CN103706797B - The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite - Google Patents
The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite Download PDFInfo
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- CN103706797B CN103706797B CN201310738226.7A CN201310738226A CN103706797B CN 103706797 B CN103706797 B CN 103706797B CN 201310738226 A CN201310738226 A CN 201310738226A CN 103706797 B CN103706797 B CN 103706797B
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Abstract
The preparation method of broad-width multi-layer Cu CuMo70 Cu composite, pretreated CuMo70 sheet material is put in a mold, then CuNi10 material and surface-treated Cu material are together placed in graphite crucible, graphite crucible is placed on mould and is placed on together in vacuum sintering furnace and carry out insulation after melting infiltration sintering, finally remove unnecessary Cu, multi-pass rolling and get final product at 650 900 DEG C.Preparation method of the present invention, utilize Ni metal and CuMo70 alloy difference on the coefficient of expansion and fusing point, between Cu and CuMo70, add appropriate third element CuNi10 material realize the metallurgical binding of both high intensity, through vacuum high-temperature sintering and Slow cooling, the double metallic composite material formed is in addition to having the respective feature performance benefit of Ni metal and CuMo70 alloy, the most also having higher bond strength, its interface bond strength is up to more than 200Mpa.
Description
Technical field
The invention belongs to technical field of composite preparation, relate to a kind of broad-width multi-layer Cu-CuMo70-Cu
The preparation method of composite.
Background technology
Copper (Cu) has high conduction, heat conductivility, and copper molybdenum alloy (CuMo70) has low heat
The advantages such as the coefficient of expansion, high intensity, low remanent magnetism rate, if leading to two kinds of dissimilar materials of Cu with CuMo70
The method crossing special material molding links together, and is prepared as many stratiforms of a kind of high comprehensive performance
Cu-CuMo70-Cu heterogeneous material compound, it will the collaborative performance respective feature performance benefit of both materials,
Realizing structure-function integration, it is used widely as heat sink or electronic package material, at micro-electricity
Son and other field aspect also have wide practical use.
At present, grade and submillimeter level can be obtained by cold rolling owing to copper has good ductility
Copper Foil, but the coefficient of expansion of copper is higher, easily deforms when being heated or cool down, it is impossible to directly
As encapsulating material.CuMo70 alloy can use the method such as hot isostatic pressing method, infiltration method to prepare, but logical
It is commonly used for block materials, it is possible to use the method for hot rolling to obtain grade sheet material.Report has by heat
Pressing method, die pressing prepare Cu-Mo-Cu composite, but due to Cu Yu Mo bond strength
Relatively low, often there is the defect such as cracking, deformation to produce in the operation of rolling preparing Cu-Mo-Cu thin plate, lead
Cause can not prepare wide cut large scale multi-layer C u-Mo-Cu composite；In order to obtain wide cut of good performance
Multilayer materials, the present invention uses the CuMo70 with certain plastic deformation ability to replace Mo to prepare
Multi-layer C u-CuMo70-Cu composite, for the Cu-CuMo70-Cu composite wood mentioned in the present invention
Material and preparation method thereof there is presently no report.
Summary of the invention
It is an object of the invention to provide the preparation side of a kind of broad-width multi-layer Cu-CuMo70-Cu composite
Method, solves in the operation of rolling of existing Cu-Mo-Cu thin plate and often has the defect such as cracking, deformation to produce,
The problem causing preparing wide cut large scale multi-layer C u-Mo-Cu composite.
The technical solution adopted in the present invention is, the preparation of broad-width multi-layer Cu-CuMo70-Cu composite
Method, puts in a mold by pretreated CuMo70 sheet material, then by CuNi10 material and surface
The Cu material processed together is placed in graphite crucible, is placed in by graphite crucible on mould and together
It is placed in vacuum sintering furnace after carrying out melting infiltration sintering and is incubated, finally remove unnecessary Cu, at 650～900 DEG C
Lower multi-pass rolling, i.e. obtains broad-width multi-layer Cu-CuMo70-Cu composite.
The feature of the present invention also resides in,
After melting infiltration sintering, insulation is to carry out in ZRS-18Q type micro-computer controlled vacuum high-temperature sintering stove, tool
Body operating process is: first micro-computer controlled to ZRS-18Q type vacuum high-temperature sintering stove evacuation, takes seriously
Reciprocal of duty cycle reaches 3.0 × 10-3Pa～9.0 × 10-3Beginning to warm up sintering 40～80min after Pa, temperature reaches
1100～1200 DEG C, it is incubated 0.5～3h, treats that Cu liquid fully flows into mould and realizes boundary with CuMo70 sheet material
Face fully spread after furnace cooling.
