CN110468295A - A kind of strong―binding interface type Ag/SnO2The preparation method of contact material - Google Patents
A kind of strong―binding interface type Ag/SnO2The preparation method of contact material Download PDFInfo
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- CN110468295A CN110468295A CN201910715907.9A CN201910715907A CN110468295A CN 110468295 A CN110468295 A CN 110468295A CN 201910715907 A CN201910715907 A CN 201910715907A CN 110468295 A CN110468295 A CN 110468295A
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- 239000000463 material Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011159 matrix material Substances 0.000 claims abstract description 26
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 239000004964 aerogel Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims description 62
- 239000000843 powder Substances 0.000 claims description 39
- 238000000498 ball milling Methods 0.000 claims description 28
- 238000007873 sieving Methods 0.000 claims description 20
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 16
- 229910001887 tin oxide Inorganic materials 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 150000001298 alcohols Chemical class 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000003643 water by type Substances 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000748 compression moulding Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 150000001805 chlorine compounds Chemical class 0.000 claims description 6
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical class O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 13
- 238000004220 aggregation Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 18
- 239000000956 alloy Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000010949 copper Substances 0.000 description 6
- 238000010891 electric arc Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 239000000306 component Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 150000002825 nitriles Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 229960004643 cupric oxide Drugs 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 102220469587 Voltage-dependent L-type calcium channel subunit beta-2_D60K_mutation Human genes 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 238000011010 flushing procedure Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
- C22C32/001—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
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to a kind of strong―binding interface type Ag/SnO2The preparation method of contact material belongs to contact material technical field.The present invention is modified integral material structure using aerogel composite, due to SnO2It is a kind of typical N-type wide bandgap semiconductor, in its composite inner, in aeroge skeleton particle, Lacking oxygen is more, the nanocrystalline form that is primarily present should be SnO, simultaneously in the SnO2 aeroge with high surface area and minimum crystallite dimension, surface atom accounts for the overwhelming majority, material is mainly made of surface, it is very big with common body differences in materials, the electronic structure of its skeleton particle is similar to the surface of body material, it is modified matrix by this material with excellent structural performance of aeroge, since aeroge is nanoporous three-dimensional net structure material made of a kind of colloidal particle as nanometer scale or the high-polymer molecule aggregation, the composite material being prepared effectively improves the performance between material between interface cohesion, further improve the bond strength of material.
Description
Technical field
The present invention relates to a kind of strong―binding interface type Ag/SnO2The preparation method of contact material, belongs to contact material
Technical field.
Background technique
Electrical contact is defined as to ensure the interface between electrical, electronic equipment the current carrying element for the purpose of circuit is continuous,
And the component comprising the interface.Contact material is switching control and load current electric appliance in electric power preparation and appliance circuit
The core component and critical material of (such as switch, starter, relay, instrument and meter) are mainly born on-off, are led
The effect of stream, isolation electric current.Its performance quality directly affects the reliability of electronic apparatus part, stability, accuracy and uses the longevity
Life.So contact material is both the heart and its heel of Achilles of electric equipment products.
In actual application, we have following performance requirement to ideal contact material:
(1) physical property: low resistivity is to guarantee good conductance, and low vapour pressure is to limit the metal steam steam packing after the starting the arc
Degree, the heat that high thermal conductivity conveniently generates electric arc or joule heat source are transported to contact base as early as possible and are distributed, high fusing point, boiling
Point decomposes latent heat and specific heat to reduce arcing trend, in addition, electron work functon wants high, to guarantee arcing voltage height.
(2) chemical property: contact material should have higher chemical stability, i.e. electrochemical bit wants high.In air
Not will form oxidation, carbonization, vulcanization and other be not easy conductive compound film layer, even if being formed should also be as being easy decomposition.
(3) electrical contact performance: being summarised as at 3 points, and low and stable contact resistance, resistance fusion welding is good, resistance to arc erosion.
(4) mechanical performance: suitable consistency and elasticity modulus.Lesser hardness can periodically increase contact in contact pressure one
Area reduces contact resistance, reduces contact fever, deadmelt tendency and moving contact spring；Higher hardness can reduce melting welding area,
Improve mechanical wear ability.It is also required that contact material is easy welding in room temperature, when high temperature, still keeps certain intensity, tough
Property etc..
