CN106834764A - A kind of preparation method of copper-molybdenum copper multilayer materials - Google Patents
A kind of preparation method of copper-molybdenum copper multilayer materials Download PDFInfo
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- CN106834764A CN106834764A CN201710015526.0A CN201710015526A CN106834764A CN 106834764 A CN106834764 A CN 106834764A CN 201710015526 A CN201710015526 A CN 201710015526A CN 106834764 A CN106834764 A CN 106834764A
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- 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
- C22C1/02—Making non-ferrous alloys by melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/202—Conductive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
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Abstract
A kind of preparation method of copper-molybdenum copper multilayer materials, including the pre-treatment step of molybdenum plate and copper base, the arrangement number of assembling steps of castingin sheet material, heating castingin step, polishing pre-shaping step, hot rolling and annealing heat-treats step and cold rolling and annealing heat-treats step.The method that the present invention utilizes castingin+rolling, copper-molybdenum copper coin material is combined with each other, form multi-layer compound structure, and crucible is designed, improve copper-molybdenum copper thickness than accuracy, this method not only makes copper-molybdenum material tight be combined with each other, and significantly enhances the bond strength of compound interface, meanwhile, heat conduction, conductive and coefficient of expansion controllability to copper-molybdenum copper composite board are all obviously improved.
Description
Technical field
The present invention relates to metallic composite interconnection technique field, and in particular to a kind of system of copper-molybdenum copper multilayer materials
Preparation Method.
Background technology
Copper is good heat conduction and conductive material, and with good pliability, it is easy to machine-shaping, it is widely used
In electronic package material field.But because its thermal coefficient of expansion is larger, it is impossible to match with many semi-conducting materials, limit it
Further apply；Refractory metal molybdenum, with excellent elevated temperature strength, and its thermal coefficient of expansion is low, and thermal conductivity is good,
Meanwhile, molybdenum belongs to body-centered cubic structure, and copper belongs to face-centred cubic structure, and both objectionable interminglings are combined, and are made composite wood
Material, to integrate and keep relatively independent in both advantages, and each comfortable component, so as to can obtain the unexistent spy of homogenous material
Different performance；Also, programmable thermal coefficient of expansion can be reached and good led by changing the thickness ratio of copper-molybdenum carbon/carbon-copper composite material
Electrical conductivity energy.Copper-molybdenum copper three layer composite plate not only has the above performance, also with good processability and good
Elevated temperature strength.Therefore, it is used widely in electronic industry field.
With the continuous progress of science and technology, the development of electronic industry is advanced by leaps and bounds, to the demand of copper-molybdenum carbon/carbon-copper composite material
It is continuously increased.And compared with the materials such as molybdenum copper, tungsten copper, its low production cost, plane thermal conductivity is good, and consistency is high；Meanwhile,
Copper-molybdenum copper laminar composite material has in fields such as HB-LED, many substrate group plate materials, Electronic Packaging, heat sink material, Aero-Space
The prospect of being widely applied.
At present, the method for manufacture copper-molybdenum carbon/carbon-copper composite material mainly has：Roll-bonding method, explosion composite method, liquid-solid phase casting
Composite algorithm, reverse solidification method and laser surface deposition technology.But roll-bonding method one-time investment is larger, is unfavorable for small lot
Production, and Rolling compund edge is easy to crack；The danger of explosion composite method is higher, and the composite surface of production is second-rate,
Performance is difficult to meet use requirement；Liquid-solid phase Rolling compund, reverse solidification method and cladding laser surfaces technology are also in theoretical rank
Section, does not put into practice also.Therefore, be badly in need of it is a kind of be beneficial to actual production, and the good copper-molybdenum carbon/carbon-copper composite material of properties of product system
Preparation Method.
The content of the invention
It is an object of the invention to provide a kind of preparation method of copper-molybdenum copper multilayer materials, different materials interface cohesion is good
It is good, solve the problems, such as that Rolling compund edge is easy to crack.