The addition of CuNi10 material is determined according to the surface area of CuMo70 sheet material, i.e. 100～
500g/m2。
The pretreatment of CuMo70 sheet material be with 75% phosphoric acid in CuMo70 plate surface electrolytic etching 1～
3min。
The surface of Cu material processes the oxide skin being to rinse Cu material surface residual with gasoline, then uses ethanol
Clean the greasy dirt remaining in Cu material surface.
The invention has the beneficial effects as follows, the preparation of broad-width multi-layer Cu-CuMo70-Cu composite of the present invention
Method, utilizes Ni metal and CuMo70 alloy difference on the coefficient of expansion and fusing point, Cu with
Add appropriate third element CuNi10 material between CuMo70 and realize the metallurgical binding of both high intensity,
Processing through vacuum high-temperature sintering and Slow cooling, the double metallic composite material of formation is except having metal
Outside the respective superior function of Cu and CuMo70 alloy, the most also there is higher bond strength, its boundary
Face bond strength is up to more than 200Mpa, it is achieved structure-function integration.
Accompanying drawing explanation
Fig. 1 is the process chart of the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite；
Fig. 2 is the die cut view that embodiment 2 prepares used by 7 layers of Cu-CuMo70-Cu.
In figure, 1.CuMo70 sheet material, 2.7 layers of dissimilar materials mould.
Detailed description of the invention
The present invention is described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite of the present invention, by pretreated
CuMo70 sheet material is put in a mold, then by CuNi10 material and surface-treated Cu material together
It is placed in graphite crucible, graphite crucible is placed on mould and is placed on together in vacuum sintering furnace and carry out
It is incubated after melting infiltration sintering, finally removes unnecessary Cu, multi-pass rolling at 650～900 DEG C, to obtain final product.
Technological process as shown in Figure 1, specifically implements according to following steps:
Step 1, Design of Dies and raw-material preparation
Number of plies design mould according to multilayer materials, and add according to the geomery machinery of mould therefor
Work CuMo70 sheet material；Cu material needed for the number of plies according to multilayer materials and the Size calculation of mould
Weight；
Step 2, Cu Yu CuMo70 plate surface processes
First, rinse the oxide skin of Cu material surface residual with gasoline, then remain in Cu with alcohol washes
The greasy dirt of material surface；CuMo70 plate surface is carried out the electrolytic etching 1～3min of 75% phosphoric acid；
Step 3, under vacuum condition, high temperature sintering and interface diffusion connect
The CuMo70 sheet material of step 2 pretreatment is placed in a mold；By CuNi10 material (CuNi10
The addition of material is determined according to the surface area of CuMo70 sheet material, i.e. 100～500g/m2) and table
The Cu material that face processed together is placed in graphite crucible, and graphite crucible is placed on mould and together
Being placed in vacuum sintering furnace, whole process is complete in ZRS-18Q type micro-computer controlled vacuum high-temperature sintering stove
Becoming, in order to prevent from occurring on interface oxide, first micro-computer controlled to ZRS-18Q type vacuum high-temperature burns
Freezing of a furnace evacuation, when in sintering furnace, vacuum reaches 3.0 × 10-3Pa～9.0 × 10-3Burning is begun to warm up after Pa
Tie 40～80 minutes, be incubated 0.5～3h after heating-up temperature to 1100～1200 DEG C, treat that Cu liquid flows completely
Enter mould and CuMo70 and realize after interface fully spreads, furnace cooling, it is thus achieved that multilamellar
Cu-CuMo70-Cu composite blank；
Step 4, multi-layer C u-CuMo70-Cu composite blank step 3 obtained carries out machinery and adds
Work, removes unnecessary Cu, and multi-pass rolling at 650～900 DEG C i.e. obtains broad-width multi-layer
Cu-CuMo70-Cu composite.
CuNi10 material is as intermediate alloy, and Ni element therein all has necessarily in the middle of Cu Yu Mo
Solid solubility, prepare Cu-CuMo70-Cu composite time add can improve Cu Yu CuMo70 plate
Interface bond strength between material.
