CN106711262B - A kind of space molybdenum/titanium/silver metal laminar composite and preparation method thereof - Google Patents
A kind of space molybdenum/titanium/silver metal laminar composite and preparation method thereof Download PDFInfo
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- CN106711262B CN106711262B CN201510781955.XA CN201510781955A CN106711262B CN 106711262 B CN106711262 B CN 106711262B CN 201510781955 A CN201510781955 A CN 201510781955A CN 106711262 B CN106711262 B CN 106711262B
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- silver
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 139
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 133
- 239000011733 molybdenum Substances 0.000 title claims abstract description 133
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000010936 titanium Substances 0.000 title claims abstract description 96
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000011888 foil Substances 0.000 claims abstract description 64
- 238000005096 rolling process Methods 0.000 claims abstract description 36
- 238000000137 annealing Methods 0.000 claims abstract description 26
- 239000011261 inert gas Substances 0.000 claims abstract description 21
- 238000011282 treatment Methods 0.000 claims abstract description 9
- ZPZCREMGFMRIRR-UHFFFAOYSA-N molybdenum titanium Chemical compound [Ti].[Mo] ZPZCREMGFMRIRR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000011221 initial treatment Methods 0.000 claims abstract description 3
- 239000003960 organic solvent Substances 0.000 claims description 9
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- 238000005488 sandblasting Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 4
- MZFIXCCGFYSQSS-UHFFFAOYSA-N silver titanium Chemical compound [Ti].[Ag] MZFIXCCGFYSQSS-UHFFFAOYSA-N 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 238000010923 batch production Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005098 hot rolling Methods 0.000 abstract 2
- 229910052709 silver Inorganic materials 0.000 description 21
- 239000004332 silver Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 239000010944 silver (metal) Substances 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 11
- 238000007747 plating Methods 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000010946 fine silver Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910000833 kovar Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000002203 pretreatment Methods 0.000 description 5
- 238000003466 welding Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- LFDBSBBPLDBESI-UHFFFAOYSA-N [Ag].[Ti].[Mo] Chemical compound [Ag].[Ti].[Mo] LFDBSBBPLDBESI-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000005422 blasting Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical compound OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N hydrofluoric acid Substances F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000011536 re-plating Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- FSVVWABMXMMPEE-UHFFFAOYSA-N molybdenum silver Chemical compound [Mo][Ag][Mo] FSVVWABMXMMPEE-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/05—Electrical interconnection means between PV cells inside the PV module, e.g. series connection of PV cells
- H01L31/0504—Electrical interconnection means between PV cells inside the PV module, e.g. series connection of PV cells specially adapted for series or parallel connection of solar cells in a module
- H01L31/0512—Electrical interconnection means between PV cells inside the PV module, e.g. series connection of PV cells specially adapted for series or parallel connection of solar cells in a module made of a particular material or composition of materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
- B21B45/02—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for lubricating, cooling, or cleaning
- B21B45/0269—Cleaning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
- B21B45/04—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for de-scaling, e.g. by brushing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B47/00—Auxiliary arrangements, devices or methods in connection with rolling of multi-layer sheets of metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B9/00—Measures for carrying out rolling operations under special conditions, e.g. in vacuum or inert atmosphere to prevent oxidation of work; Special measures for removing fumes from rolling mills
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1876—Particular processes or apparatus for batch treatment of the devices
- H01L31/188—Apparatus specially adapted for automatic interconnection of solar cells in a module
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Sustainable Development (AREA)
- Life Sciences & Earth Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Sustainable Energy (AREA)
- Manufacturing & Machinery (AREA)
- Metal Rolling (AREA)
- Laminated Bodies (AREA)
Abstract
The present invention relates to space molybdenum/titanium/silver metal laminar composites and preparation method thereof, and composite material includes：One layer of pure molybdenum foil；Two layers of pure titanium foil；Two layers of pure silver foil builds up class " sandwich " structure, and link into an integrated entity according to the sequence of pure silver foil, pure titanium foil, pure molybdenum foil, pure titanium foil and pure silver foil, and molybdenum titanium interface and silver-colored titanium interface are with enhanced primary treatment.Preparation method includes：The combination blank of class " sandwich " structure is built up in sequence；Combination blank is subjected to hot rolling composite joint, after rolling, is further made annealing treatment under inert gas atmosphere；Space molybdenum/titanium/silver metal laminar composite is obtained after annealing.The composite material of the present invention has good space environment adaptability, thermal conductivity, electric conductivity and solderability, meets the requirement of space electronic package application；Preparation method is formed by hot rolling composite rolling composite joint, the roll-to-roll batch production of simple, stable and controllable for quality, easy to operate, the achievable large area automation of manufacture craft.
