CN106903325A - The preparation method of silver-tin contact material and its contact material being made - Google Patents
The preparation method of silver-tin contact material and its contact material being made Download PDFInfo
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- CN106903325A CN106903325A CN201510977375.8A CN201510977375A CN106903325A CN 106903325 A CN106903325 A CN 106903325A CN 201510977375 A CN201510977375 A CN 201510977375A CN 106903325 A CN106903325 A CN 106903325A
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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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
Abstract
A kind of silver-tin contact material and preparation method thereof, including：Certain density reductant solution, silver ammino solution and sodium stannate solution are prepared respectively；Silver ammino solution is mixed by a certain percentage with sodium stannate solution, to constitute mixed liquor, acetic acid is added dropwise in mixed liquor, the pH value in regulation mixed liquor contains Ag to be formed+Sn (OH)4Colloidal sol or solution；Reductant solution is added dropwise to Sn (OH)4In colloidal sol or solution, constant temperature is stirred or ultrasonic wave added reaction, and collection obtains powder after supernatant liquor, and cleaning, dry, cooling are removed after standing；Powder is heat-treated under non-reducing atmosphere, Ag-SnO is prepared2Composite granule.So make the particle of its composite granule up to nanoscale, improve sintering character, solve the SnO of prior powder metallurgy technique presence2With Ag interface cohesion problems, and have the advantages that preparation process is simple, low cost, preparation condition are easily controllable, synthesis cycle is short, properties of product are good.
Description
Technical field
The present invention relates to the silver-based electric contact material in a kind of contactor, relay and switch.Especially
It is related to a kind of silver-tin (Ag-SnO2) contact material and preparation method thereof.
Background technology
Typically, contact material uses silver-based electric contact material, because it has preferable resistance to electric mill
Damage, resistance fusion welding energy and excellent electric conductivity, its contact resistance are stable and smaller, therefore all kinds of
It is widely used in electrical equipment, household electrical appliance, car electrics part, the Aero-Space electric component of commutator for light-heavy load,
It is one of the most commonly used contact material.
Specifically, the electric current of Ag-MeO applications is widely used in several volts and arrives several from tens peaces to several kilo-amperes
In various low-voltage electrical apparatuses of kilovolt.Most widely used in Ag-MeO materials is Ag-CdO, Ag-CdO because
Its excellent resistance fusion welding energy, resistance to electrical wear and relatively low contact resistance, it is wide in medium load electrical equipment
It is general to use, it is referred to as omnipotent contact, but due to that can be produced during manufacturing, using Ag-CdO materials
Raw " cadmium poison ", some countries and regions disable or limit the use of to Ag-CdO contact materials.For ring
The requirement of border protection, an important development direction of silver-based electric contact material is to develop to substitute
The new material of Ag-CdO.
Further, Ag-SnO2Contact material is a kind of novel non-toxic electrical contact that have developed rapidly in recent years
Material, in addition to the popular feature with general Ag-MeO materials, also invades with stronger arc resistant
Erosion, resistance fusion welding and heat endurance, using scope up to 10~1000A, be at present contactor, after
One of main environment-friendly type contact material of Ag-CdO is substituted in electrical equipment and switch.
In this way, the making Ag-SnO for arising at the historic moment2The method of contact material has various.At present, alloy
Internal oxidation and powder metallurgic method are the relatively broad Ag-SnO of industrial applications2The system of contact material
Standby technique.The material grains structure that wherein prepared by the alloy inner oxidation method is fine, intensity, hardness, resistance to electricity
Ability is lost in arcing and anti-melting welding power is all higher, but, material uneven microstructure in itself prepared by the method,
Easily there is poor oxide strip and oxide buildup, be mingled with and the tissue defects such as stomata.The powder metallurgic method exists
Material powder preparatory phase, mainly using mechanical mixture, such as mechanical alloying method, using this mixed powder work
Skill, equipment is simple, using silver powder and putty powder mechanical mixture, can arbitrarily add different type and difference
The additive of amount, can be uniform in the composition of interior adjustment alloy in a big way, materials microstructure, without poor
Metal oxide area, if mixed powder time control is bad, easily becomes powder surface appearance or distribution of particles
Change, cause component segregation to process hardening etc., the final density of material for preparing is relatively low, tin oxide powder granule
Size is generally that 3~5cm is thicker, the contact resistance for causing contact is big, temperature rise, arc ablation resistance compared with
Difference, influences electrical contact endurance.