The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite of the present invention, utilize Ni metal with
The difference that CuMo70 alloy is fastened in expansion, adds appropriate third element between Cu and CuMo70
CuNi10 material realizes the metallurgical binding of both high intensity, through vacuum high-temperature sintering and annealing,
The double metallic composite material formed is in addition to having the respective performance of Ni metal and CuMo70 alloy, same
Time also there is higher bond strength, its interface bond strength is up to more than 200Mpa, it is achieved structure merit
Can integration.
Cu-CuMo70-Cu composite bond strength prepared by the present invention is high, also substantially reduces
CuMo70 and Cu resistance of deformation difference is uneven compared with the deformation caused greatly, and then rolling is reduced or eliminated
Rear material thickness is than uneven phenomenon, and its preparation technology is simple and reliable, environmental protection.
Embodiment 1
In order to prepare 3 layers of Cu-CuMo70-Cu composite, design has the dissimilar materials molding that haves three layers
Mould, maching dimension is the CuMo70 plate 1 of 100mm × 100mm × 3mm, prepares size
Size is the T2 pure Cu material of Φ 48mm × 198mm；
Rinse the oxide skin of Cu material surface residual with gasoline, then remain in Cu material with alcohol washes
The greasy dirt on surface；CuMo70 plate surface is carried out the electrolytic etching 1min of 75% phosphoric acid；
CuMo70 sheet material is placed on the intermediate layer in 3 layers of dissimilar materials mould, by surface-treated
Cu material put into graphite crucible, and add 10 grams of CuNi10 materials, graphite crucible wherein
It is placed on mould and puts into ZRS-18Q type micro-computer controlled vacuum high-temperature sintering stove, micro-to ZRS-18Q type
Machine program control vacuum high-temperature sintering stove evacuation, when in sintering furnace, vacuum reaches 3.0 × 10-3Start after Pa to add
Thermal sintering 40 minutes, heating-up temperature to 1200 DEG C, it is incubated 0.5 hour, treats that Cu liquid fully flows into mould
Realize after interface fully spreads with CuMo70 plate, furnace cooling, it is thus achieved that the number of plies is 3 layers
Cu-CuMo70-Cu composite blank；
3 layers of Cu-CuMo70-Cu composite blank are carried out machining, remove unnecessary Cu,
Carry out rolling at 650 DEG C and obtain 3 layers of Cu-CuMo70-Cu composite board of wide cut, after rolling
Cu-CuMo70-Cu composite board thickness is 1mm, and wherein CuMo70 thickness is about 0.8mm,
Both sides Cu thickness is about 0.1mm.
Embodiment 2
In order to prepare 7 layers of Cu-CuMo70-Cu composite, design have as shown in Figure 27 layers heterogeneous
The mould 2 of material molding, maching dimension is the CuMo70 plate 3 of 100mm × 100mm × 1mm
, prepare the T2 pure Cu material that size is Φ 48mm × 172mm；
Rinse the oxide skin of Cu material surface residual with gasoline, then remain in Cu material with alcohol washes
The greasy dirt on surface；CuMo70 plate surface is carried out the electrolytic etching 2min of 75% phosphoric acid；
The CuMo70 sheet material 1 of pretreatment is placed on the even level in 7 layers of dissimilar materials mould 2,
The Cu material carrying out surface process is put into graphite crucible, and adds 30 grams of CuNi10 materials wherein
Material, graphite crucible is placed on mould puts into ZRS-18Q type micro-computer controlled vacuum high-temperature sintering stove, right
ZRS-18Q type micro-computer controlled vacuum high-temperature sintering stove evacuation, when in sintering furnace vacuum reach 6.0 ×
10-3Pa post-heating sinters 60 minutes, and heating-up temperature to 1150 DEG C is incubated 2 hours, treats that Cu liquid is complete
Flow into mould and CuMo70 plate and realize after interface fully spreads, furnace cooling, it is thus achieved that total number of plies is 7
The Cu-CuMo70-Cu composite blank of layer (4 layers of Cu and 3 layers of CuMo70)；
7 layers of Cu-CuMo70-Cu composite blank are carried out machining, removes both sides unnecessary
Cu, carries out 4 passes at 800 DEG C and obtains 7 layers of Cu-CuMo70-Cu composite board of wide cut,
Cu-CuMo70-Cu composite board thickness after rolling is 2.2mm, wherein 3 layers of CuMo70 thickness
Degree is about 0.4mm, and middle two-layer Cu thickness is about 0.4mm, and both sides Cu thickness is about 0.1mm.