Description
Technical field
The present invention relates to space equipment and method field, more particularly to a kind of space molybdenum/titanium/silver metal stratiform composite wood
Material and preparation method thereof.
Background technology
Space technology develops and the space launch cost of costliness is to the spacecraft normally new requirement of service life proposition in orbit.
Complicated and changeable to the effect of spacecraft surfacing since space environment is severe, long-term work is in the solar energy on spacecraft surface
Cell array will suffer from the erosions such as high energy particle, micrometeor, space junk, elemental oxygen, so as to influence aircraft normally in orbit
Service life.
Solar array is the array formed by monomer gallium arsenide solar cell by metal interconnection concatenation, empty at present
Between the interconnection metal material that uses on solar array be mainly fine silver interconnection piece, space environment adaptability is poor, seriously
Constrain the spacecraft in-orbit flight service life.
Metal molybdenum can be cut down（Kovar）The metal materials such as alloy are due to good conductive, heat conductivility and resistance to atom
Oxygen performance, and it is widely used in space electronic encapsulation field, relative to that can cut down-silver composite material, molybdenum-silver composite material has nothing
The advantages that remanent magnetism, high intensity, is particularly suited for space electronic interconnection.In the side that molybdenum foil, Kovar alloy surface pass through electrosilvering
Laminar composite prepared by formula has been used for spacecraft solar cell interconnection package, and confirm that this is compound in foreign countries
The space reliability of material, but since film purity that electroplating technology is coated with is low, compactness is poor causes prepared mutually to weld in flakes
Connect reliability still can not with fine silver mutually in flakes compared with；In recent years, as domestic long-life satellite technology develops, relevant unit
Carried out the development for the metallic composite of resistance to elemental oxygen, as the 18th joint University Of Tianjin of research institute of electronics technology group use from
Silver particles are injected into molybdenum foil surface in advance and carry out high-temperature heat treatment to it, then by the way that silvery is electroplated by beamlet injection technique
It is standby mutually in flakes；In molybdenum foil, kovar alloy surface preplating buffer layer metal by the way of plating（Such as platinum, nickel, chromium, copper, titanium）,
Then re-plating silvery is standby mutually in flakes；Using prepared by the way of the gold-plated protection of silver surface mutually in flakes；Shanghai space power system research
Also similar technology is used, is prepared mutually in flakes in Kovar alloy, molybdenum foil electroplate.But since Domestic Plating technology is opposite
It is external also there are certain gap, it is domestic at present by plating mode prepare mutually solderability is poor in flakes, coating firmness is poor, it is difficult to
Meet space application.For plating, vacuum coating technology particle energy is high, and coating purity is consistent with block, is coated with
Silver layer compactness is high, and based on this, Shanghai Institute of Space Power-Sources is by layer buffer design, using vacuum coating technology in Kovar
Alloy, molybdenum foil surface deposition silvering are prepared mutually in flakes, prepared mutually to have good solderability in flakes, and have passed through ground sky
Between environment examine, but vacuum plating silver is of high cost, be not easy to large area production, compactness of electroplating with respect to fine silver interconnect piece it is poor.