The content of the invention
The purpose of the present invention is mainly to provide a kind of Ag-SnO2The preparation method of contact material and
Ag-SnO2Contact material, its Ag-SnO2The preparation method of contact material is closed by using in situ
Ag-SnO is prepared into liquid phase reduction2Nano-powder, powder process is mixed with chemically composited replacement physics, from
And realize SnO2More uniformly mix with Ag, and improve SnO simultaneously2With the wellability of Ag.
It is that, up to above-mentioned purpose, the present invention provides a kind of Ag-SnO2The preparation method of contact material, the party
Method is comprised the following steps：
(1) certain density reductant solution, silver ammino solution and sodium stannate solution are prepared respectively；
(2) silver ammino solution is mixed by a certain percentage with the sodium stannate solution, to constitute a mixed liquor,
Acetic acid is added dropwise in the mixed liquor, the pH value in the mixed liquor is adjusted, to form Sn (OH)4Colloidal sol or
Solution；
(3) reductant solution is added dropwise to the Sn (OH) of gained in step (2)4In colloidal sol or solution,
Constant temperature is stirred or ultrasonic wave added reaction, is received after supernatant liquor, and cleaning, dry, cooling are removed after standing
Collection obtains powder；
(4) powder for obtaining will be collected in step (3) to be heat-treated under non-reducing atmosphere, is prepared
Obtain Ag-SnO2Composite granule.
The present invention also provides a kind of Ag-SnO being made of above-mentioned preparation method2Contact material.
The present invention also provides a kind of silver-tin contact material, wherein the silver-tin contact material
Comprising Ag particles and SnO2Particle, the wherein SnO2Particle is uniformly coated on Ag particle surfaces,
To obtain uniform Ag-SnO2Composite granule.
Brief description of the drawings
Fig. 1 is Ag-SnO of the present invention2The flow chart of the preparation method of contact material；
Fig. 2 is the Ag-SnO that preparation method of the present invention is made2ESEM (SEM) figure of product；
Fig. 3 is energy spectrum analysis (EDS) figure in Fig. 2；
Fig. 4 is the Ag-SnO that preparation method of the present invention is made2The transmission electron microscope (TEM) of product
Figure；
Fig. 5 A are existing Ag-SnO2The effect diagram of sample arcing energy；；
Fig. 5 B are Ag-SnO of the invention2The effect diagram of sample arcing energy；
Fig. 6 A are existing Ag-SnO2Sample opens the effect diagram of arc time；
Fig. 6 B are Ag-SnO of the invention2Sample opens the effect diagram of arc time；
Specific embodiment
Ag-SnO2The current preparation method of material has：Its colloidal sol is prepared by raw material of two hydrated stannous chlorides
Solution, adds silver nitrate solution, regulation pH value control Sn2 +Sol particles and Ag+Ion is in situ to be occurred
Chemical reaction, the Ag-SnO for preparing2Composite particles, due to SnO2Content more a height of 10~90%,
Also need to mix reduction SnO with fine silver powder2Content is to 5~30% then repressed, sintering, hot extrusion are obtained
To electric contact composite material.The method will inevitably generate a part of silver nitride precipitation to be caused finally
Contact product content it is impure, and the Ag-SnO that the method is prepared2SnO in composite particles2Contain
Amount is higher also to need addition fine silver powder to reduce SnO2Content, not only increase preparation section and addition silver
Powder and Ag-SnO2Easily form the uneven problem of mixing.
Therefore, the present invention has innovated a kind of Ag-SnO2Preparation method, it is mainly by nanoscale
It is compound to prepare that addition phase particle size is smaller, the uniform mixed powder of Dispersed precipitate.I.e.：By argentiferous
The precursor solution (i.e. sodium stannate solution) of precursor solution (i.e. silver ammino solution) and tin oxide is fully mixed
Close, the silver powder of Surface coating nano tin dioxide presoma prepared using fabricated in situ liquid phase reduction,
Then by the heat treatment such as drying and calcining so that tin oxide presoma is changed into the nanoscale powder of tin oxide
End, and forming core is grown in silver powder surface relevant position, so that nanoscale silver powder particles are successfully coated, from
And the purpose that nanoscale is combined-converts is reached, and improve Ag and SnO2Wellability.