Electricity, which connects, melts Materials so far there are many preparation method, and two classes is divided to be introduced below.One kind is industrial metaplasia
Prevailing technology in production common are four kinds: general powder metallurgic method, infiltration method, alloy inner oxidation method and powder pre-oxidation method；
Another kind of is the cutting edge technology of a small number of enterprises or research institution's research and development, such as the compacting of static pressure, ultrasonic wave, electric arc melting, ion note
Enter, react synthesis, repeat extruding and fibre strengthening etc. indirectly, is the hot spot studied at present.
Powder metallurgic method is widely used in preparing all kinds of contact materials, such as Ag/SnO2, Ag/ZnO, Ag/Ni, Ag/C etc..
Its technical process is that raw material silver powder and reinforced phase powder are carried out to ingredient, mixed powder, compression moulding, sintering in proportion, is then rolled
At plate or wire rod is squeezed into manufacture all kinds of electrical contact elements.The advantages of powder metallurgic method, is to be applicable in the electricity of any component
Contact material preparation, and can easily be accommodated materials microstructure structure, it eliminates in " poor metal oxide area ", while the work of powder metallurgic method
Skill is simple, at low cost, less investment, therefore is chiefly used in that volume is big, contact production of simple shape.The disadvantage is that prepared by powder metallurgic method
Hardness, the density of contact material are generally low compared with internal oxidation, and material porosity is high, and oxide particle is coarse, easily leads to and connects
Electric shock resistance is big, the problems such as temperature rise height.In addition, uneven if there is mixed powder in traditional handicraft, nanoparticle agglomerates etc. are lacked
It falls into, can also seriously affect the comprehensive performance of contact material.
Infiltration method is commonly used to prepare the contact material of the systems such as Cu/W, Cu/Cr, Ag/W, Cu/Mo, its main feature is that specially
For the preparation of refractory metal and low melting point metal pseudo-alloy contact material.Infiltration method is divided into two kinds, and one is first high temperature will
Refractory metal (W, Mo, Cr etc.) sinters skeleton into, then in low temperature or reducing atmosphere, makes the Ag dissolved or Cu by capillary
The effect of power penetrates among skeleton；After another kind is first low-temperature sintering part mixed powder, then low-melting-point metal is penetrated into, in turn
It is prepared into required composited contact material.
Alloy inner oxidation method is to prepare an important means of Ag/MeO electric contact composite material.It firstly the need of Ag and
Other metal components are smelted into alloy pig according to the ratio, then through rolling, punch forming, internal oxidition processing are finally carried out, due to Ag
It is not easy to be oxidized at high temperature, the Ag/MeO of silver with metal oxide composition is formed after base metal constituent element is fully oxidized
Composite material.
Alloy powder preoxidation greatly reduces the period of internal oxidition since the atomized alloy powder quickly solidified,
And oxide particle is evenly distributed tiny, the anti-melting welding of material, anti electric arc corrosion better performances.Each oxygen in material simultaneously
Compound particle is all connected with rich Ag, increases the Ag-Ag conductive channel density of material internal, reduces the resistivity of material.
But the consistency and mechanical and physical performance of the method resulting materials are high not as good as the contact material of internal oxidition preparation, process cycle,
It is also a kind of contact material preparation method that advantage and disadvantage are compromised relatively in terms of cost.
Ag base electrical contact material is using the material having a large capacity and a wide range the most in Electrical Contact Industry, and wherein Ag/CdO electrical contact accounts for
60% or more of all electrical contact products.In the environment-friendly type contact material system of substitution Ag/CdO, Ag/SnO2It is to be ground
The most one kind studied carefully, but SnO2There are some defects, such as SnO for the physical property of itself2Resistivity it is too big, be more than electrical contact
8 orders of magnitude of resistivity of material；SnO2The interface compatibility of particle and Ag are bad, are also easy to produce segregation；High with temperature rise,
The problems such as anti electric arc corrosion performance is poor.Researcher is using all multi-methods to Ag/SnO2Material is modified, and is achieved gratifying
Progress.And on the other hand, a part research starts to focus on new contact material system of exploring, especially Ag/ conduction and makes pottery
The research of porcelain contact material provides new thinking to the exploitation of environment-friendly type contact material.