The technical scheme that is used to achieve the above object of the present invention for：A kind of preparation side of copper-molybdenum copper multilayer materials
Method, comprises the following steps：
The pretreatment of step one, molybdenum plate and copper base
By pure molybdenum plate through wire cutting, the molybdenum plate of target size is processed into, copper coin base is processed into the copper of target size through wire cutting
Base, the molybdenum plate that then will be processed carries out surface polishing with water mill bed so that the roughness R on molybdenum plate surfacea≤ 10 μm, polish
Molybdenum plate and copper base cleaned with acetone respectively, remove surface contaminants；
The arrangement assembling of step 2, castingin sheet material
Crucible is taken, multiple strip-shaped clamp grooves, the length side of strip-shaped clamp groove are opened up on the wall of two for being oppositely arranged in crucible interior side
Extend at crucible opening to along crucible bottom；By in the strip-shaped clamp groove on the molybdenum plate insertion crucible internal walls after cleaning, then will
In strip-shaped clamp groove on the copper base insertion crucible internal walls of corresponding block number, make molybdenum plate spaced with copper base；
Step 3, heating castingin
Crucible is placed in vacuum furnace, copper base is heated to and is melted completely, and after being evenly distributed in crucible, be placed in vacuum and add
Cooled down in hot stove so that molybdenum plate is embedded in the copper base of thawing, multiple layer of copper composite material of molybdenum and copper strand is obtained；
Step 4, polishing finishing
The good multiple layer of copper composite material of molybdenum and copper strand of castingin is taken out from crucible, the unnecessary molybdenum plate in excision strand both sides, strand
Surface repairs smooth through milling machine, strand one end is polished with abrasive machine 30 ° of gradient, so as to stinging for follow-up rolling milling train
Enter；
Step 5, hot rolling and annealing heat-treats
The strand that polishing is trimmed is placed in the heating furnace of hydrogen shield, 500 ~ 800 DEG C are heated to, 10 ~ 60min is incubated, entered
After the hot rolling of row multi-pass, 400 ~ 800 DEG C are heated in the heating furnace of hydrogen shield atmosphere, make annealing treatment 0.5 ~ 5h, be obtained
Composite board；
Step 6, cold rolling and annealing heat-treats
Composite board after annealing is carried out into cold-rolling treatment, after being cold-rolled to required thickness, under the conditions of hydrogen shield, heating
To 200 ~ 600 DEG C, 30 ~ 60min is made annealing treatment, copper-molybdenum copper multilayer materials are obtained.
Wherein, the thickness of the pure molybdenum plate selected by step one of the invention is 0.5 ~ 2mm, and the thickness of copper coin base is 2 ~ 6mm.
Wherein, in step 2, the multilayer that the position of the strip-shaped clamp groove on molybdenum plate insertion crucible prepares according to needed for target is answered
Spacing between the molybdenum plate of condensation material determines.
Wherein, in step 2, after the completion of molybdenum plate is spaced with copper base, if space is left in crucible both sides, quadrel is used
Ink stick is filled space.
Preferably, step 2 of the present invention using cube structure crucible, the apparent size of crucible is wide × height × a length of 53mm
× 165mm × 230mm, wall thickness 15mm；Size it is wide × two inwalls of a height of 23mm × 165mm on, along the width side of inwall
A draw-in groove of wide × height × a length of 1mm × 150mm × 2mm is designed to every 1mm.The crucible of the size is mainly used to castingin molybdenum
The copper-molybdenum copper composite plate blanks of plate thickness≤1mm.
Preferably, step 2 of the present invention using cube structure crucible, the apparent size of crucible is wide × height × a length of 73mm
× 165mm × 230mm, wall thickness 15mm；Size it is wide × two inwalls of a height of 43mm × 165mm on, along the width side of inwall
A draw-in groove of wide × height × a length of 2mm × 150mm × 2mm is designed to every 1mm.The crucible of the size is mainly used to castingin molybdenum
The copper-molybdenum copper composite plate blanks of 1 ~ 2mm of plate thickness.
According to the crucible of both the above size, by the pure molybdenum plate in step one through wire cutting be cut into dimensional height ×
Length is：The pure molybdenum plate material of 150mm × 204mm；T2 red copper slab warps are cut into dimensional height × length and are：
The plate of 150mm × 200mm.
After the insertion assembling of castingin sheet material, because the difference of required slab thickness, castingin plate and crucible be high × size long
To have certain cavity between two medial surfaces of 165mm × 230mm.Therefore, different-thickness is prepared according to actual conditions
Quadrel ink stick, for filling cavity.Square graphite block size thickness × height × length is：Undetermined × 150mm × 200mm.
The crucible of present invention design can not meet for the crucible design of reusable edible, but some molybdenum copper product Thickness ratios,
Therefore the strip-shaped clamp groove of crucible madial wall can also be designed according to actual molybdenum copper product Thickness ratio.
