CN106636723B - One kind is with La1‑xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase - Google Patents
One kind is with La1‑xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- C01G15/00—Compounds of gallium, indium or thallium
- C01G15/006—Compounds containing, besides gallium, indium, or thallium, two or more other elements, with the exception of oxygen or hydrogen
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses one kind with La1‑xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, belongs to field of compound material.This method includes：La is prepared using hydro-thermal method1‑xSrxInO3System conductivity ceramics microballoon, and silver ammino solution and organic complexing agent are used to La in water-heat process1‑xSrxInO3Microballoon progress one step of hydro-thermal is silver-carrying modified, carries silver La1‑xSrxInO3Microspherulite diameter is distributed between 5~50 μm；By blender by above-mentioned load silver La1‑ xSrxInO3Microballoon is uniformly mixed with metal Ag powder, wherein carrying silver La1‑xSrxInO3The mass ratio of microballoon is 10%~24%；Powder after mixing is used into powder metallurgic method, the process procedures such as isostatic pressed base, sintering, multiple pressure, resintering, hot extrusion drawing shaping is passed sequentially through, prepares environment-friendly type Ag/La1‑xSrxInO3Electric contact composite material.The present invention prepares the silver-carrying modified La in surface using hydro-thermal one-step method1‑xSrxInO3Microballoon, by regulating and controlling its granularity, form factor, improving Ag/La with the wetting of Ag matrixes and its distribution in Ag matrixes, synthesis1‑xSrxInO3Anti electric arc corrosion performance, reliability and the service life of contact material.
Description
Technical field
It is one kind with La specifically the present invention relates to a kind of preparation method of novel environment friendly electric contact composite material1- xSrxInO3Microballoon is the Ag/La of enhancing phase1-xSrxInO3The preparation method of electric contact composite material.
Background technology
Contact material is the critical material for preparing power switch, breaker, relay and all kinds of electrical and electronic components,
The main effect for being responsible for on-off and load current, is widely used in household low pressure electric appliance, automobile, instrument and meter, industry
The fields such as automation, information electronics and aerospace, it is closely bound up with national life and industrial development.Inherently see, Ag bases
Electric contact composite material can be divided into two big function ingredients：First, basis material Ag, ensure the high conductivity of contact material；Second,
Strengthen phase material, determine the anti electric arc corrosion ability and service life of contact material.
CdO because it is widely used as with excellent electric arc breaking capacity the enhancing phase of Ag base electric contact composite materials,
Ag/CdO was once known as " omnipotent contact material ".But Cd elements are poisonous, when Ag/CdO contact materials resist arc erosion
Cd elements can volatilize, containing cancer caused by the poisonous contact materials of Cd is occurred frequently and whole body ostalgia case has caused extensive concern.With
《Limitation uses some harmful substances in electronic electric equipment》(RoHS instructions) and《Waste and old electric/electronic device》(WEEE refers to
Make) promulgation and execution, European and American developed countries progressively disable Ag/CdO, and Devoting Major Efforts To Developing is formed without Cd environmental protection contact materials
Skill error, though China has introduced the Ag/SnO of environmental protection2Contact material, but still have more than half electrical and electronic components at present
The Ag/CdO materials used are difficult to be substituted, and research and development highly reliable, long-life, anti electric arc corrosion ability are strong to be made electrical contact with without Cd environmental protection
Material seems extremely urgent.
The content of the invention
It is an object of the invention to provide a kind of new A g/La1-xSrxInO3The preparation method of electric contact composite material.
With La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, is specifically comprised the following steps：
(1) the silver-carrying modified La in surface is prepared using hydro-thermal one-step method1-xSrxInO3Microballoon；
(2) by blender by above-mentioned load silver La1-xSrxInO3Microballoon is uniformly mixed with metal Ag powder, wherein carrying silver La1- xSrxInO3The mass ratio of microballoon is 10%~24%；
(3) powder after mixing is used into powder metallurgic method, passes sequentially through isostatic pressed base, sintering, press again, is multiple
Burn, hot extrusion drawing shaping process procedure, prepare Ag/La1-xSrxInO3Electric contact composite material.
Preferably, hydro-thermal one-step method prepares the silver-carrying modified La in surface employed in step (1)1-xSrxInO3Microballoon
Method is：Stoichiometrically weigh La (NO3)3、Sr(NO3)2、InCl3·4H2O, mixed powder are simultaneously dissolved in deionized water；Filling
Divide under conditions of stirring, add appropriate citric acid and make organic complexing agent, adjust pH with ammonium hydroxide and form colloidal sol, with water-bath or oil bath
Constant temperature is controlled, after still aging a period of time, the silver ammino solution now matched somebody with somebody is slowly added in above-mentioned colloidal sol under stirring, waits to mix
Close liquid it is uniform after, add enough reducing agents, continue after 10~90min of stirring obtained precursor solution being added to 50~
In the hydrothermal reaction kettle of 200ml, compactedness is 50%~80%, is placed in 10~60h of reaction at 120~250 DEG C, takes out centrifugation
Cleaning, drying；Powder after drying is calcined, 600~1000 DEG C of sintering temperature, keep the temperature 3~18h, furnace cooling obtains
La1-xSrxInO3Microballoon.