Specifically, Fig. 1, Ag-SnO of the present invention please be refer to2The preparation method of contact material is main
Comprise the following steps：
(1) certain density reductant solution, silver ammino solution and sodium stannate solution are prepared respectively；
(2) above-mentioned silver ammino solution is mixed by a certain percentage with above-mentioned sodium stannate solution, is mixed with constituting one
Liquid is closed, acetic acid is added dropwise in the mixed liquor, adjust pH value in the mixed liquor, Ag is contained to be formed+'s
Sn(OH)4Colloidal sol or solution；
(3) reductant solution is added dropwise to the Sn (OH) of gained in step (2)4In colloidal sol, constant temperature is stirred
Mix or ultrasonic wave added reaction, remove supernatant liquor after standing, and cleaning, dry, collect after cooling and obtain
Powder；
(4) powder for obtaining will be collected in step (3) to be heat-treated under non-reducing atmosphere, is prepared
Obtain Ag-SnO2Composite granule.
Wherein above-mentioned reducing agent may be selected from formaldehyde, glyoxal, ethylenediamine, glucose, sodium potassium tartrate tetrahydrate,
One or more in sodium citrate, hydrazine hydrate, vitamin C, sodium borohydride or ascorbic acid.It is described
The concentration of reductant solution, the concentration containing silver concentration, sodium stannate solution of silver ammino solution are respectively：
10~2000ppm, 10~2000ppm, 10~2000ppm.
The mixed proportion of silver ammino solution and sodium stannate solution described in above-mentioned steps (2) is with the silver-colored ammonia
Silver in solution: the mass ratio of the tin ash in the sodium stannate solution is calculated as 4~20:1, adjust pH value
It is 0.5~11.
Reaction temperature described in above-mentioned steps (3) is 10~40 DEG C, and the time is 1~24h.
The non-reducing atmosphere includes inert atmosphere or oxidizing atmosphere.The oxidizing atmosphere is oxygen or air
Or other oxygen-containing atmospheres.The inert atmosphere includes nitrogen and rare gas.The rare gas can be used
At least one in argon gas, helium, neon.
The heat treatment process can be calcined in the range of 1~12h at 150~800 DEG C and select.
Set according to above-mentioned every scope and matched, the silver-metallic oxide electrical contact material can be made
The mass percent of silver is up to 86~99.5% in material.
With reference to the above, the present invention further discloses following several specific embodiments：
Embodiment 1
(1) respectively compound concentration be the hydrazine hydrate solution of 10ppm, the silver ammino solution of 50ppm and
The sodium stannate solution of 1000ppm；
(2) by the mixed proportion of silver ammino solution and sodium stannate solution with silver: tin ash is calculated as 4：1,
To constitute mixed liquor, acetic acid is added dropwise in the mixed liquor, is 3.5 for adjusting the pH value of the mixed liquor,
Contain Ag to be formed+Sn (OH)4Colloidal sol；
(3) hydrazine hydrate solution is added dropwise to the Sn (OH) of gained in step (2)4In colloidal sol, in 10 DEG C
Constant temperature stirring reaction 1h, removes supernatant liquor after standing, collected after cleaning, dry, cooling and obtain powder；
(4) powder for obtaining will be collected in step (3) in a nitrogen atmosphere in being calcined 5h at 300 DEG C,
Prepare Ag-SnO2Composite granule.
Embodiment 2
(1) respectively compound concentration be the ascorbic acid solution of 200ppm, the silver ammino solution of 10ppm and
The sodium stannate solution of 10ppm；
(2) by the mixed proportion of above-mentioned silver ammino solution and sodium stannate solution with silver: tin ash is calculated as
10:1, to constitute mixed liquor, acetic acid is added dropwise in the mixed liquor, be for adjusting the mixed liquor pH value
0.5, contain Ag to be formed+Sn (OH)4Colloidal sol；
(3) ascorbic acid solution is added dropwise in the colloidal sols of Sn (OH) 4 of gained in step (2), in
25 DEG C of constant temperature stirring reaction 2h, remove supernatant liquor after standing, collected after cleaning, dry, cooling and obtained
Powder；
(4) powder for obtaining will be collected in step (3) in air atmosphere in being calcined 12h at 150 DEG C,
Prepare Ag-SnO2Composite granule.