Wherein, in step 3, crucible is placed in vacuum furnace, is heated to 1150 ~ 1300 DEG C, 2 ~ 3h of insulation to copper base
Melt completely；Vacuum furnace is cooled down with the cooldown rate of 1 ~ 3 DEG C/s.
Wherein, in step 5, the operation that strand carries out the hot rolling of multi-pass is：First passes deflection is 5%, rear several
Passage is using the deflection more than 5%.The first passage of rolling uses less rolling reduction, afterwards using larger deflection,
Certain size is rolled to, so that plate surface obtained in castingin and internal homogenising.
In the present invention, by the good draw-in groove of the molybdenum plate insertion castingin crucible design after cleaning, insertion position is with required preparation
The Thickness ratio of composite determine that molybdenum plate institute slot is put as far as possible in the draw-in groove of crucible middle part.
The method to castingin with crucible designed, by molybdenum plate be fixed on crucible interior design draw-in groove in, with protect
The stability and Cast-in Bonding slab Thickness ratio of molybdenum plate match with required composite plate blanks Thickness ratio during card castingin.
The present invention, is heated to copper by composite board under vacuum using the fusing point of the fusing point significantly lower than molybdenum of copper
More than fusing point so that copper base is melted completely.Then, cooled down with certain speed so that molybdenum plate castingin is passed through in the copper base of founding
Cross rolling and annealing heat-treats are obtained copper-molybdenum carbon/carbon-copper composite material of good performance, different materials interface cohesion is good, solves and rolls
The compound edge of system problem easy to crack.
Copper-molybdenum carbon/carbon-copper composite material prepared by the present invention is general more than three layers, and different materials interface cohesion is good, compares
Explosion composite method, improves the security of production process, also solves the problems, such as Rolling compund edge crack.Equipment requirement letter
It is single, low production cost, beneficial to small lot batch manufacture.
The method is designed crucible, molybdenum plate is fixed in the draw-in groove of crucible interior design, to ensure castingin mistake
In journey the stability of molybdenum plate and cause Cast-in Bonding slab Thickness ratio matched with required composite plate blanks Thickness ratio.
Be combined with each other for copper-molybdenum copper coin material using the method for castingin+rolling by the present invention, forms multi-layer compound structure,
And to castingin with crucible designed, improve copper-molybdenum copper thickness than accuracy.This method not only makes copper-molybdenum material
Material is closely combined with each other, and significantly enhances the bond strength of compound interface, meanwhile, copper-molybdenum copper composite board is led
Heat, conductive and coefficient of expansion controllability are all obviously improved.Castingin process is carried out under vacuum, it is to avoid castingin mistake
The problem of oxidation of journey compound interface, and the problem that copper liquid process of setting bubble is retained.
Brief description of the drawings
Fig. 1 is the stereogram of crucible；
Fig. 2 is the top view on strip-shaped clamp groove width surface where the strip-shaped clamp groove of the crucible of 1mm in Fig. 1；
Fig. 3 is strip-shaped clamp groove width inner surface profile where the strip-shaped clamp groove of the crucible of 1mm；
Fig. 4 is the top view on strip-shaped clamp groove width surface where the strip-shaped clamp groove of the crucible of 2mm in Fig. 1；
Fig. 5 is strip-shaped clamp groove width inner surface profile where the strip-shaped clamp groove of the crucible of 2mm.
In figure：1st, crucible；2nd, strip-shaped clamp groove.
Specific embodiment
A kind of preparation method of copper-molybdenum copper multilayer materials, comprises the following steps：
The pretreatment of step one, molybdenum plate and copper base
By pure molybdenum plate through wire cutting, the molybdenum plate of target size is processed into, copper coin base is processed into the copper of target size through wire cutting
Base, the molybdenum plate that then will be processed carries out surface polishing with water mill bed so that the roughness R on molybdenum plate surfacea≤ 10 μm, polish
Molybdenum plate and copper base cleaned with acetone respectively；Wherein, the thickness of selected pure molybdenum plate is 0.5 ~ 2mm, the thickness of copper coin base
It is 2 ~ 6mm to spend；
The arrangement assembling of step 2, castingin sheet material
Crucible is taken, multiple strip-shaped clamp grooves, the length side of strip-shaped clamp groove are opened up on the wall of two for being oppositely arranged in crucible interior side
Extend at crucible opening to along crucible bottom；By in the strip-shaped clamp groove on the molybdenum plate insertion crucible internal walls after cleaning, then will
In strip-shaped clamp groove on the copper base insertion crucible internal walls of corresponding block number, make molybdenum plate spaced with copper base；Molybdenum plate is alternate with copper base
After the completion of arrangement, if leaving space between crucible both sides inwall and copper base, space is filled using square graphite block.