Summary of the invention
The technical problems to be solved by the invention: it for the problem that current material contact resistance is poor, provides a kind of strong
The preparation method of interface cohesion type Ag/SnO2 contact material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) according to parts by weight, 45~50 parts of acetonitriles, 35~40 parts of ethyl orthosilicates, 3~5 parts of deionized waters and 6 are weighed respectively
~8 parts of propylene oxide are placed in conical flask, are stirred juxtaposition and are stood 1~2h at room temperature, and matrix liquid A is obtained；Again by weight
Number meter weighs 45~50 parts of acetonitriles, 3~5 parts of Copper dichloride dihydrates and 6~8 parts of deionized waters respectively and is placed in a beaker, stirs
Mixing juxtaposition stands 1~2h at room temperature, obtains matrix liquid B；
(2) according to parts by weight, 45~50 parts of dehydrated alcohols, 10~15 parts of acetums and 10~15 parts of metatitanic acid fourths are weighed respectively
Ester is placed in conical flask, is stirred to obtain modified complex liquid；By volume 1: 2: 2, by matrix liquid B and matrix liquid A and modification
Complex liquid is stirred to obtain mixed liquor, then in mass ratio 1: 5, and mixed liquor is added dropwise in propylene oxide, after being added dropwise to complete, receives
Collection is added dropwise complex liquid and is placed in insulation reaction, collects to obtain reaction sol solutions；
(3) according to parts by weight, 45~50 parts of dehydrated alcohols, 3~5 parts of stannic chlorides and 10~15 parts of propylene oxide are weighed respectively to set
In conical flask, be stirred juxtaposition and stand at room temperature, collect aged gel liquid and by aged gel liquid with react colloidal sol
Liquid is stirred and ultrasonic disperse, then stands aging at room temperature again, carrying out washing treatment, then in CO2Supercritical fluid drying dress
Set middle drying, after the completion of to be dried, collect dry aerogels and the heating and thermal insulation that heats up and react, standing is cooled to room temperature and ball milling,
Sieving, obtains composite tin oxide aerogel powder；
(4) silver powder and ball milling sieving are taken, sieving powder and in mass ratio 1: 8 is taken, by composite tin oxide aerogel powder and sieving
Powder, which is stirred, to be placed in high energy ball mill, ball milling, collects ball milling mixing powder and compression moulding, collects compacting blank simultaneously
It is placed in Muffle furnace, heating heating, heat preservation sintering, then the processing of multiple pressure, after secondary temperature elevation heating, heat preservation sintering, annealing, i.e.,
The strong―binding interface type Ag/SnO can be prepared into2Contact material.
The acetum concentration is mass fraction 1%.
The carrying out washing treatment is successively to be rinsed 3~5 times respectively with dehydrated alcohol and acetone.
The CO2Supercritical fluid drying device drying parameter is that control critical-temperature is 31~32 DEG C, pressure 7.0
~7.5MPa.
The mixed liquor drop rate is 0.1mL/s.
The mesh size is 70~75 μm.
The aged gel liquid is in mass ratio 1: 1 with sol solutions compositely proportional is reacted.
The multiple pressure processing pressure is 1250~1300MPa.
The secondary temperature elevation heats, heat preservation sintering is to be warming up to 655~680 DEG C by 5 DEG C/min, 3~4h of heat preservation sintering.
The high energy ball mill is preferably QM-3A type high energy ball mill.