Embodiment 3
(1) respectively compound concentration be the ascorbic acid solution of 100ppm, the silver ammino solution of 100ppm and
The sodium stannate solution of 100ppm；
(2) by the mixed proportion of silver ammino solution and sodium stannate solution with silver: tin ash is calculated as 7.3:1,
To form a mixed liquor, acetic acid is added dropwise in the mixed liquor, is 2.0 for adjusting the mixed liquor pH value,
To form Sn (OH)4Colloidal sol；(it is noted here that the property of stannic hydroxide, with amphiprotic substance,
Sn(OH)2Based on alkalescence, Sn (OH)4Based on acidity, stannic hydroxide and stannous hydroxide meet highly basic,
Can react and dissolve, stannate and stannite are generated respectively.Due to the property of stannic hydroxide, pH
It is not stannic hydroxide colloidal sol when value is higher, so pH value here can be written as acidity, other
Embodiment is same.The result being currently understood that shows, colloidal sols of the pH between 0.5~1 preferably)
(3) ascorbic acid solution is added dropwise to the Sn (OH) of gained in step (2)4In colloidal sol, in 25 DEG C
Constant temperature stirring reaction 6h, removes supernatant liquor after standing, collected after cleaning, dry, cooling and obtain powder
Body；
(4) powder for obtaining will be collected in step (3) in a nitrogen atmosphere in being calcined 3h at 550 DEG C,
Prepare Ag-SnO2Composite granule.
Embodiment 4
(1) respectively compound concentration be the sodium citrate solution of 150ppm, the silver ammino solution of 500ppm and
The sodium stannate solution of 50ppm；
(2) by the mixed proportion of silver ammino solution and sodium stannate solution with silver: tin ash is calculated as 20:1,
To form a mixed liquor, acetic acid is added dropwise in the mixed liquor, is 11 for adjusting the mixed liquor pH value,
Contain Ag to be formed+Sn (OH)4Solution；
(3) sodium citrate solution is added dropwise to the Sn (OH) of gained in step (2)4In solution, in 40 DEG C
Constant temperature stirring reaction 2h, removes supernatant liquor after standing, collected after cleaning, dry, cooling and obtain powder
Body；
(4) powder for obtaining will be collected in step (3) under nitrogen and helium mix atmosphere in 700 DEG C
Lower roasting 5h, prepares Ag-SnO2Composite granule.
Embodiment 5
(1) compound concentration is vitamin c solution, the silver ammino solution of 600ppm of 2000ppm respectively
With the sodium stannate solution of 100ppm；
(2) by the mixed proportion of silver ammino solution and sodium stannate solution with silver: tin ash is calculated as 12：1,
To form a mixed liquor, acetic acid is added dropwise in the mixed liquor, is 8.5 for adjusting the mixed liquor pH value,
Contain Ag to be formed+Sn (OH)4Solution；
(3) vitamin c solution is added dropwise to the Sn (OH) of gained in step (2)4In solution, in
20 DEG C of constant temperature stirring reaction 12h, remove supernatant liquor after standing, collected after cleaning, dry, cooling
To powder；
(4) powder for obtaining will be collected in step (3) in a nitrogen atmosphere in being calcined 6h at 450 DEG C,
Prepare Ag-SnO2Composite granule.
Embodiment 6
(1) compound concentration is ascorbic acid solution, the silver ammino solution of 2000ppm of 500ppm respectively
With the sodium stannate solution of 2000ppm；
(2) by the mixed proportion of silver ammino solution and sodium stannate solution with silver: tin ash is calculated as 15:1,
To constitute a mixed liquor, acetic acid is added dropwise in the mixed liquor, is 5.5 for adjusting the mixed liquor pH value,
Formed and contain Ag+Sn (OH)4Colloidal sol；
(3) ascorbic acid solution is added dropwise to the Sn (OH) of gained in step (2)4In colloidal sol, in 25 DEG C
Constant temperature stirring reaction 20h, removes supernatant liquor after standing, collected after cleaning, dry, cooling and obtain powder
Body；
(4) powder for obtaining will be collected in step (3) under nitrogen and argon gas mixed atmosphere in 800 DEG C
Lower roasting 1h, prepares Ag-SnO2Composite granule.