Step 3, heating castingin
Crucible is placed in vacuum furnace, 1150 ~ 1300 DEG C are heated to, 2 ~ 3h of insulation to copper base melts completely, and in crucible
In be evenly distributed after, vacuum furnace is cooled down with the cooldown rate of 1 ~ 3 DEG C/s so that molybdenum plate is embedded in the copper base of thawing
In, multiple layer of copper composite material of molybdenum and copper strand is obtained；
Step 4, polishing finishing
The good multiple layer of copper composite material of molybdenum and copper strand of castingin is taken out from crucible, the unnecessary molybdenum plate in excision strand both sides, strand
Surface repairs smooth through milling machine, strand one end is polished with abrasive machine 30 ° of gradient, so as to stinging for follow-up rolling milling train
Enter；
Step 5, hot rolling and annealing heat-treats
The strand that polishing is trimmed is placed in the heating furnace of hydrogen shield, 500 ~ 800 DEG C are heated to, 10 ~ 60min is incubated, entered
After the hot rolling of row multi-pass, first passes deflection is 5%, and rear several passages are using the deflection more than 5%；Then in hydrogen
400 ~ 800 DEG C are heated in the heating furnace of protective atmosphere, 0.5 ~ 5h is made annealing treatment, composite board is obtained；
Step 6, cold rolling and annealing heat-treats
Composite board after annealing is carried out into cold-rolling treatment, after being cold-rolled to required thickness, under the conditions of hydrogen shield, heating
To 200 ~ 600 DEG C, 30 ~ 60min is made annealing treatment, copper-molybdenum copper multilayer materials are obtained.
With reference to specific embodiment, the invention will be further described, so that those skilled in the art can be more preferable
Understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine by any way.
Any feature disclosed in this specification (including any accessory claim, summary and accompanying drawing), except non-specifically is chatted
State, can alternative features equivalent by other or with similar purpose replaced.I.e., unless specifically stated otherwise, each feature
It is an example in a series of equivalent or similar characteristics.
The present invention is illustrated in conjunction with specific embodiments：
Embodiment 1：Selected molybdenum plate thickness is 1mm, and copper base thickness is 3mm.Production copper-molybdenum seven layers of composite of copper.
A kind of preparation method of copper-molybdenum copper multilayer materials of the present embodiment, comprises the following steps：
（1）, by technical pure molybdenum plate through wire cutting, be processed into the molybdenum plate of dimensional height × length=150mm × 204mm, T2 copper plates
Base is processed into the copper base of dimensional height × length=150mm × 200mm, the molybdenum plate that then will be processed water mill bed through wire cutting
Carry out surface polishing so that the roughness R on molybdenum plate surfacea≤ 10 μm, the molybdenum plate polished and copper base are carried out clearly with acetone respectively
Wash, remove surface contaminants；
（2）, take crucible, open up multiple strip-shaped clamp grooves, the length of strip-shaped clamp groove on the wall of two for being oppositely arranged in crucible interior side
Degree direction extends along crucible bottom at crucible opening；The molybdenum plate after three pieces of cleanings is chosen, insertion strip-shaped clamp groove width is 1mm
, from crucible from left to right number the 2nd, the 4th, in the strip-shaped clamp groove of the 6th, then choose the copper base insertion earthenware after four pieces of cleanings
Crucible, makes molybdenum plate spaced with copper base, and then the graphite square billet of rectangular shape is filled between copper base and crucible internal walls
In space, wherein, graphite square billet dimensional thickness × height × length=7mm × 150mm × 200mm；Using the earthenware of cube structure
Crucible, the apparent size of crucible is wide × height × length=53mm × 165mm × 230mm, wall thickness 15mm；Size it is wide × height=23mm ×
On two inwalls of 165mm, along the width of inwall every one wide × height × length=1mm × 150mm × 2mm's of 1mm designs
Draw-in groove；
（3）, the crucible that will assemble be placed in vacuum furnace, be heated to 1200 DEG C, 2h is incubated, to ensure that copper base is melted completely
Change, and be evenly distributed in crucible；After the completion of insulation, vacuum furnace is cooled down with the cooldown rate of 1 DEG C/s so that molybdenum
Plate is embedded in the copper base of founding, and seven layers of copper-molybdenum carbon/carbon-copper composite material strand are obtained；