The present invention is compared with other methods, and advantageous effects are:
(1) technical solution of the present invention uses cupric oxide doped composite titanium oxide/silica aerogel materials prepared by the present invention, system
Standby composite Nano tin oxide aeroge effectively improves the adhesion work of composite material, while material due to effective addition of copper oxide
The wettability of the adhesion work characterization material of material, this is because wet processes are by so-called adhesion work according to thermodynamic (al) analysis
It determining, adhesion work indicates function consumed by separation unit solid liquid interface, for measuring the bond strength of solid and liquid, adherency
Function is bigger, and solid liquid interface combination is more secured, and system is more stable, and simultaneous oxidation copper effectively changes the ingredient of reinforcement, solid to reduce
Light-liquid interfacial tension can be obviously improved wetability, make Ag/SnO2Interface becomes dissolution from mechanical bond and is combined with wetting, concurrently
The reciprocation of raw atom (molecule) level, thus the bond strength at interface can be made to be improved, simultaneous oxidation copper product adds
Add, can obviously inhibit SnO2The aggregation of particle at high temperature with grow up, and the nano SnO containing doped chemical2Particle dispersion distribution
Ag quite in, the viscosity of Ag under high temperature can be further increased, reduce Ag melting zone setting time substantially, textura epidermoidea is substantially
Degree refinement and homogenization, the probability that the textura epidermoidea uniformly refined forms contact surface particle significantly reduce, and breakdown weak points subtract
It is few, to facilitate the raising of alloy dieletric strength and anti electric arc corrosion performance；
(2) technical solution of the present invention is modified integral material structure using aerogel composite, due to SnO2It is a kind of
Typical N-type wide bandgap semiconductor, in its composite inner, aeroge skeleton particle, Lacking oxygen is more, nanocrystalline master
Existence form is wanted to should be SnO, while in the SnO2 aeroge with high surface area and minimum crystallite dimension, surface atom is accounted for
The overwhelming majority, material are mainly made of surface, very big with common body differences in materials, the electronic structure and body material of skeleton particle
The surface of material is similar, is modified matrix by this material with excellent structural performance of aeroge, since aeroge is a kind of
The nanoporous three-dimensional net structure material as made of colloidal particle or the high-polymer molecule aggregation of nanometer scale, is prepared
Composite material effectively improves the performance between material between interface cohesion, further improves the bond strength of material.
Specific embodiment
According to parts by weight, respectively weigh 45~50 parts of acetonitriles, 35~40 parts of ethyl orthosilicates, 3~5 parts of deionized waters and
6~8 parts of propylene oxide are placed in conical flask, are stirred juxtaposition and are stood 1~2h at room temperature, and matrix liquid A is obtained；Again by weight
Number meter weighs 45~50 parts of acetonitriles, 3~5 parts of Copper dichloride dihydrates and 6~8 parts of deionized waters respectively and is placed in a beaker, stirs
Mixing juxtaposition stands 1~2h at room temperature, obtains matrix liquid B；According to parts by weight, 45~50 parts of dehydrated alcohols, 10 are weighed respectively
~15 parts of 1% acetums of mass fraction and 10~15 parts of butyl titanates are placed in conical flask, are stirred modified compound
Liquid；By volume 1: 2: 2, matrix liquid B and matrix liquid A and modification complex liquid are stirred to obtain mixed liquor, then in mass ratio 1:
5, mixed liquor is added dropwise in propylene oxide, control drop rate is 0.1mL/s, after being added dropwise to complete, collects and complex liquid is added dropwise
It is placed in 25~30min of insulation reaction at 30~40 DEG C, collects to obtain reaction sol solutions；According to parts by weight, respectively weigh 45~
50 parts of dehydrated alcohols, 3~5 parts of stannic chlorides and 10~15 parts of propylene oxide are placed in conical flask, are stirred and are placed in room temperature
3~5h of lower standing collects aged gel liquid and in mass ratio 1: 1, aged gel liquid is stirred juxtaposition with sol solutions are reacted
10~15min of ultrasonic disperse under 200~300W then stands 40~48h of aging, with dehydrated alcohol and acetone at room temperature again
After successively rinsing 3~5 times respectively, then in CO2Dry in supercritical fluid drying device, control critical-temperature is 31~32 DEG C,
Pressure be 7.0~7.5MPa, after the completion of to be dried, collect dry aerogels be placed in 100~110 DEG C of Muffle furnaces, by 1 DEG C/
Min is warming up to 455~480 DEG C, and after 3~5h of insulation reaction, standing, which is cooled to room temperature, is placed in ball milling 3 under 250~300r/min
~5h crosses 500 meshes, obtains composite tin oxide aerogel powder；Silver powder and ball milling sieving are taken, setting mesh size is 70~75 μ
M takes sieving powder and in mass ratio 1: 8, is stirred and is placed in high energy composite tin oxide aerogel powder and sieving powder
In ball mill, ball milling 1h in the environment of ball-milling medium is steel ball, ball material mass ratio is 10: 1 collects ball milling mixing powder juxtaposition
The compression moulding under 250~300MPa is collected compacting blank and is placed at 100~110 DEG C in Muffle furnace, heats up by 5 DEG C/min
To 655~680 DEG C, after 6~8h of heat preservation sintering, then the multiple pressure processing at 1250~1300MPa, it is then placed in 100~110 DEG C again
In lower Muffle furnace, 655~680 DEG C are warming up to by 5 DEG C/min, after 3~4h of heat preservation sintering, then are made annealing treatment at 250~280 DEG C
2~3h can be prepared into the strong―binding interface type Ag/SnO2Contact material；The high energy ball mill is preferably QM-
3A type high energy ball mill.