Embodiment 7
(1) compound concentration is glucose solution, the silver ammino solution of 1200ppm of 1500ppm respectively
With the sodium stannate solution of 1000ppm；
(2) by the mixed proportion of silver ammino solution and sodium stannate solution with silver: tin ash is calculated as 6：1,
To form a mixed liquor, acetic acid is added dropwise in the mixed liquor, is 3.5 for adjusting the mixed liquor pH value,
Contain Ag to be formed+Sn (OH)4Colloidal sol；
(3) glucose solution is added dropwise to the Sn (OH) of gained in step (2)4In colloidal sol, in 10 DEG C
Constant temperature stirring reaction 24h, removes supernatant liquor after standing, collected after cleaning, dry, cooling and obtain powder
Body；
(4) powder for obtaining will be collected in step (3) in a nitrogen atmosphere in being calcined 4h at 600 DEG C,
Prepare Ag-SnO2Composite granule.
Fig. 2,3,4 please be refer to, a kind of silver-tin contact material of the present invention is mainly included
Ag particles and SnO2Particle, the wherein SnO2Particle is uniformly coated on Ag particle surfaces, to obtain
Uniform Ag-SnO2Composite granule.And it is coated on the circumgranular SnO of Ag2In bar-shaped and graininess.
The SnO2Particles coat is 10%~100%, preferably 90% in the clad ratio of Ag particle surfaces
More than.
Described Ag, SnO2And it is coated with SnO2Ag particles be nano-grade size, nano SnO2
Particle diameter up to about 5-100nm, be preferably about 50nm.
The optimal components ratio of wherein described silver-tin contact material is 88.10%, Sn for the content of Ag
Content for 9.37%, O content be 2.53%.
The mass percent of silver is 86~99.5% in the silver-tin contact material.
In the silver-tin contact material, SnO2Content be 0.5%~14%.General SnO2
Content be 12%.
The Ag-SnO that the present invention is made by method made above2Composite granule product has following spy
Point：
Please refer to Fig. 2 and Fig. 3, Fig. 2 are Ag-SnO that preparation method of the present invention is made2Product
ESEM (SEM) figure, Fig. 3 is energy spectrum analysis (EDS) figure in Fig. 2, so be can be seen that
It is of the invention to have coated SnO2Ag particle size uniformities, and nanoscale is, wherein to SEM
Square region carries out energy spectrum analysis in image, and when total amount is Unit 100, optimal components ratio is Ag elements
Content for 88.10%, Sn elements content for 9.37%, O constituent contents be 2.53%, you can obtain
The Ag-SnO of higher proportion2Material.
Fig. 4 please be refer to, it is the Ag-SnO that preparation method of the present invention is made2The transmission electron microscope of product
(TEM) figure, XRD proves argentiferous and tin ash two-phase simultaneously, and TEM is as a result, in fig. 4
Dark particulate material is Ag simple substance, SnO2It is distributed in around Ag particles in bar-shaped and graininess,
And be nano-grade size.
Above-mentioned Ag-SnO2Material can draw through arcing experiment, of the invention to carry out contrast and obtain with existing
Know, Ag-SnO of the invention2The high-quality characteristic that material has, as shown in Fig. 5 A, Fig. 5 B, figure
5A is existing Ag-SnO2The schematic diagram of sample arcing energy, illustrated in Figure 1 where it can be seen that, existing AgSnO2
Sample increases with action frequency, and arcing energy is in rising trend；And Fig. 5 B are Ag-SnO of the invention2
In the effect diagram of sample arcing energy, illustrated in Figure 1 where it can be seen that, AgSnO of the invention2Sample is servo-actuated
Making number of times increases arcing energy without significant change, and 20,000 average arcing energies are less than above-mentioned existing
AgSnO2The half of sample.
Please referring also to Fig. 6 A, Fig. 6 B again, wherein Fig. 6 A are existing Ag-SnO2Sample opens combustion
The effect diagram of arc time, it shows existing Ag-SnO2Sample increases with action frequency, opens
Arc time is in increase trend；And Fig. 6 B are Ag-SnO of the invention2Sample opens the effect of arc time
Fruit schematic diagram, wherein showing AgSnO of the invention2Sample increases with action frequency, when opening arcing
Between without significant change, and 20,000 average arc times are significantly lower than existing AgSnO2 samples.
Can so draw, the Ag-SnO drawn by preparation method of the present invention2For preferably electricity connects
Material is touched, its properties of product is more preferably.