（4）, by seven layers of good copper-molybdenum carbon/carbon-copper composite material strand of castingin, taken out from crucible, the unnecessary molybdenum plate in excision strand both sides,
Surface repairs smooth through milling machine, strand one end is polished with abrasive machine 30 ° of gradient, so as to stinging for follow-up rolling milling train
Enter；
（5）, the strand that will trim be placed in the heating furnace of hydrogen shield, be heated to 600 DEG C, be incubated 20min, carry out hot rolling,
Be rolled to 5mm through five passages, first passes deflection is 5%, and rear four-pass uses larger deflection, successively using 10%,
30%th, 28%, 23% deflection, after the completion of rolling, in hydrogen shield heating furnace, is heated to 500 DEG C, makes annealing treatment 0.5h, system
Obtain composite board；
（6）, hot-roll annealing is processed after composite board, carry out cold-rolling treatment, be rolled to 2mm；After the completion of rolling, in hydrogen shield
Under the conditions of, 300 DEG C are heated to, make annealing treatment 40min.
Embodiment 2：Selected molybdenum plate thickness is 1.5mm, and copper base thickness is 4.5mm.Produce two groups of five layers of copper-molybdenum copper multiple
Condensation material.
A kind of preparation method of copper-molybdenum copper multilayer materials of the present embodiment, comprises the following steps：
（1）, by technical pure molybdenum plate through wire cutting, be processed into the molybdenum plate of dimensional height × length=150mm × 204mm, T2 copper plates
Base is processed into the copper base of dimensional height × length=150mm × 200mm, the molybdenum plate that then will be processed water mill bed through wire cutting
Carry out surface polishing so that the roughness R on molybdenum plate surfacea≤ 10 μm, the molybdenum plate polished and copper base are carried out clearly with acetone respectively
Wash, remove surface contaminants；
（2）, take crucible, open up multiple strip-shaped clamp grooves, the length of strip-shaped clamp groove on the wall of two for being oppositely arranged in crucible interior side
Degree direction extends along crucible bottom at crucible opening；The molybdenum plate after four pieces of cleanings is chosen, insertion width is the strip-shaped clamp groove of 2mm
In, insertion position is：In the 2nd from left to right, crucible, the 4th strip-shaped clamp groove, another the 2nd from right to left, the 4th, two pieces of insertion castingins crucible
In strip-shaped clamp groove；Then choose in the strip-shaped clamp groove of the copper base insertion crucible after six pieces of cleanings, molybdenum plate is spaced with copper base, will
Graphite square billet is filled into two groups of cavitys being located between crucible most inner side copper base, wherein, graphite square billet dimensional thickness × height
× length=10mm × 150mm × 200mm；Using the crucible of cube structure, the apparent size of crucible is wide × height × a length of 73mm ×
165mm × 230mm, wall thickness 15mm；Size it is wide × two inwalls of a height of 43mm × 165mm on, along the width of inwall
A draw-in groove of wide × height × a length of 2mm × 150mm × 2mm is designed every 1mm.
（3）, the crucible that will assemble be placed in vacuum furnace, be heated to 1300 DEG C, 2.5h is incubated, to ensure that copper base is complete
It is complete to melt, and be evenly distributed in crucible；After the completion of insulation, vacuum furnace is cooled down with the cooldown rate of 2 DEG C/s, made
Obtain molybdenum plate to be embedded in the copper base of founding, two groups of five layers of copper-molybdenum carbon/carbon-copper composite material strands are obtained；
（4）, by two groups of good five layers of copper-molybdenum carbon/carbon-copper composite material strands of castingin, taken out from crucible, excision strand both sides are unnecessary
Molybdenum plate, surface repairs smooth through milling machine, strand one end is polished with abrasive machine 30 ° of gradient, so as to follow-up rolling milling train
Nip；
（5）, the strand that will trim be placed in the heating furnace of hydrogen shield, be heated to 800 DEG C, be incubated 60min, carry out hot rolling,
Be rolled to 5mm through five passages, first passes deflection is 5%, and rear four-pass uses larger deflection, successively using 17%,
30%th, 28%, 23% deflection, after the completion of rolling, in hydrogen shield heating furnace, is heated to 400 DEG C, makes annealing treatment 5h, is obtained
Composite board；
（6）, hot-roll annealing is processed after composite board, carry out cold-rolling treatment, be rolled to 2mm；After the completion of rolling, in hydrogen shield
Under the conditions of, 600 DEG C are heated to, make annealing treatment 30min.