Embodiment 1
According to parts by weight, 45 parts of acetonitriles, 35 parts of ethyl orthosilicates, 3 parts of deionized waters and 6 parts of propylene oxide are weighed respectively to be placed in
It in conical flask, is stirred juxtaposition and stands 1h at room temperature, obtain matrix liquid A；Again according to parts by weight, 45 parts of second are weighed respectively
Nitrile, 3 parts of Copper dichloride dihydrates and 6 parts of deionized waters are placed in a beaker, and are stirred juxtaposition and are stood 1h at room temperature, obtain matrix liquid
B；According to parts by weight, 45 parts of dehydrated alcohols, 10 parts of 1% acetums of mass fraction and 10 parts of butyl titanates are weighed respectively to be placed in
In conical flask, it is stirred to obtain modified complex liquid；By volume 1: 2: 2, by matrix liquid B and matrix liquid A and modification complex liquid
It is stirred to obtain mixed liquor, then in mass ratio 1: 5, mixed liquor is added dropwise in propylene oxide, control drop rate is 0.1mL/
S collects dropwise addition complex liquid and is placed in insulation reaction 25min at 30 DEG C, collect to obtain reaction sol solutions after being added dropwise to complete；By weight
Number meter is measured, 45 parts of dehydrated alcohols, 3 parts of stannic chlorides and 10 parts of propylene oxide is weighed respectively and is placed in conical flask, be stirred
Juxtaposition stands 3h at room temperature, collects aged gel liquid and in mass ratio 1: 1, and aged gel liquid is mixed with sol solutions stirring is reacted
Merging is placed in ultrasonic disperse 10min under 200~300W, then stands aging 40h at room temperature again, with dehydrated alcohol and acetone according to
After secondary flushing respectively 3 times, then in CO2Dry in supercritical fluid drying device, control critical-temperature is 31 DEG C, and pressure is
7.0MPa after the completion of to be dried, collect dry aerogels and is placed in 100 DEG C of Muffle furnaces, is warming up to 455 DEG C by 1 DEG C/min, protects
After temperature reaction 3h, standing, which is cooled to room temperature, is placed in ball milling 3h under 250r/min, crosses 500 meshes, obtains composite tin oxide aeroge
Powder；Silver powder and ball milling sieving are taken, setting mesh size is 70 μm, sieving powder and in mass ratio 1: 8 is taken, by composite tin oxide
Aerogel powder and sieving powder are stirred and are placed in QM-3A type high energy ball mill, are steel ball, ball material matter in ball-milling medium
Amount ratio is ball milling 1h in the environment of 10: 1, collects ball milling mixing powder and is placed in compression moulding under 250MPa, collects compacting blank
It is placed at 100 DEG C in Muffle furnace, 655 DEG C is warming up to by 5 DEG C/min, after heat preservation sintering 6h, then at 1250MPa at multiple pressure
Reason, is then placed in again at 100 DEG C in Muffle furnace, is warming up to 655 DEG C by 5 DEG C/min, after heat preservation sintering 3h, then moves back at 250 DEG C
Fire processing 2h, can be prepared into the strong―binding interface type Ag/SnO2Contact material.