Wherein, La1-xSrxInO3In conductivity ceramics microballoon the scope of X be 0.05~0.3, complexing agent Citric Acid Dosage with it is molten
The ratio between total amount of metal ion N/J (molar ratio) is 0.5 in glue:1~3:1, the holding constant temperature in ageing process is 45~120
DEG C, the still aging time is 30~600min, controls the load silver La finally obtained1-xSrxInO3Microspherulite diameter is distributed in 5~50 μ
Between m.
Preferably, described in step (2) in blending processes of powders, silver La is carried1-xSrxInO3Microspherulite diameter scope is 5~50 μm,
The purity of silver powder is 99.99%, and particle size range is 20~100 μm, mixes 2~8h of the powder time；
Preferably, the pressure range of isostatic pressed base described in step (3) is 30~300MPa；
Preferably, sintering process described in step (3), refers to sinter in the case where argon gas atmosphere is protected, sintering temperature 720~
950 DEG C, 3~12h of soaking time；
It is that hot pressing is carried out at 300~800 DEG C preferably, pressing technique again described in step (3), pressure range 500~
1000MPa, 2~30min of dwell time；
Preferably, resintering technique described in step (3), refers to sinter again in the case where argon gas is protected, sintering temperature 720~
950 DEG C, 3~12h of sintering time；
Preferably, described in step (3) in hot extrusion drawing moulding process, mold preheating temperature is 350~860 DEG C,
Blank temperature is 500~800 DEG C, and extrusion ratio scope is 16~225, and extrusion speed is 10~60m/min.
With poisonous Ag/CdO materials or common Ag/SnO2Material is compared, the beneficial effects of the invention are as follows：
New A g/La1-xSrxInO3Electric contact composite material is free of harmful element, belongs to environment-friendly type electrical contact
Material, meets RoHS instructions and WEEE instructions.
Microspheroidal La is prepared by hydro-thermal method1-xSrxInO3Enhancing phase of the conductivity ceramics as Ag base electrical contact materials, foundation
" molten bath viscosity " theoretical mechanism of Ag base electrical contact material anti electric arc corrosions, passes through Reasonable Regulation And Control La1-xSrxInO3Microballoon is in Ag bases
Granularity, grading and form factor in body, avoid occur electric arc when contact material surface molten bath because of the excessive generation melting welding of viscosity
Or the too low generation flowing of viscosity, splash loss.Comprehensive mechanical strength, wearability and the anti electric arc corrosion energy for improving contact material
Power, while there is no the problem of processing, difficult forming.
La1-xSrxInO3Belong to the high-performance conductive ceramics of perovskite structure, collect metal electrical properties and ceramic structure characteristic
.Test result indicates that during equal conditions, Ag/La1-xSrxInO3Material transfer indfficiency under material arc corrodes is less than
Ag/CdO, electrical contact performance are better than common no Cd contact materials, such as Ag/SnO2、Ag/ZnO。
The present invention is by hydro-thermal one-step method to La1-xSrxInO3Mutually progress surface is silver-carrying modified for microballoon enhancing, enhances
La1-xSrxInO3Wetability between microballoon and Ag matrixes；La is optimized by hot extrusion drawing process1-xSrxInO3Microballoon is in Ag
Distribution in matrix.Further improve contact material strengthen after by arc erosion mutually separated with silver matrix, segregation the problem of,
Substantially increase Ag/La1-xSrxInO3The reliability and service life of contact material.
The present invention is by La1-xSrxInO3The granularity of microballoon enhancing phase, form factor regulation and control, mating surface are silver-carrying modified
Technology, can be under the requirement of equal electrical contact performance, the volume of increase enhancing phase, it is however generally that, compared to common Ag/SnO2Material
Material, Ag/La1-xSrxCoO3Silver 5%~10% can be economized on.
Brief description of the drawings
Fig. 1 is La prepared by hydro-thermal method1-xSrxInO3Microballoon；
Fig. 2 is Ag/La1-xSrxInO3Contact material metallograph；
Fig. 3 is arc time spectral line of the different contact materials in 20000 break-make cyclic processes, wherein (a) Ag/
SnO2(average arc time 18.69ms), (b) Ag/La1-xSrxInO3(average arc time 14.57ms).