Embodiment 3：Selected molybdenum plate thickness is 0.5mm, and copper base thickness is 2mm.Production copper-molybdenum five layers of composite of copper.
A kind of preparation method of copper-molybdenum copper multilayer materials of the present embodiment, comprises the following steps：
（1）, by technical pure molybdenum plate through wire cutting, be processed into the molybdenum plate of dimensional height × length=150mm × 204mm, T2 copper plates
Base is processed into the copper base of dimensional height × length=150mm × 200mm, the molybdenum plate that then will be processed water mill bed through wire cutting
Carry out surface polishing so that the roughness R on molybdenum plate surfacea≤ 10 μm, the molybdenum plate polished and copper base are carried out clearly with acetone respectively
Wash, remove surface contaminants；
（2）, take crucible, open up multiple strip-shaped clamp grooves, the length of strip-shaped clamp groove on the wall of two for being oppositely arranged in crucible interior side
Degree direction extends along crucible bottom at crucible opening；The molybdenum plate after four pieces of cleanings is chosen, insertion strip-shaped clamp groove width is 1mm
, from crucible from left to right number the 3rd, the strip-shaped clamp groove of the 4th, the 3rd from right to left, another two pieces of insertion crucibles, the bar shaped card of the 4th
In groove；Then the copper base after six pieces of cleanings is chosen, the same side of every three pieces of insertion crucibles makes molybdenum plate spaced with copper base, so
The graphite square billet of rectangular shape is filled into the space between copper base and crucible internal walls afterwards, wherein, graphite square billet size is thick
Degree × height × length=3mm × 150mm × 200mm（It is placed in the both sides of cube structure crucible）Two pieces and 4mm × 150mm ×
200mm（It is placed in the center of cube structure crucible）One piece；Using the crucible of cube structure, the apparent size of crucible is wide × and it is high × long
=53mm × 165mm × 230mm, wall thickness 15mm；Size it is wide × two inwalls of height=23mm × 165mm on, along the width of inwall
A draw-in groove of wide × height × length=1mm × 150mm × 1mm is designed every 1mm in degree direction；
（3）, the crucible that will assemble be placed in vacuum furnace, be heated to 1150 DEG C, 3h is incubated, to ensure that copper base is melted completely
Change, and be evenly distributed in crucible；After the completion of insulation, vacuum furnace is cooled down with the cooldown rate of 3 DEG C/s so that molybdenum
Plate is embedded in the copper base of founding, and two groups of five layers of copper-molybdenum carbon/carbon-copper composite material strands are obtained；
（4）, by two groups of good five layers of copper-molybdenum carbon/carbon-copper composite material strands of castingin, taken out from crucible, excision strand both sides are unnecessary
Molybdenum plate, surface repairs smooth through milling machine, strand one end is polished with abrasive machine 30 ° of gradient, so as to follow-up rolling milling train
Nip；
（5）, the strand that will trim be placed in the heating furnace of hydrogen shield, be heated to 500 DEG C, be incubated 35min, carry out hot rolling,
4mm is rolled to through three passages, every time deflection is 5% → 19% → 20%, after the completion of rolling, in hydrogen shield heating furnace, plus
Heat makes annealing treatment 2h to 600 DEG C, and composite board is obtained；
（6）, hot-roll annealing is processed after composite board, carry out cold-rolling treatment, be rolled to 2mm；After the completion of rolling, in hydrogen shield
Under the conditions of, 400 DEG C are heated to, make annealing treatment 60min.
Embodiment 4：Selected molybdenum plate thickness is 2mm, and copper base thickness is 6mm.Production copper-molybdenum copper 3-layer composite material.