The present invention is due to Ag-SnO2SnO in contact material2Particle reaches nanoscale, therefore has
Strong dispersion-strengthened effect, significantly increases the intensity and hardness of silver matrix material.Further, since nanometer
Particle has unique small-size effect, it is contemplated that will make the processing characteristics of contact material, electric conductivity,
Electric erosion resistance energy and resistance fusion welding can be than micron Ag-SnO2Contact material is significantly increased.Ag-SnO2
Material is Ag bases, SnO2Particle is the diffusion-type metal-base composites of hardening constituent.Due to most of feelings
Under condition, SnO2Particle size is 0.5-1 μm, and particle enhancing exists simultaneously with dispersion-strengthened action mechanism,
And particle is more tiny, volume fraction is higher, and particle is better to the enhancing effect of composite, material it is strong
Degree is higher.
The present invention is obtained in one layer of nano SnO of silver powder coated with uniform with fabricated in situ liquid phase reduction2
Obtain uniform Ag-SnO2Composite granule, reduces SnO2Granularity, improve SnO2With Ag powder
Wellability, improve in its processing characteristics and performance, and composite granule as slider material Ag with
SnO2Ratio easy-regulating.
In sum, the present invention uses in-situ synthesis technique, with silver ammino solution, Na2SnO3For
Initiation material, both at alkaline matter, uniformly can mix to constitute mixed liquor in aqueous, lead to
The mixed liquor pH value is overregulated, silver ion and Sn (OH) is realized4Colloidal sol it is dispersed,
Sn(OH)4Acted on by reducing agent in colloidal sol and obtain silver powder, such silver powder surface cleaning, with bigger
Surface-active, and silver powder granularity is smaller, with bigger specific surface area, makes Sn (OH)4Particle can
It is effectively adsorbed in silver powder surface and is coated with it and mixes.
In addition, the presoma of silver powder and addition phase is generated when in-situ synthesis of the invention react simultaneously
Sn(OH)4Two kinds of precipitations, the precipitation is by the heat treatment such as drying and calcining so that tin oxide presoma changes
It is the nano-scale powders of tin oxide, and forming core is grown in silver powder surface relevant position, so as to successfully coats
Nanoscale silver powder particles, the purpose for being combined-converting so as to reach nanoscale, and improve Ag and SnO2
Wellability.The impurities of materials content prepared by the method is low, wherein Bi, Sb, As, Pb content
No more than 0.003%, total impurities content is not more than 0.1%.
The present invention can reduce SnO by the above method simultaneously2Granularity, improve SnO2With Ag powder
Wellability, in one layer of nano SnO of silver powder coated with uniform2Particle obtains uniform Ag-SnO2It is compound
Powder, and make Ag and SnO in composite granule2Ratio easy-regulating, improves its processing as slider material
Performance and performance.The invention enables particle refinement, the sintering character of material is improved, solve tradition
The SnO that powder metallurgical technique is present2With the interface problem of Ag, and with preparation process is simple, low cost,
The advantages of preparation condition is easily controllable, synthesis cycle is short, properties of product are good.
Although disclosing the present invention with reference to above example, but it is not limited to the present invention, any
Those of ordinary skill in the art, without departing from the spirit and scope of the present invention, can do some
Perhaps change and retouching, therefore protection scope of the present invention should be with what the claim enclosed was defined
It is accurate.
Claims (18)
1. a kind of preparation method of silver-tin contact material, it is characterised in that the preparation method bag
Include following steps：
(1) certain density reductant solution, silver ammino solution and sodium stannate solution are prepared respectively；
(2) silver ammino solution is mixed by a certain percentage with the sodium stannate solution, to constitute mixed liquor,
Acetic acid is added dropwise in the mixed liquor, the pH value in the mixed liquor is adjusted, Ag is contained to be formed+Sn (OH)4
Colloidal sol or solution；
(3) reductant solution is added dropwise to the Sn (OH) of gained in step (2)4In colloidal sol or solution,
Constant temperature is stirred or ultrasonic wave added reaction, is received after supernatant liquor, and cleaning, dry, cooling are removed after standing
Collection obtains powder；
(4) powder for obtaining will be collected in step (3) to be heat-treated under non-reducing atmosphere, is prepared
Obtain Ag-SnO2Composite granule.
2. the preparation method of silver-tin contact material according to claim 1, its feature exists
In, the reducing agent be formaldehyde, glyoxal, ethylenediamine, glucose, sodium potassium tartrate tetrahydrate, sodium citrate,
One or more in hydrazine hydrate, vitamin C, sodium borohydride or ascorbic acid.