Embodiment
The present invention is further described by the following examples.
The present invention provides one kind with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, is specifically wrapped
Include following steps：
(1) the silver-carrying modified La in surface is prepared using hydro-thermal one-step method1-xSrxInO3Microballoon.
Stoichiometrically weigh La (NO3)3、Sr(NO3)2、InCl3·4H2O, mixed powder are simultaneously dissolved in deionized water；Filling
Divide under conditions of stirring, add appropriate citric acid and make organic complexing agent, adjust pH with ammonium hydroxide and form colloidal sol, with water-bath or oil bath
Constant temperature is controlled, after still aging a period of time, the silver ammino solution now matched somebody with somebody is slowly added in above-mentioned colloidal sol under stirring, waits to mix
After conjunction liquid is uniform, enough reducing agents such as formaldehyde, glucose, ascorbic acid etc. are added, will be obtained after continuing 10~90 min of stirring
Precursor solution be added in the hydrothermal reaction kettle of 50~200ml, compactedness be 50%~80%, be placed at 120~250 DEG C
10~60h is reacted, takes out eccentric cleaning, drying；Powder after drying is calcined, 600~1000 DEG C of sintering temperature, kept the temperature
3~18h, furnace cooling obtain La1-xSrxInO3Microballoon.
Wherein, La1-xSrxInO3In conductivity ceramics microballoon the scope of X be 0.05~0.3, complexing agent Citric Acid Dosage with it is molten
The ratio between total amount of metal ion N/J is 0.5 in glue:1~3:1, the holding constant temperature in ageing process is 45~120 DEG C, is stood old
The change time is 30~600min, controls the load silver La finally obtained1-xSrxInO3Microspherulite diameter is distributed between 5~50 μm.
(2) by blender by above-mentioned load silver La1-xSrxInO3Microballoon is uniformly mixed with metal Ag powder, carries silver La1- xSrxInO3Microspherulite diameter scope is 5~50 μm；The purity of silver powder is 99.99%, and particle size range is 20~100 μm；The mixed powder time
2~8h；Silver La is carried in the mixture1-xSrxInO3The mass ratio of microballoon is 10%~24%.
(3) powder after mixing is used into powder metallurgic method, passes sequentially through isostatic pressed base, sintering, press again, is multiple
Burn, after hot extrusion drawing shaping process procedure, prepare Ag/La1-xSrxInO3Electric contact composite material.
In each process procedure, design parameter is as follows：
The pressure range of isostatic pressed base is 30~300MPa；
Sintering process, refers to sinter in the case where argon gas atmosphere is protected, 720~950 DEG C of sintering temperature, 3~12h of soaking time；
Technique is pressed again, is that hot pressing is carried out at 300~800 DEG C, 500~1000MPa of pressure range, the dwell time 2~
30min；
Resintering technique, refers to sinter again in the case where argon gas is protected, 720~950 DEG C of sintering temperature, 3~12h of sintering time；
In hot extrusion drawing moulding process, mold preheating temperature is 350~860 DEG C, and blank temperature is 500~800 DEG C, is squeezed
Pressure ratio scope is 16~225, and extrusion speed is 10~60m/min.
It is specifically described below by embodiment 1~6 pair of technique and effect of the invention.Processing step as it was previously stated,
Specific data in each embodiment see the table below：
Embodiment 1~6 can prepare the Ag/La of the present invention1-xSrxInO3Electric contact composite material.Below with embodiment 2
Exemplified by, the characterization and performance of its material are illustrated.
The silver-carrying modified La in surface is prepared using hydro-thermal one-step method in step (1)1-xSrxInO3Microballoon, its SEM photograph is as schemed
Shown in 1.Powder metallurgic method is used in step (3), passes sequentially through isostatic pressed base, sintering, pressure, resintering, hot extrusion are drawn into again
The process procedures such as type, the Ag/La prepared1-xSrxInO3Electric contact composite material, its metallograph are as shown in Figure 2.
In the contact material course of work, break-make circulation each time all inevitably produces electricity in material interpolar
Arc, electric arc can produce erosion damage to material, so as to influence the job stability and service life of contact material, electric arc is lasting
Time it is longer, the reliability of contact material is poorer, and service life is shorter.Therefore, the arc time is to influence contact material
The important indicator of dynamic electrical contact performance.Under equal conditions, by Ag/SnO2Material and Ag/La1-xSrxInO3Material carries out
The electrical endurance test of 20000 break-make circulations, the arc time spectral line of measure are as shown in Figure 3.Test result indicates that 20000
During the electrical endurance test of secondary break-make circulation, with common no Cd contact materials Ag/SnO2Compare, it is of the present invention new
Type Ag/La1-xSrxInO3The contact material arc time stablizes, and the average arc time is short, and the arc erosion that material is subject to is small, table
The dynamic electrical contact performance of bright material during the work time be improved significantly, electric life is improved.
