxide composite granule for being 80% by mass fraction and mass fraction are 20%；It presses
Ratio, which is put into planetary ball mill, carries out the mixed powder of ball milling, and uniformly mixed silver-is obtained in vacuum atmosphere, after annealing
Carbon-tin oxide composite granule, annealing temperature are 500 DEG C, annealing time 2h；
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 10mm, 5mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material 15:1, rotational speed of ball-mill 400r/min, Ball-milling Time 8h；
Ingredient is prepared using traditional compacting-sintering-extrusion process in silver-carbon-tin oxide composite granule by step 6
For Ag70-C20-SnO210 silver-colored oxidation of coal tin alloy as electric contact material.
Embodiment 2
Step 1, first by tin grain be added to mass fraction be 50% HNO3It is sufficiently dissolved in solution, the Sn of 2mol/L is made
(NO3)4Solution；Then by Sn (NO3)4Solution is slowly added into the AgNO of 2mol/L3In aqueous solution, mixed solution A is obtained；
Step 2, addition concentration is 0.8mol/L polyvinylpyrrolidonesolution solution in mixed solution A, after mixing evenly, then
The sodium borohydride solution of 2.5mol/L is added thereto, and constantly stirs evenly, obtains mixed solution B；
Step 3, mixed solution B is carried out at 60 DEG C ultrasonic wave stirring 3h, and in this process by be added dropwise ammonium hydroxide with
Solution ph is adjusted to 3,2h is stirred for after being added dropwise to complete, until precipitating is completely, obtains precipitated product；
Precipitated product is first put into vacuum oven by step 4, in 80 DEG C of dryings, until moisture evaporates, is obtained dry
Powder；Then dry powder is put into Muffle furnace, calcines 4h at 500 DEG C；Finally the powder obtained after calcining taking-up is ground
Levigateization obtains siller tin oxide composite granule；
The graphite composite powder that step 5, the siller tin oxide composite granule for being 70% by mass fraction and mass fraction are 30%；It presses
Ratio, which is put into planetary ball mill, carries out the mixed powder of ball milling, and uniformly mixed silver-is obtained in vacuum atmosphere, after annealing
Carbon-tin oxide composite granule, annealing temperature are 500 DEG C, annealing time 2h；
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 10mm, 5mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material 18:1, rotational speed of ball-mill 400r/min, Ball-milling Time 10h；
Ingredient is prepared using traditional compacting-sintering-extrusion process in silver-carbon-tin oxide composite granule by step 6
For Ag62-C30-SnO28 silver-colored oxidation of coal tin alloy as electric contact material.
Embodiment 3
Step 1, first by tin grain be added to mass fraction be 60% HNO3It is sufficiently dissolved in solution, the Sn of 2mol/L is made
(NO3)4Solution；Then by Sn (NO3)4Solution is slowly added into the AgNO of 2mol/L3In aqueous solution, mixed solution A is obtained；
Step 2, addition concentration is 0.6mol/L polyvinylpyrrolidonesolution solution as dispersing agent in mixed solution A, is stirred
After mixing uniformly, then the sodium borohydride solution of 2mol/L is added thereto, and constantly stir evenly, obtains mixed solution B；
Step 3, mixed solution B is carried out at 50 DEG C ultrasonic wave stirring 2h, and in this process by be added dropwise ammonium hydroxide with
Solution ph is adjusted to 4,1h is stirred for after being added dropwise to complete, until precipitating is completely, obtains precipitated product；
Precipitated product is first put into vacuum oven by step 4, in 90 DEG C of dryings, until moisture evaporates, is obtained dry
Powder；Then dry powder is put into Muffle furnace, calcines 2h at 500 DEG C；Finally the powder obtained after calcining taking-up is ground
Levigateization obtains siller tin oxide composite granule；
The graphite composite powder that step 5, the siller tin oxide composite granule for being 60% by mass fraction and mass fraction are 40%；It presses
Ratio, which is put into planetary ball mill, carries out the mixed powder of ball milling, and uniformly mixed silver-is obtained in vacuum atmosphere, after annealing
Carbon-tin oxide composite granule, annealing temperature are 500 DEG C, annealing time 2h；
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 10mm, 5mm, and presses the number of 2:3:1
Amount proportion, ratio of grinding media to material 20:1, rotational speed of ball-mill 400r/min, Ball-milling Time 12h；
Ingredient is prepared using traditional compacting-sintering-extrusion process in silver-carbon-tin oxide composite granule by step 6
For Ag55-C40-SnO25 silver-colored oxidation of coal tin alloy as electric contact material.