3. the preparation method of silver-tin contact material according to claim 1, its feature exists
In the concentration of the reductant solution, the difference of the concentration containing silver concentration, sodium stannate solution of silver ammino solution
For：10~2000ppm, 10~2000ppm, 10~2000ppm.
4. the preparation method of silver-tin contact material according to claim 1, its feature exists
In the mixed proportion of silver ammino solution and sodium stannate solution described in step (2) is with the silver ammino solution
Silver: the mass ratio of the tin ash in the sodium stannate solution is calculated as 4~20:1, adjusting pH value is
0.5~11.
5. the preparation method of silver-tin contact material according to claim 1, its feature exists
In the reaction temperature described in step (3) is 10~40 DEG C, and the time is 1~24h.
6. the preparation method of silver-tin contact material according to claim 1, its feature exists
In the non-reducing atmosphere includes inert atmosphere or oxidizing atmosphere.
7. the preparation method of silver-tin contact material according to claim 6, its feature exists
In the oxidizing atmosphere is oxygen or air.
8. the preparation method of silver-tin contact material according to claim 6, its feature exists
In the inert atmosphere includes nitrogen and rare gas.
9. the preparation method of silver-tin contact material according to claim 8, its feature exists
In the rare gas is at least one in argon gas, helium, neon.
10. the preparation method of silver-tin contact material according to claim 1, its feature
It is that described heat treatment process is 150~800 DEG C of 1~12h of roasting.
The preparation method of 11. silver-tin contact materials according to claim 1, its feature
It is that the mass percent of silver is 86~99.5% in the silver-tin contact material.
A kind of 12. silver-tin contact materials as described in claim 1-11 wherein at least one
Preparation method and the silver-tin contact material that is made.
A kind of 13. silver-tin contact materials, wherein the silver-tin contact material include Ag
Particle and SnO2Particle, the wherein SnO2Particle is uniformly coated on Ag particle surfaces, to obtain
Even Ag-SnO2Composite granule.
14. silver-tin contact materials as claimed in claim 13, wherein being coated on Ag particles
The SnO of surrounding2In bar-shaped and graininess.
15. silver-tin contact materials as claimed in claim 13, wherein each be coated with SnO2
Ag particle size uniformities.
16. silver-tin contact materials as claimed in claim 15, wherein the SnO2To receive
It is meter-sized.
17. silver-tin contact materials as claimed in claim 13, the wherein SnO2Particle bag
The clad ratio for overlaying on Ag particle surfaces is 10%~100%.
18. silver-tin contact materials as claimed in claim 13, wherein in silver-tin electricity
In contact material, SnO2Content be 0.5%~14%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510977375.8A CN106903325B (en) | 2015-12-23 | 2015-12-23 | Preparation method of silver-tin oxide electric contact material and electric contact material prepared by same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510977375.8A CN106903325B (en) | 2015-12-23 | 2015-12-23 | Preparation method of silver-tin oxide electric contact material and electric contact material prepared by same |
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| CN109128212A (en) * | 2018-08-16 | 2019-01-04 | 西安工程大学 | A kind of preparation method of silver nickel zinc oxide alloy as electric contact material |
| CN109128213A (en) * | 2018-08-16 | 2019-01-04 | 西安工程大学 | A kind of preparation method of silver oxidation of coal tin contact alloy |
| CN112609247A (en) * | 2020-11-06 | 2021-04-06 | 东北大学 | Method for preparing silver tin oxide electric contact material by electrostatic spinning method |
| CN114082978A (en) * | 2021-11-29 | 2022-02-25 | 大连大学 | Nano AgSn-SnO2Preparation method of needle-shaped composite powder |
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| CN109128212A (en) * | 2018-08-16 | 2019-01-04 | 西安工程大学 | A kind of preparation method of silver nickel zinc oxide alloy as electric contact material |
| CN109128213A (en) * | 2018-08-16 | 2019-01-04 | 西安工程大学 | A kind of preparation method of silver oxidation of coal tin contact alloy |
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| CN112609247A (en) * | 2020-11-06 | 2021-04-06 | 东北大学 | Method for preparing silver tin oxide electric contact material by electrostatic spinning method |
| CN114082978A (en) * | 2021-11-29 | 2022-02-25 | 大连大学 | Nano AgSn-SnO2Preparation method of needle-shaped composite powder |
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