Embodiment 2
According to parts by weight, 47 parts of acetonitriles, 37 parts of ethyl orthosilicates, 4 parts of deionized waters and 7 parts of propylene oxide are weighed respectively to be placed in
It in conical flask, is stirred juxtaposition and stands 1h at room temperature, obtain matrix liquid A；Again according to parts by weight, 47 parts of second are weighed respectively
Nitrile, 4 parts of Copper dichloride dihydrates and 7 parts of deionized waters are placed in a beaker, and are stirred juxtaposition and are stood 1h at room temperature, obtain matrix liquid
B；According to parts by weight, 47 parts of dehydrated alcohols, 12 parts of 1% acetums of mass fraction and 12 parts of butyl titanates are weighed respectively to be placed in
In conical flask, it is stirred to obtain modified complex liquid；By volume 1: 2: 2, by matrix liquid B and matrix liquid A and modification complex liquid
It is stirred to obtain mixed liquor, then in mass ratio 1: 5, mixed liquor is added dropwise in propylene oxide, control drop rate is 0.1mL/
S collects dropwise addition complex liquid and is placed in insulation reaction 28min at 35 DEG C, collect to obtain reaction sol solutions after being added dropwise to complete；By weight
Number meter is measured, 47 parts of dehydrated alcohols, 4 parts of stannic chlorides and 12 parts of propylene oxide is weighed respectively and is placed in conical flask, be stirred
Juxtaposition stands 4h at room temperature, collects aged gel liquid and in mass ratio 1: 1, and aged gel liquid is mixed with sol solutions stirring is reacted
Merging is placed in ultrasonic disperse 12min under 250W, then stands aging 44h at room temperature again, is successively divided with dehydrated alcohol and acetone
It Chong Xi not be after 4 times, then in CO2Dry in supercritical fluid drying device, control critical-temperature is 31 DEG C, pressure 7.2MPa,
After the completion of to be dried, collect dry aerogels and be placed in 105 DEG C of Muffle furnaces, be warming up to 465 DEG C by 1 DEG C/min, insulation reaction
After 4h, standing, which is cooled to room temperature, is placed in ball milling 4h under 280r/min, crosses 500 meshes, obtains composite tin oxide aerogel powder；It takes
Silver powder and ball milling sieving, setting mesh size are 72 μm, sieving powder and in mass ratio 1: 8 are taken, by composite tin oxide aeroge
Powder and sieving powder are stirred and are placed in QM-3A type high energy ball mill, ball-milling medium is steel ball, ball material mass ratio is
Ball milling 1h in the environment of 10: 1 collects ball milling mixing powder and is placed in compression moulding under 280MPa, collects compacting blank and is placed in
At 105 DEG C in Muffle furnace, 665 DEG C are warming up to by 5 DEG C/min, after heat preservation sintering 7h, then the multiple pressure processing at 1275MPa, then
It is placed at 105 DEG C in Muffle furnace again, is warming up to 665 DEG C by 5 DEG C/min, after heat preservation sintering 3h, then made annealing treatment at 265 DEG C
2h can be prepared into the strong―binding interface type Ag/SnO2Contact material.