The Chinese patent that notification number is 103681952A be " spacecraft molybdenum/platinum/silver laminar metal matrix composite
Preparation process ", wherein, molybdenum base electrosilvering is mutually that buffer layer metallic film is electroplated in advance on molybdenum foil surface in flakes, then re-plating
Silver.This preparation method is influenced due to being limited to plating solution and technique, and plating silver layer purity is relatively low, compactness is poor, so as to cause system
Standby mutual solderability in flakes is poor, and firmness is poor, and surface state is easily affected by environment.
Invention content
The purpose of the present invention is to provide a kind of space molybdenum/titanium/silver metal laminar composite and preparation method thereof, with
Solve that layered metal composite material coating prepared by existing molybdenum base electrosilvering is insecure, compactness is poor, solderability is poor, electroplating quality
The problems such as uncontrollable, complex process.
In order to solve the above-mentioned technical problem, the technical scheme is that：It is answered with molybdenum/titanium/silver metal stratiform in a kind of space
Condensation material, including：One layer of pure molybdenum foil；Two layers of pure titanium foil；Two layers of pure silver foil, according to the pure silver foil, pure titanium foil, described pure
The sequence of molybdenum foil, the pure titanium foil and the pure silver foil builds up class " sandwich " structure, and links into an integrated entity, molybdenum-titanium interface and
Silver-titanium interface is with enhanced primary treatment.
Further, in the space in molybdenum/titanium/silver metal laminar composite, the pure molybdenum foil, the pure titanium foil
It is all higher than being equal to 99.9% with the purity of the pure silver foil.
Further, in the space in molybdenum/titanium/silver metal laminar composite, the thickness of the pure molybdenum foil for 10 ~
80μm。
Further, in the space in molybdenum/titanium/silver metal laminar composite, the thickness of the pure titanium foil for 5 ~
15μm。
Further, in the space in molybdenum/titanium/silver metal laminar composite, the thickness of the pure silver foil for 8 ~
50μm。
Further, the space is for space gallium arsenide solar cell with molybdenum/titanium/silver metal laminar composite
Series and parallel connects.
The present invention also provides a kind of space preparation method of molybdenum/titanium/silver metal laminar composite, a kind of space is used
The preparation method of molybdenum/titanium/silver metal laminar composite, including：It will be respectively by pure molybdenum foil, pure titanium foil and the fine silver of pretreatment
Foil builds up class " three according to the sequence of the pure silver foil, the pure titanium foil, the pure molybdenum foil, the pure titanium foil and the pure silver foil
The combination blank of Mingzhi " structure；
The combination blank under vacuum or inert gas shielding is first subjected to constant temperature pretreatment, then carries out rolling again multiple
Connection is closed, the test specimen after rolling further makes annealing treatment under inert gas atmosphere, after the completion of annealing, obtains space and uses
Molybdenum/titanium/silver metal laminar composite.
Further, in the space in the preparation method of molybdenum/titanium/silver metal laminar composite, to the combination
Before blank carries out Rolling compund connection, carry out the pretreatment of 500 ~ 750 °C of constant temperature to the combination blank, constant temperature time for 10 ~
30min。
Further, in the space in the preparation method of molybdenum/titanium/silver metal laminar composite, to the constant temperature
Pretreated combination blank carries out Rolling compund connection, wherein, rolling temperature is 650 ~ 750 °C, and reduction ratio is 10% ~ 40%,
Mill speed is 0.01 ~ 0.5m/s
Further, in the space in the preparation method of molybdenum/titanium/silver metal laminar composite, to the rolling
Test specimen afterwards further makes annealing treatment under inert gas atmosphere, wherein, annealing temperature is 400 ~ 650 °C, annealing time 0.5
~3h
Further, in the space in the preparation method of molybdenum/titanium/silver metal laminar composite, Rolling compund ring
Border is inert gas atmosphere or vacuum, wherein, the vacuum degree of vacuum environment is 1Pa ~ 1.0 × 10Pa。
Further, in the space in the preparation method of molybdenum/titanium/silver metal laminar composite, to the pure molybdenum
The pretreatment that foil carries out includes：Molybdenum foil is subjected to surface sand-blasting, molybdenum foil surface and oil contaminant is removed using organic solvent, it is molten using soda acid
Liquid removes molybdenum foil surface oxide layer.