A kind of preparation method of copper-molybdenum copper multilayer materials of the present embodiment, comprises the following steps：
（1）, by technical pure molybdenum plate through wire cutting, be processed into the molybdenum plate of dimensional height × length=150mm × 204mm, T2 copper plates
Base is processed into the copper base of dimensional height × length=150mm × 200mm, the molybdenum plate that then will be processed water mill bed through wire cutting
Carry out surface polishing so that the roughness R on molybdenum plate surfacea≤ 10 μm, the molybdenum plate polished and copper base are carried out clearly with acetone respectively
Wash, remove surface contaminants；
（2）, take crucible, open up multiple strip-shaped clamp grooves, the length of strip-shaped clamp groove on the wall of two for being oppositely arranged in crucible interior side
Degree direction extends along crucible bottom at crucible opening；The molybdenum plate after two pieces of cleanings is chosen, insertion strip-shaped clamp groove width is 2mm
, one of insertion from the crucible from left to right strip-shaped clamp groove of number the 4th, another piece of insertion crucible the 4th strip-shaped clamp groove from right to left
In；Then the copper base insertion crucible after four pieces of cleanings is chosen, makes molybdenum plate spaced with copper base, then by the stone of rectangular shape
Black square billet is filled into the space between copper base and crucible internal walls, wherein, graphite square billet dimensional thickness × height × length=4mm
×150mm×200mm（It is placed in the both sides of cube structure crucible）2 pieces and 7mm × 150mm × 200mm（It is placed in cube structure crucible
Center）1 piece；Using the crucible of cube structure, the apparent size of crucible is wide × height × length=73mm × 165mm × 230mm, wall
Thick 15mm；Size it is wide × two inwalls of height=43mm × 165mm on, along inwall width every 1mm design one it is wide
The draw-in groove of × height × length=1mm × 150mm × 2mm；
（3）, the crucible that will assemble be placed in vacuum furnace, be heated to 1300 DEG C, 2h is incubated, to ensure that copper base is melted completely
Change, and be evenly distributed in crucible；After the completion of insulation, vacuum furnace is cooled down with the cooldown rate of 1 DEG C/s so that molybdenum
Plate is embedded in the copper base of founding, and two groups of three layers of copper-molybdenum carbon/carbon-copper composite material strands are obtained；
（4）, by two groups of good three layers of copper-molybdenum carbon/carbon-copper composite material strands of castingin, taken out from crucible, excision strand both sides are unnecessary
Molybdenum plate, surface repairs smooth through milling machine, strand one end is polished with abrasive machine 30 ° of gradient, so as to follow-up rolling milling train
Nip；
（5）, the strand that will trim be placed in the heating furnace of hydrogen shield, be heated to 700 DEG C, be incubated 10min, carry out hot rolling,
5mm is rolled to through five passages, every time deflection is followed successively by 5% → 15% → 20% → 28% → 23%, after the completion of rolling, is protected in hydrogen
In shield heating furnace, 800 DEG C are heated to, make annealing treatment 5h, composite board is obtained；
（6）, hot-roll annealing is processed after composite board, carry out cold-rolling treatment, be rolled to 2mm；After the completion of rolling, in hydrogen shield
Under the conditions of, 200 DEG C are heated to, make annealing treatment 50min.
Four embodiments of the above are prepared for seven layers, five layers, five layers and three layers copper-molybdenum carbon/carbon-copper composite material respectively, and embodiment 2,
Embodiment 3 and embodiment 4 are prepared for two blocks of copper-molybdenum copper composite boards inside a crucible, show the crucible designed by the present invention
Can be according to required different plates thickness, during template inserted into corresponding strip-shaped clamp groove, so that the number of plies needed for castingin and thickness ratio
Copper-molybdenum copper composite board.For three layers and five layers of composite board can at least produce 1 according to required thickness in a crucible
Block.
Laminar composite prepared by the present invention is mainly used in Electronic Packaging and heat sink material field.
The embodiment selected herein for the open purpose of the present invention, is presently considered to be suitable, but answer
Solution, it is contemplated that all changes for belonging to the embodiment in this design and the scope of the invention including all and improvement.