Embodiment 3
According to parts by weight, 50 parts of acetonitriles, 40 parts of ethyl orthosilicates, 5 parts of deionized waters and 8 parts of propylene oxide are weighed respectively to be placed in
It in conical flask, is stirred juxtaposition and stands 2h at room temperature, obtain matrix liquid A；Again according to parts by weight, 50 parts of second are weighed respectively
Nitrile, 5 parts of Copper dichloride dihydrates and 8 parts of deionized waters are placed in a beaker, and are stirred juxtaposition and are stood 2h at room temperature, obtain matrix liquid
B；According to parts by weight, 50 parts of dehydrated alcohols, 15 parts of 1% acetums of mass fraction and 15 parts of butyl titanates are weighed respectively to be placed in
In conical flask, it is stirred to obtain modified complex liquid；By volume 1: 2: 2, by matrix liquid B and matrix liquid A and modification complex liquid
It is stirred to obtain mixed liquor, then in mass ratio 1: 5, mixed liquor is added dropwise in propylene oxide, control drop rate is 0.1mL/
S collects dropwise addition complex liquid and is placed in insulation reaction 30min at 40 DEG C, collect to obtain reaction sol solutions after being added dropwise to complete；By weight
Number meter is measured, 50 parts of dehydrated alcohols, 5 parts of stannic chlorides and 15 parts of propylene oxide is weighed respectively and is placed in conical flask, be stirred
Juxtaposition stands 5h at room temperature, collects aged gel liquid and in mass ratio 1: 1, and aged gel liquid is mixed with sol solutions stirring is reacted
Merging is placed in ultrasonic disperse 15min under 300W, then stands aging 48h at room temperature again, is successively divided with dehydrated alcohol and acetone
It Chong Xi not be after 5 times, then in CO2Dry in supercritical fluid drying device, control critical-temperature is 32 DEG C, pressure 7.5MPa,
After the completion of to be dried, collect dry aerogels and be placed in 110 DEG C of Muffle furnaces, be warming up to 480 DEG C by 1 DEG C/min, insulation reaction
After 5h, standing, which is cooled to room temperature, is placed in ball milling 5h under 300r/min, crosses 500 meshes, obtains composite tin oxide aerogel powder；It takes
Silver powder and ball milling sieving, setting mesh size are 75 μm, sieving powder and in mass ratio 1: 8 are taken, by composite tin oxide aeroge
Powder and sieving powder are stirred and are placed in QM-3A type high energy ball mill, ball-milling medium is steel ball, ball material mass ratio is
Ball milling 1h in the environment of 10: 1 collects ball milling mixing powder and is placed in compression moulding under 300MPa, collects compacting blank and is placed in
At 110 DEG C in Muffle furnace, 680 DEG C are warming up to by 5 DEG C/min, after heat preservation sintering 8h, then the multiple pressure processing at 1300MPa, then
It is placed at 110 DEG C in Muffle furnace again, is warming up to 680 DEG C by 5 DEG C/min, after heat preservation sintering 4h, then made annealing treatment at 280 DEG C
3h can be prepared into the strong―binding interface type Ag/SnO2Contact material.
Reference examples: the contact material of Dongguan company production.
The contact material that embodiment and reference examples are prepared is detected, specific detection is as follows:
Hardness: instrument is HBRVU-187.5 type Michael Burawoy optics hardometer, and pressure head is positive rectangular pyramid made of diamond
Body, the angle between two opposite faces is 136 °, test force 294.2N, retention time 15s.
Resistivity: using the square resistance of RTS-8 type four-point probe measurement sample, then it is scaled conductivity value；
Using the resistivity of D60K digital metal conductivity meter measurement sheet material.
Electrical contact performance: the JF04C type electric life stimulation tester produced using Kunming Guiyan Jinfeng Technology Co., Ltd.
The electric life and dynamic electrical contact performance of electrical contact sample are characterized, experiment condition is that AC load voltage is 380V, load current
25A, test frequency are 60 times/min.Sample all undergoes more than 10,000 times on-off loop tests.
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples |
| Hardness/HV | 88.09 | 88.56 | 89.01 | 70.13 |
| Resistivity/u Ω cm | 2.81 | 2.76 | 2.93 | 3.73 |
| Contact resistance/m Ω | 4.41 | 4.30 | 4.22 | 9.31 |
As shown in Table 1, contact material prepared by the present invention has good hardness and electrical contact performance.