Further, in the space in the preparation method of molybdenum/titanium/silver metal laminar composite, to the fine silver
The pretreatment that foil carries out includes：Using the greasy dirt on organic solvent removal silver foil surface, using acid-base solution removal silver foil surface
Oxide layer.
Further, in the space in the preparation method of molybdenum/titanium/silver metal laminar composite, to the pure titanium
The pretreatment that foil carries out includes：Using the greasy dirt on organic solvent removal titanium foil surface, using acid-base solution removal titanium foil surface
Oxide layer.
Space provided by the invention molybdenum/titanium/silver metal laminar composite, since pure molybdenum foil has good vacuum-resistant
Elemental oxygen performance, block pure silver foil have higher compactness and good welding performance so that the molybdenum of preparation-titanium-Yin Jin
Belonging to laminar composite has good space environment adaptability, and the interface cohesion of composite material is secured, has good space
Environmental suitability, thermal conductivity, electric conductivity and solderability meet the requirement of space electronic package application.
Further, welding layer is block pure silver foil used by the molybdenum/titanium/silver metal laminar composite of space, because
This, traditional space by prepared by electrosilvering or other vacuum plating silver technologies is with mutually weldability is good in flakes, technique is simple relatively
Single controllable, achievable large area batch production etc..
The preparation method of space provided by the invention molybdenum/titanium/silver metal laminar composite, space molybdenum/titanium/silver gold
Belong to laminar composite and pass through Rolling compund under vacuum environment or inert gas shielding by bulk metal pure silver foil and pure molybdenum foil
Connection is formed, manufacture craft is simple, it is stable and controllable for quality, easy to operate, large area automatic batch production can be achieved.
Further, in space in the preparation method of molybdenum/titanium/silver metal laminar composite, due to metal molybdenum and titanium
And Titanium and silver can form effective solid solution at a certain temperature, meanwhile, Rolling compund connection before, to combination blank into
500 ~ 750 °C of constant temperature pretreatments of row, to reduce the resistance of deformation of each metal foil so that molybdenum-titanium-silver metal of Rolling compund
Laminar composite interface cohesion is secured.
Description of the drawings
Invention is described further below in conjunction with the accompanying drawings：
Fig. 1 is that the cross-section structure of space molybdenum/titanium/silver metal laminar composite provided in an embodiment of the present invention is illustrated
Figure；
The step of Fig. 2 is the preparation method of space molybdenum/titanium/silver metal laminar composite provided in an embodiment of the present invention
Flow diagram.
Specific embodiment
Below in conjunction with the drawings and specific embodiments to a kind of space proposed by the present invention molybdenum/titanium/silver metal lamellar composite
Material and preparation method thereof is described in further detail.According to following explanation and claims, advantages and features of the invention
It will become apparent from.It should be noted that attached drawing is using very simplified form and using non-accurate ratio, only to it is convenient,
Lucidly aid in illustrating the purpose of the embodiment of the present invention.
The present invention core concept be, space provided by the invention molybdenum/titanium/silver metal laminar composite, due to
Pure molybdenum foil has good vacuum-resistant elemental oxygen performance, and block pure silver foil has higher compactness and good weldability
It can so that molybdenum-titanium-silver metal laminar composite of preparation has good space environment adaptability, the interface of composite material
It is firmly combined with, there is good space environment adaptability, thermal conductivity, electric conductivity and solderability, meet space electronic package application
It is required that.The preparation method of space provided by the invention molybdenum/titanium/silver metal laminar composite, space molybdenum/titanium/silver metal
Laminar composite is connected under vacuum environment or inert gas shielding by bulk metal pure silver foil with pure molybdenum foil by Rolling compund
It connects to be formed, the roll-to-roll batch production of simple, stable and controllable for quality, easy to operate, the achievable large area automation of manufacture craft.