Claims (8)
1. a kind of preparation method of copper-molybdenum copper multilayer materials, it is characterised in that comprise the following steps：
The pretreatment of step one, molybdenum plate and copper base
By pure molybdenum plate through wire cutting, the molybdenum plate of target size is processed into, copper coin base is processed into the copper of target size through wire cutting
Base, the molybdenum plate that then will be processed carries out surface polishing with water mill bed so that the roughness R on molybdenum plate surfacea≤ 10 μm, polish
Molybdenum plate and copper base cleaned with acetone respectively；
The arrangement assembling of step 2, castingin sheet material
Crucible is taken, multiple strip-shaped clamp grooves, the length side of strip-shaped clamp groove are opened up on the wall of two for being oppositely arranged in crucible interior side
Extend at crucible opening to along crucible bottom；By in the strip-shaped clamp groove on the molybdenum plate insertion crucible internal walls after cleaning, then will
In strip-shaped clamp groove on the copper base insertion crucible internal walls of corresponding block number, make molybdenum plate spaced with copper base；
Step 3, heating castingin
Crucible is placed in vacuum furnace, copper base is heated to and is melted completely, and after being evenly distributed in crucible, be placed in vacuum and add
Cooled down in hot stove so that molybdenum plate is embedded in the copper base of thawing, multiple layer of copper composite material of molybdenum and copper strand is obtained；
Step 4, polishing finishing
The good multiple layer of copper composite material of molybdenum and copper strand of castingin is taken out from crucible, the unnecessary molybdenum plate in excision strand both sides, strand
Surface repairs smooth through milling machine, strand one end is polished with abrasive machine 30 ° of gradient, so as to stinging for follow-up rolling milling train
Enter；
Step 5, hot rolling and annealing heat-treats
The strand that polishing is trimmed is placed in the heating furnace of hydrogen shield, 500 ~ 800 DEG C are heated to, 10 ~ 60min is incubated, entered
After the hot rolling of row multi-pass, 400 ~ 800 DEG C are heated in the heating furnace of hydrogen shield atmosphere, make annealing treatment 0.5 ~ 5h, be obtained
Composite board；
Step 6, cold rolling and annealing heat-treats
Composite board after annealing is carried out into cold-rolling treatment, after being cold-rolled to required thickness, under the conditions of hydrogen shield, heating
To 200 ~ 600 DEG C, 30 ~ 60min is made annealing treatment, copper-molybdenum copper multilayer materials are obtained.
2. the preparation method of a kind of copper-molybdenum copper multilayer materials according to claim 1, it is characterised in that：Step one institute
The thickness of the pure molybdenum plate selected is 0.5 ~ 2mm, and the thickness of copper coin base is 2 ~ 6mm.
3. the preparation method of a kind of copper-molybdenum copper multilayer materials according to claim 1, it is characterised in that：Step 2
In, between the molybdenum plate of multilayer materials that the position of the strip-shaped clamp groove on molybdenum plate insertion crucible prepares according to needed for target between
Away from determination.
4. the preparation method of a kind of copper-molybdenum copper multilayer materials according to claim 1, it is characterised in that：Step 2
In, after the completion of molybdenum plate is spaced with copper base, if space is left in crucible both sides, space is filled using square graphite block.
5. the preparation method of a kind of copper-molybdenum copper multilayer materials according to claim 1, it is characterised in that：Step 2 is adopted
With the crucible of cube structure, the apparent size of crucible is wide × height × a length of 53mm × 165mm × 230mm, wall thickness 15mm；In size
On two inwalls of width × a height of 23mm × 165mm, the width along inwall is wide × high × a length of every 1mm designs one
The draw-in groove of 1mm × 150mm × 2mm.
6. the preparation method of a kind of copper-molybdenum copper multilayer materials according to claim 1, it is characterised in that：Step 2 is adopted
With the crucible of cube structure, the apparent size of crucible is wide × height × a length of 73mm × 165mm × 230mm, wall thickness 15mm；In size
On two inwalls of width × a height of 43mm × 165mm, the width along inwall is wide × high × a length of every 1mm designs one
The draw-in groove of 2mm × 150mm × 2mm.
7. the preparation method of a kind of copper-molybdenum copper multilayer materials according to claim 1, it is characterised in that：Step 3
In, crucible is placed in vacuum furnace, 1150 ~ 1300 DEG C are heated to, 2 ~ 3h of insulation to copper base melts completely；By heating in vacuum
Stove is cooled down with the cooldown rate of 1 ~ 3 DEG C/s.
8. the preparation method of a kind of copper-molybdenum copper multilayer materials according to claim 1, it is characterised in that：Step 5
In, the operation that strand carries out the hot rolling of multi-pass is：First passes deflection is 5%, and rear several passages are using the change more than 5%
Shape amount.
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| CN113664063A (en) * | 2021-08-26 | 2021-11-19 | 西安航空学院 | Preparation method of copper-molybdenum-copper laminated composite material |
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Application publication date: 20170613 |