Claims (10)
1. a kind of strong―binding interface type Ag/SnO2The preparation method of contact material, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, 45~50 parts of acetonitriles, 35~40 parts of ethyl orthosilicates, 3~5 parts of deionized waters and 6 are weighed respectively
~8 parts of propylene oxide are placed in conical flask, are stirred juxtaposition and are stood 1~2h at room temperature, and matrix liquid A is obtained；Again by weight
Number meter weighs 45~50 parts of acetonitriles, 3~5 parts of Copper dichloride dihydrates and 6~8 parts of deionized waters respectively and is placed in a beaker, stirs
Mixing juxtaposition stands 1~2h at room temperature, obtains matrix liquid B；
(2) according to parts by weight, 45~50 parts of dehydrated alcohols, 10~15 parts of acetums and 10~15 parts of metatitanic acid fourths are weighed respectively
Ester is placed in conical flask, is stirred to obtain modified complex liquid；By volume 1: 2: 2, by matrix liquid B and matrix liquid A and modification
Complex liquid is stirred to obtain mixed liquor, then in mass ratio 1: 5, and mixed liquor is added dropwise in propylene oxide, after being added dropwise to complete, receives
Collection is added dropwise complex liquid and is placed in insulation reaction, collects to obtain reaction sol solutions；
(3) according to parts by weight, 45~50 parts of dehydrated alcohols, 3~5 parts of stannic chlorides and 10~15 parts of propylene oxide are weighed respectively to set
In conical flask, be stirred juxtaposition and stand at room temperature, collect aged gel liquid and by aged gel liquid with react colloidal sol
Liquid is stirred and ultrasonic disperse, then stands aging at room temperature again, carrying out washing treatment, then in CO2Supercritical fluid drying dress
Set middle drying, after the completion of to be dried, collect dry aerogels and the heating and thermal insulation that heats up and react, standing is cooled to room temperature and ball milling,
Sieving, obtains composite tin oxide aerogel powder；
(4) silver powder and ball milling sieving are taken, sieving powder and in mass ratio 1: 8 is taken, by composite tin oxide aerogel powder and sieving
Powder, which is stirred, to be placed in high energy ball mill, ball milling, collects ball milling mixing powder and compression moulding, collects compacting blank simultaneously
It is placed in Muffle furnace, heating heating, heat preservation sintering, then the processing of multiple pressure, after secondary temperature elevation heating, heat preservation sintering, annealing, i.e.,
The strong―binding interface type Ag/SnO can be prepared into2Contact material.
2. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the acetum concentration is mass fraction 1%.
3. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the carrying out washing treatment is successively to be rinsed 3~5 times respectively with dehydrated alcohol and acetone.
4. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the CO2Supercritical fluid drying device drying parameter be control critical-temperature be 31~32 DEG C, pressure be 7.0~
7.5MPa。
5. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the mixed liquor drop rate is 0.1mL/s.
6. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the mesh size is 70~75 μm.
7. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the aged gel liquid is in mass ratio 1: 1 with sol solutions compositely proportional is reacted.
8. a kind of preparation method of strong―binding interface type Ag/SnO2 contact material according to claim 1, feature exist
In: the multiple pressure processing pressure is 1250~1300MPa.
9. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the secondary temperature elevation heats, heat preservation sintering is to be warming up to 655~680 DEG C by 5 DEG C/min, 3~4h of heat preservation sintering.
10. a kind of strong―binding interface type Ag/SnO according to claim 12The preparation method of contact material, feature exist
In: the high energy ball mill is preferably QM-3A type high energy ball mill.
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| CN1137068A (en) * | 1995-02-01 | 1996-12-04 | 底古萨股份公司 | Sintering material on basis of silver-tin oxide for electrical contacts and process for its manufacture |
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| CN106086495A (en) * | 2016-06-17 | 2016-11-09 | 石家庄铁道大学 | Cupric oxide doped siller tin oxide composite and preparation method thereof |
| CN106191495A (en) * | 2016-07-12 | 2016-12-07 | 西安工程大学 | The tin-oxygen-silver electric contact material preparation method of chemically based sedimentation |
| US20190114712A1 (en) * | 2017-10-16 | 2019-04-18 | Zepa Financial Technology Ltd. | System and method for supporting decision according to multiple aggregated decisions |
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| CN1137068A (en) * | 1995-02-01 | 1996-12-04 | 底古萨股份公司 | Sintering material on basis of silver-tin oxide for electrical contacts and process for its manufacture |
| CN102432284A (en) * | 2011-08-23 | 2012-05-02 | 陕西科技大学 | Preparation method of crystal boundary layer type structure ceramic membrane |
| CN106086495A (en) * | 2016-06-17 | 2016-11-09 | 石家庄铁道大学 | Cupric oxide doped siller tin oxide composite and preparation method thereof |
| CN106191495A (en) * | 2016-07-12 | 2016-12-07 | 西安工程大学 | The tin-oxygen-silver electric contact material preparation method of chemically based sedimentation |
| US20190114712A1 (en) * | 2017-10-16 | 2019-04-18 | Zepa Financial Technology Ltd. | System and method for supporting decision according to multiple aggregated decisions |
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