Fig. 1 is that the cross-section structure of space molybdenum/titanium/silver metal laminar composite provided in an embodiment of the present invention is illustrated
Figure.With reference to Fig. 1, a kind of space molybdenum/titanium/silver metal laminar composite provided, including：One layer of pure molybdenum foil 11；Two layers pure
Titanium foil 12；Two layers of pure silver foil 13, according to the pure silver foil 13, the pure titanium foil 12, the pure molybdenum foil 11,12 and of the pure titanium foil
The sequence of the pure silver foil 13 builds up class " sandwich " structure, and links into an integrated entity, molybdenum-titanium interface and being of silver-titanium interface
Learn metallurgical binding.
In embodiments of the present invention, the purity of the pure molybdenum foil 11, the pure titanium foil 12 and the pure silver foil 13 is all higher than
Equal to 99.9%, the thickness of the pure molybdenum foil is 10 ~ 80 μm, and the thickness of the pure titanium foil is 5 ~ 15 μm, the thickness of the pure silver foil
It is 8 ~ 50 μm.
The step of Fig. 2 is the preparation method of space molybdenum/titanium/silver metal laminar composite provided in an embodiment of the present invention
Flow diagram.Reference Fig. 2, the preparation method of space molybdenum/titanium/silver metal laminar composite, including：
S21, pure molybdenum foil, pure titanium foil and the pure silver foil that pretreatment will be passed through respectively, according to the pure silver foil, the pure titanium
Foil, the pure molybdenum foil, the pure titanium foil and the pure silver foil sequence build up the combination blank of class " sandwich " structure；
S22, the combination blank is subjected to Rolling compund connection under vacuum or inert gas environment, wherein, rolling temperature
It is 650 ~ 750 °C to spend, and reduction ratio is 10% ~ 40%, and mill speed is 0.01 ~ 0.5m/s；
S23, it after the combination blank is rolled, further makes annealing treatment under inert gas atmosphere, wherein annealing temperature
It is 400 ~ 650 °C to spend, and annealing time is 0.5 ~ 3h, after the completion of annealing, obtains space molybdenum/titanium/silver metal lamellar composite
Material.
Since metal molybdenum and titanium and Titanium and silver can form effective solid solution at a certain temperature, meanwhile, it is rolling
Before composite joint, 500 ~ 750 °C of constant temperature pretreatments are carried out to combination blank, to reduce the resistance of deformation of each metal foil, make
Molybdenum-titanium-silver metal stratiform the composite material interface for obtaining Rolling compund is firmly combined with.
In embodiments of the present invention, it is rolled in the space in the preparation method of molybdenum/titanium/silver metal laminar composite
Combinational environment processed is inert gas atmosphere or vacuum, wherein, the vacuum degree of vacuum environment is 1Pa ~ 1.0 × 10Pa。
In the space pretreatment in the preparation method of molybdenum/titanium/silver metal laminar composite, carried out to the pure molybdenum foil
Including：Molybdenum foil is subjected to surface sand-blasting, molybdenum foil surface and oil contaminant is removed using organic solvent, using acid-base solution removal molybdenum foil surface
Oxide layer；The pretreatment carried out to the pure silver foil includes：It is molten using soda acid using the greasy dirt on organic solvent removal silver foil surface
The oxide layer on liquid removal silver foil surface；The pretreatment carried out to the pure titanium foil includes：Using organic solvent removal titanium foil surface
Greasy dirt, using the oxide layer on acid-base solution removal titanium foil surface.
Embodiment 1
The space pure molybdenum that the intermediate layer thickness in molybdenum/titanium/silver metal laminar composite is 50 μm, purity is 99.99%
Foil, the pure titanium foil that it is 8 μm that both sides, which help composite bed thickness, purity is 99.99%, two layers of outside welding layer thickness is 20 μm, pure
It spends the pure silver foil for 99.99%, is combined as a whole between five layers by Rolling compund connection, Ag/Ti/Mo/Ti/Ag interfaces are to change
Metallurgical binding is learned, which is welded into space gallium arsenide solar cell using parallel resistance,
Mechanical properties are 6 ~ 8N, and interface does not occur obscission.