Claims (9)
1. a kind of preparation method of silver oxidation of coal tin contact alloy, which comprises the following steps:
Step 1, preparation Sn (NO3)4And AgNO3Mixed solution A；
Successively polyvinylpyrrolidonesolution solution, sodium borohydride solution is added in step 2 in the mixed solution A, and stirs equal
It is even, obtain mixed solution B；
Ammonium hydroxide is added dropwise into the mixed solution B and adjusts pH value for step 3, obtains precipitated product；
Step 4 prepares siller tin oxide composite granule using the precipitated product；
Siller tin oxide composite granule and graphite composite powder are put into the mixed powder of progress ball milling, annealing in ball mill by step 5 in proportion
Uniformly mixed silver-carbon-tin oxide composite granule is obtained afterwards；
Silver-carbon-tin oxide the composite granule is prepared into silver-colored oxidation of coal tin alloy as electric contact material by step 6.
2. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that the tool of step 1
Body step are as follows: tin grain is first added to the HNO that mass fraction is 60%~80%3It is sufficiently dissolved in solution, is made 2mol/L's
Sn(NO3)4Solution；Then by the Sn (NO3)4Solution is slowly added into the AgNO of 2mol/L3In aqueous solution, mixed solution is obtained
A。
3. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that in step 2: institute
The concentration for stating polyvinylpyrrolidonesolution solution is 0.6~1mol/L, and the concentration of the sodium borohydride is 2~3mol/L.
4. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that step 3 is specific
Are as follows: the mixed solution B is carried out to ultrasonic wave at 60 DEG C and stirs 2~3h, and in this process by the way that ammonium hydroxide is added dropwise to adjust
Solution ph is stirred for 1~3h after being added dropwise to complete, until precipitating is completely, obtains precipitated product to 2~4.
5. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that step 4 is specific
Are as follows: first the precipitated product is put into vacuum oven, obtains dry powder after dry at 70~90 DEG C；It then will be described
Dry powder is put into Muffle furnace, and 2~4h is calcined at 500~650 DEG C；Finally the powder obtained after calcining is taken out and is ground
Refinement, obtains siller tin oxide composite granule.
6. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that in step 5: institute
The mass fraction for stating siller tin oxide composite granule is 60%~80%, and the mass fraction of the graphite composite powder is 20%~40%,
The sum of mass fraction of the two is 100%.
7. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that described in step 5
In mechanical milling process: abrading-ball is aluminium oxide abrading-ball, and ball radius is respectively 12mm, 10mm, 5mm, and presses the quantitative proportion of 2:3:1,
Ratio of grinding media to material is 15~20:1, and rotational speed of ball-mill 400r/min, Ball-milling Time is 8~12h.
8. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that in step 5: moving back
Fiery temperature is 500 DEG C, annealing time 2h.
9. a kind of preparation method of silver-colored oxidation of coal tin contact alloy as described in claim 1, which is characterized in that have in step 6
Body are as follows: silver-colored oxidation of coal tin is prepared using traditional compacting-sintering-extrusion process in the silver-carbon-tin oxide composite granule
Alloy as electric contact material.
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| CN113500170A (en) * | 2021-07-13 | 2021-10-15 | 桂林金格电工电子材料科技有限公司 | Method for mixing and recycling silver tin oxide indium oxide waste and silver graphite waste |
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