Finally, it should also be noted that it is listed above be only the present invention some embodiments.Obviously, it is of the invention
Above example is not limited to, there can also be many deformations.Those skilled in the art can directly lead from present disclosure
All deformations for going out or associating, are considered as protection scope of the present invention.
Claims (7)
1. one kind is with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, it is characterised in that specific bag
Include following steps：
（1）The silver-carrying modified La in surface is prepared using hydro-thermal one-step method1-xSrxInO3Microballoon, specific method are as follows：
Stoichiometrically weigh La (NO3)3、Sr(NO3)2、InCl3•4H2O, mixed powder are simultaneously dissolved in deionized water；Fully stirring
Under conditions of mixing, add appropriate citric acid and make organic complexing agent, adjust pH with ammonium hydroxide and form colloidal sol, controlled with water-bath or oil bath
The silver ammino solution now matched somebody with somebody, after still aging a period of time, is slowly added in above-mentioned colloidal sol, liquid to be mixed by constant temperature under stirring
After uniformly, enough reducing agents are added, continue that obtained precursor solution is added to 50 ~ 200 ml's after 10 ~ 90 min of stirring
In hydrothermal reaction kettle, compactedness is 50% ~ 80%, is placed in 10 ~ 60 h of reaction at 120 ~ 250 DEG C, takes out eccentric cleaning, drying；Will
Powder after drying is calcined, 600 ~ 1000 DEG C of sintering temperature, keeps the temperature 3~18 h, and furnace cooling obtains La1-xSrxInO3It is micro-
Ball；
Wherein, La1-xSrxInO3The scope of X is 0.05~0.3 in conductivity ceramics microballoon, in complexing agent Citric Acid Dosage and colloidal sol
The ratio between total amount of metal ion N/J is 0.5:1~3:1, the holding constant temperature in ageing process is 45~120 DEG C, the still aging time
For 30 ~ 600min, the load silver La finally obtained is controlled1-xSrxInO3Microspherulite diameter is distributed between 5 ~ 50 μm；
（2）By blender by above-mentioned load silver La1-xSrxInO3Microballoon is uniformly mixed with metal Ag powder, wherein carrying silver La1- xSrxInO3The mass ratio of microballoon is 10% ~ 24%；
（3）Powder after mixing is used into powder metallurgic method, passes sequentially through isostatic pressed base, sintering, multiple pressure, resintering, heat
After extruding drawing shaping process procedure, Ag/La is prepared1-xSrxInO3Electric contact composite material.
It is 2. according to claim 1 with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, its
It is characterized in that, step（2）Described in blending processes of powders, carry silver La1-xSrxInO3Microspherulite diameter scope be 5 ~ 50 μm, silver powder it is pure
Spend for 99.99%, particle size range is 20~100 μm, mixes 2~8h of the powder time.
It is 3. according to claim 1 with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, its
It is characterized in that, step（3）Described in the pressure range of isostatic pressed base be 30~300MPa.
It is 4. according to claim 1 with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, its
It is characterized in that, step（3）Described in sintering process, refer to argon gas atmosphere protect under sinter, 720~950 DEG C of sintering temperature, protect
Warm 3~12h of time.
It is 5. according to claim 1 with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, its
It is characterized in that, step（3）Described in press technique again, be that hot pressing is carried out at 300~800 DEG C, 500~1000MPa of pressure range,
2~30min of dwell time.
It is 6. according to claim 1 with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, its
It is characterized in that, step（3）Described in resintering technique, refer to argon gas protect under sinter again, 720~950 DEG C of sintering temperature, burn
Tie 3~12h of the time.
It is 7. according to claim 1 with La1-xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase, its
It is characterized in that, step（3）Described in hot extrusion drawing moulding process, mold preheating temperature is 350~860 DEG C, blank temperature
For 500~800 DEG C, extrusion ratio scope is 16~225, and extrusion speed is 10~60m/min.
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| CN102312150A (en) * | 2011-09-29 | 2012-01-11 | 浙江大学 | Preparation method of Ag / Ti3SiC2 electric contact composite material |
| CN102321838B (en) * | 2011-10-11 | 2013-02-27 | 浙江大学 | Method for preparing Ag/SnO2 composite material |
| CN102618773B (en) * | 2012-04-05 | 2013-06-19 | 浙江大学 | Method for preparing Ag/La1-xSrxCoO3 electric contact composite material |
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