Space is prepared to be operated as follows with the operation of molybdenum/titanium/silver metal laminar composite:By the silver foil of two piece of 20 μ m-thick,
The titanium foil of two piece of 8 μ m-thick is respectively successively using isopropanol, semiconductor washing solution, that is, 1# electronics cleaning solution removal silver foil and titanium foil
The greasy dirt on surface, using 25% hydrofluoric acid（HF）Aqueous solution removes the oxide layer on silver foil and titanium foil surface；Simultaneously by one piece 50
The molybdenum foil surface of μ m-thick carries out blasting treatment, and successively using isopropanol, semiconductor washing solution（1# electronics cleaning solutions）Cleaning, with
The greasy dirt on molybdenum foil surface and sulfuric acid (H2SO2) and hydrochloric acid (HCl) mixed solution the removal molybdenum foil table of use 5% after removal sandblasting
The oxide layer in face, the size of silver foil is consistent with molybdenum foil, is folded by the sequence of pure silver foil-pure titanium foil-pure molybdenum foil-pure titanium foil-pure silver foil
Into class " sandwich " structure（That is silver/titanium/molybdenum/titanium/silver：Ag/Ti/Mo/Ti/Ag）Combination blank；Combination blank is carried out
Combination blank is carried out Rolling compund by 600 °C of constant temperature pretreatments, constant temperature time 15min under inert gas shielding after the completion
Connection, inert gas is using argon gas in the present embodiment, and rolling temperature is 750 °C, reduction ratio 20%, and mill speed is
0.02m/s, after rolling, further annealing, annealing temperature are 550 °C under inert gas atmosphere, and annealing time 2h is moved back
After the completion of fire processing, space molybdenum/titanium/silver metal laminar composite is obtained.
Embodiment 2
The space pure molybdenum that the intermediate layer thickness in molybdenum/titanium/silver metal laminar composite is 30 μm, purity is 99.99%
Foil, the pure titanium foil that it is 6 μm that both sides, which help composite bed thickness, purity is 99.99%, two layers of outside welding layer thickness is 20 μm, pure
It spends the pure silver foil for 99.99%, is combined as a whole between five layers by Rolling compund connection, Ag/Ti/Mo/Ti/Ag interfaces are to change
Metallurgical binding is learned, which is welded into space gallium arsenide solar cell using parallel resistance,
Mechanical properties are 6 ~ 8N, and interface does not occur obscission.
The titanium foil of the silver foil of two piece of 20 μ m-thick, two piece of 6 μ m-thick is used into isopropanol, semiconductor washing solution, that is, 1# successively respectively
Electronics cleaning solution removes silver foil and the greasy dirt on titanium foil surface, using 25% hydrofluoric acid（HF）Aqueous solution removes silver foil and titanium
The oxide layer on foil surface；The molybdenum foil surface of one piece of 30 μ m-thick is subjected to blasting treatment simultaneously, and successively using isopropanol, semiconductor
Cleaning solution（1# electronics cleaning solutions）Cleaning, with remove the greasy dirt on molybdenum foil surface after sandblasting and using 5% sulfuric acid (H2SO2) and
The oxide layer on hydrochloric acid (HCl) mixed solution removal molybdenum foil surface, the size of silver foil is consistent with molybdenum foil, by pure silver foil-pure titanium foil-pure
The sequence of molybdenum foil-pure titanium foil-pure silver foil builds up class " sandwich " structure（That is silver/titanium/molybdenum/titanium/silver：Ag/Ti/Mo/Ti/Ag）
Combination blank；700 °C of constant temperature pretreatments are carried out to combination blank, constant temperature time 20min will combine blank lazy after the completion
Property gas shield under carry out Rolling compund connection, for inert gas using argon gas, rolling temperature is 700 ° in the present embodiment
C, reduction ratio 30%, mill speed 0.01m/s, after rolling, further annealing, annealing are warm under inert gas atmosphere
It is 550 °C, annealing time 2h to spend, and after the completion of annealing, obtains space molybdenum/titanium/silver metal laminar composite.