Embodiment 3
In order to prepare 13 layers of Cu-CuMo70-Cu composite, design has 13 layers of dissimilar materials molding
Mould, maching dimension is the CuMo70 plate 6 of 100mm × 100mm × 0.8mm, prepare
Size is the T2 pure Cu material of Φ 48mm × 132mm；
Rinse the oxide skin of Cu material surface residual with gasoline, then remain in Cu material with alcohol washes
The greasy dirt on surface；CuMo70 plate surface is carried out the electrolytic etching 3min of 75% phosphoric acid；
The CuMo70 sheet material of pretreatment is placed on the even level in 13 layers of dissimilar materials mould, will
Graphite crucible put into by the Cu material that surface processes, and adds 60 grams of CuNi10 materials, stone wherein
Ink crucible is placed on mould puts into ZRS-18Q type micro-computer controlled vacuum high-temperature sintering stove, to ZRS-18Q
Type micro-computer controlled vacuum high-temperature sintering stove evacuation, when in sintering furnace, vacuum reaches 9 × 10-3Add after Pa
Thermal sintering 80 minutes, heating-up temperature to 1100 DEG C, it is incubated 3 hours, treats that Cu liquid fully flows into mould
Realize after interface fully spreads with CuMo70 plate, furnace cooling, it is thus achieved that the number of plies is 13 layers
Cu-CuMo70-Cu composite；
13 layers of Cu-CuMo70-Cu composite blank are carried out machining, removes both sides unnecessary
Cu, carries out 6 passes at 900 DEG C and obtains 13 layers of Cu-CuMo70-Cu composite board of wide cut.
Cu-CuMo70-Cu composite board thickness after rolling is 4.8mm, wherein 6 layers of CuMo70 thickness
Degree is about 0.4mm, and middle 5 layers of Cu thickness are about 0.4mm, and both sides Cu thickness is about 0.2mm.
Claims (3)
1. the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite, it is characterised in that by pretreatment
The CuMo70 sheet material crossed is placed on the even level in the mould with 7 layers or 13 layers dissimilar materials molding, so
After CuNi10 material and surface-treated Cu material are together placed in graphite crucible；By graphite earthenware
Crucible is placed on mould and is placed on together in vacuum sintering furnace and carries out insulation after melting infiltration sintering, finally removes many
Remaining Cu, multi-pass rolling at 800-900 DEG C, i.e. obtain broad-width multi-layer Cu-CuMo70-Cu and be combined
Material, the number of plies is 7 layers or 13 layers；
Wherein, after melting infiltration sintering, insulation is to carry out in ZRS-18Q type micro-computer controlled vacuum high-temperature sintering stove,
Specific operation process is: first micro-computer controlled to ZRS-18Q type vacuum high-temperature sintering stove evacuation, takes seriously
Reciprocal of duty cycle reaches 6.0 × 10-3Pa～9.0 × 10-3Beginning to warm up sintering 60～80min after Pa, temperature reaches
1100～1150 DEG C, it is incubated 2～3h, treats that Cu liquid fully flows into mould and realizes interface with CuMo70 sheet material
Fully furnace cooling after diffusion.
The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite the most according to claim 1,
It is characterized in that, the addition of CuNi10 material is determined according to the surface area of CuMo70 sheet material, i.e.
100-500g/m2。
The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite the most according to claim 1,
It is characterized in that, the pretreatment of CuMo70 sheet material is to be electrolysed at CuMo70 plate surface with 75% phosphoric acid
Corrosion 1～3min.
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| CN104588646A (en) * | 2014-12-30 | 2015-05-06 | 天龙钨钼（天津）有限公司 | Method for preparing CPC layered composite materials and CPC layered composite materials |
| CN105033226B (en) * | 2015-07-09 | 2017-01-25 | 西安理工大学 | Preparing method for CuW/Al bimetallic material of porous structure blocking layer |
| CN108702847B (en) * | 2016-02-18 | 2021-03-09 | 三井金属矿业株式会社 | Copper foil for manufacturing printed wiring board, copper foil with carrier, copper-clad laminate, and method for manufacturing printed wiring board using same |
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