Embodiment 3
The space pure molybdenum that the intermediate layer thickness in molybdenum/titanium/silver metal laminar composite is 15 μm, purity is 99.99%
Foil, the pure titanium foil that it is 6 μm that both sides, which help composite bed thickness, purity is 99.99%, two layers of outside welding layer thickness is 20 μm, pure
It spends the pure silver foil for 99.99%, is combined as a whole between five layers by Rolling compund connection, Ag/Ti/Mo/Ti/Ag interfaces are to change
Metallurgical binding is learned, which is welded into space gallium arsenide solar cell using parallel resistance,
Mechanical properties are 6 ~ 8N, and interface does not occur obscission.
The titanium foil of the silver foil of two piece of 20 μ m-thick, two piece of 6 μ m-thick is used into isopropanol, semiconductor washing solution, that is, 1# successively respectively
Electronics cleaning solution removes silver foil and the greasy dirt on titanium foil surface, using 25% hydrofluoric acid（HF）Aqueous solution removes silver foil and titanium
The oxide layer on foil surface；The molybdenum foil surface of one piece of 15 μ m-thick is subjected to blasting treatment simultaneously, and successively using isopropanol, semiconductor
Cleaning solution（1# electronics cleaning solutions）Cleaning, with remove the greasy dirt on molybdenum foil surface after sandblasting and using 5% sulfuric acid (H2SO2) and
The oxide layer on hydrochloric acid (HCl) mixed solution removal molybdenum foil surface, the size of silver foil is consistent with molybdenum foil, by pure silver foil-pure titanium foil-pure
The sequence of molybdenum foil-pure titanium foil-pure silver foil builds up class " sandwich " structure（That is silver/titanium/molybdenum/titanium/silver：Ag/Ti/Mo/Ti/Ag）
Combination blank；650 °C of constant temperature pretreatments are carried out to combination blank, constant temperature time 20min will combine blank lazy after the completion
Property gas shield under carry out Rolling compund connection, for inert gas using argon gas, rolling temperature is 700 ° in the present embodiment
C, reduction ratio 40%, mill speed 0.01m/s, after rolling, further annealing, annealing are warm under inert gas atmosphere
It is 550 °C, annealing time 2h to spend, and after the completion of annealing, obtains space molybdenum/titanium/silver metal laminar composite.
Obviously, those skilled in the art can carry out the present invention essence of various changes and deformation without departing from the present invention
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (14)
1. a kind of space molybdenum/titanium/silver metal laminar composite, which is characterized in that including：
One layer of pure molybdenum foil；
Two layers of pure titanium foil；
Two layers of pure silver foil, according to the pure silver foil, the pure titanium foil, the pure molybdenum foil, the pure titanium foil and the pure silver foil
Sequence builds up class " sandwich " structure, and link into an integrated entity, and molybdenum-titanium interface and silver-titanium interface are with enhanced primary treatment.
2. space as described in claim 1 molybdenum/titanium/silver metal laminar composite, which is characterized in that the pure molybdenum foil,
The purity of the pure titanium foil and the pure silver foil is all higher than being equal to 99.9%.
3. space as described in claim 1 molybdenum/titanium/silver metal laminar composite, which is characterized in that the pure molybdenum foil
Thickness is 10 ~ 80 μm.
4. space as described in claim 1 molybdenum/titanium/silver metal laminar composite, which is characterized in that the pure titanium foil
Thickness is 5 ~ 15 μm.
5. space as described in claim 1 molybdenum/titanium/silver metal laminar composite, which is characterized in that the pure silver foil
Thickness is 8 ~ 50 μm.
6. space as described in claim 1 molybdenum/titanium/silver metal laminar composite, which is characterized in that use in the space
Molybdenum/titanium/silver metal laminar composite is connect for space gallium arsenide solar cell series and parallel.
7. a kind of space preparation method of molybdenum/titanium/silver metal laminar composite, which is characterized in that including：
It will be respectively by pure molybdenum foil, pure titanium foil and the pure silver foil of pretreatment, according to the pure silver foil, pure titanium foil, described pure
The sequence of molybdenum foil, the pure titanium foil and the pure silver foil builds up the combination blank of class " sandwich " structure；
The combination blank under vacuum or inert gas shielding is first subjected to constant temperature pretreatment, then carries out Rolling compund company again
Connect, the test specimen after rolling further makes annealing treatment under inert gas atmosphere, after the completion of annealing, obtain space with molybdenum/titanium/
Silver metal laminar composite.
8. the space as claimed in claim 7 preparation method of molybdenum/titanium/silver metal laminar composite, which is characterized in that right
Before the combination blank carries out Rolling compund connection, the pretreatment of 500 ~ 750 °C of constant temperature is carried out to the combination blank, during constant temperature
Between be 10 ~ 30min.
9. the space as claimed in claim 7 preparation method of molybdenum/titanium/silver metal laminar composite, which is characterized in that right
The pretreated combination blank of constant temperature carries out Rolling compund connection, wherein, rolling temperature is 650 ~ 750 °C, and reduction ratio is
10% ~ 40%, mill speed is 0.01 ~ 0.5m/s.
10. the preparation method of space as claimed in claim 7 molybdenum/titanium/silver metal laminar composite, which is characterized in that
Test specimen after the rolling is further made annealing treatment under inert gas atmosphere, wherein, annealing temperature is 400 ~ 650 °C, is moved back
The fiery time is 0.5 ~ 3h.
11. the space as claimed in claim 7 preparation method of molybdenum/titanium/silver metal laminar composite, which is characterized in that
Rolling compund environment is inert gas atmosphere or vacuum, wherein, the vacuum degree of vacuum environment is 1Pa ~ 1.0 × 10-3Pa。
12. the space as claimed in claim 7 preparation method of molybdenum/titanium/silver metal laminar composite, which is characterized in that
The pretreatment carried out to the pure molybdenum foil includes：Molybdenum foil is subjected to surface sand-blasting process, using organic solvent removal molybdenum foil surface
Greasy dirt removes molybdenum foil surface oxide layer using acid-base solution.
13. the preparation method of space as claimed in claim 7 molybdenum/titanium/silver metal laminar composite, which is characterized in that
The pretreatment carried out to the pure silver foil includes：Using the greasy dirt on organic solvent removal silver foil surface, removed using acid-base solution
The oxide layer on silver foil surface.
14. the space as claimed in claim 7 preparation method of molybdenum/titanium/silver metal laminar composite, which is characterized in that
The pretreatment carried out to the pure titanium foil includes：Using the greasy dirt on organic solvent removal titanium foil surface, removed using acid-base solution
The oxide layer on titanium foil surface.
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| CN113927970A (en) * | 2020-06-29 | 2022-01-14 | 江苏欣恒蕴精密零件有限公司 | Silver/molybdenum/silver metal-based layered composite material and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6909185B1 (en) * | 1998-12-07 | 2005-06-21 | Hitachi, Ltd. | Composite material including copper and cuprous oxide and application thereof |
| CN102169912A (en) * | 2011-01-17 | 2011-08-31 | 天津大学 | Mo/Ag laminated metal matrix composite for solar cell interconnected sheet and preparation process thereof |
| CN103681952A (en) * | 2013-08-20 | 2014-03-26 | 天津大学 | A preparation technique for spacecraft-used molybdenum/platinum/silver/ layered metal matrix composite materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6909185B1 (en) * | 1998-12-07 | 2005-06-21 | Hitachi, Ltd. | Composite material including copper and cuprous oxide and application thereof |
| CN102169912A (en) * | 2011-01-17 | 2011-08-31 | 天津大学 | Mo/Ag laminated metal matrix composite for solar cell interconnected sheet and preparation process thereof |
| CN103681952A (en) * | 2013-08-20 | 2014-03-26 | 天津大学 | A preparation technique for spacecraft-used molybdenum/platinum/silver/ layered metal matrix composite materials |
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