CN106695043A - Carbon base material and copper brazing connection method - Google Patents
Carbon base material and copper brazing connection method Download PDFInfo
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- CN106695043A CN106695043A CN201611198639.0A CN201611198639A CN106695043A CN 106695043 A CN106695043 A CN 106695043A CN 201611198639 A CN201611198639 A CN 201611198639A CN 106695043 A CN106695043 A CN 106695043A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
- B23K1/203—Fluxing, i.e. applying flux onto surfaces
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Abstract
The invention belongs to the technical field of material connection, and relates to a carbon base material and copper brazing connection method. The method is realized through the following steps: firstly, a layer of chromium metal slurry is brushed on the surface of a carbon base material through a silk screen printing method, and is sintered in vacuum at high temperature after drying to metallize the surface of the carbon base material; then, a layer of anaerobic pure copper is poured on the metallized surface of the carbon base material at a pouring temperature of 1150-1200 DEG C, and the segmented insulation cooling is perfomred after the pouring is finished; and finally, a pure copper carbon base material and a copper alloy material are poured by using Cu-P base brazing filler metal vacuum brazing at a brazing temperature of 700-800 DEG C. The method metallizes the surface of the carbon base material by using a slurry method to increase wettability of copper and carbon, can effectively reduce internal stress caused by thermal expansion coefficient difference between the carbon base material and the anaerobic pure copper through segmented insulation cooling, can effectively weakens such problems as copper alloy grain growth and performance reduction, and is high in efficiency, suitable for large-scale production and free of such defects as holes, inclusions and cracks.
Description
Technical field
The invention belongs to Material Joining Technology field, it is related to the soldering connecting method of a kind of carbon-based material and copper.
Background technology
Due to the excellent performance of carbon-based material (CFC and graphite), make it in nuclear fusion device as towards plasma
The usage history of body material existing decades.Domestic and international most fusion facility, such as external TFTR, DIII-D, JT-
60U, JET, Tore Supra, W7-X, domestic HL-2A, HT-7 etc. all employ carbon-based material (including graphite and CFC) conduct
First wall and divertor, the divertor vertical target Board position that ITER also once devised in the stage of bringing into operation are combined using C/C
Material.
Fusion facility divertor position due to thermic load it is higher, it is necessary to by carbon-based material combined with heat sink material copper alloy with
Constitute divertor part.Carbon-based material mainly includes bonding, mechanical connection, welding etc. with the connected mode of copper alloy.Due to
The fragility of carbon material, many inconvenience are brought at aspects such as manufacture, connections, and most simple and practical method is that machinery is carried out with bolt even
Connect, the intensity of joint depends primarily on the intensity of screwed joint.
In order to ensure between carbon and copper alloy have good heat conductivility, put typically between carbon and copper alloy one layer it is soft
Property graphite, goldleaf, Copper Foil etc..Divertor part prepared by this mechanical connecting structure is applied to that heat flux is relatively low, pulse length
Shorter tokamak device.
If divertor position heat flux is higher and long pulse runs, in order to avoid overheating occurs in material, it is necessary to filter partially
Device is carried out actively except heat in plasma discharge processes, so as to need to take various welding procedures realize carbon-based material with it is heat sink
Metallurgical binding between material, it is ensured that divertor part have excellent heat dispel ability and the security in fusion environment and
Stability.
The connection of carbon-based material and copper alloy must solve two problems of aspect, i.e. thermal expansion coefficient difference greatly and can not
Mutually wetting.
In order to solve interfacial stress caused by thermal expansion coefficient difference, generally require between carbon-based material and copper alloy plus
One intermediate layer.At present, using it is most be oxygen-free high conductivity type copper (OFHC) as intermediate layer, using the plastic deformation of oxygen-free high conductivity type copper
Release thermal stress.Can be obtained with excellent combination using connected modes such as active metal casting (AMC), soldering, diffusion welding (DW)s
Carbon-based material/copper alloy the joint of energy.Austrian PlanseeGE companies are most earlier than invention active metal casting (AMC) in 1992
Method, realizes the connection of high heat conduction carbon/carbon compound material and copper alloy (CuCrZr).Its by C/C composites and graphite/
When Cu alloys are connected, C/C composites, graphite surface first are irradiated with laser beam, form a large amount of a diameter of 50-500 μm, hole depth is
100-750 μm of circular hole, can so increase interfacial area increases surface energy, so as to improve cracking growth resistance ability；So
Afterwards, on the treated C/C composites of active metal casting, graphite surface, connected finally by electron beam weldering, high temperature insostatic pressing (HIP) etc.
Method couples together it with copper alloy, and the tensile strength of CFC/Cu alloy-junctions reaches 30MPa；It is to be noted that the skill
Art is relatively costly, the modified quality control in its surface is more difficult.
In order to realize the modified of carbon material, one layer of gold that can be reacted with carbon can also be deposited on carbon-based material surface
Category, such as Si, Al, Ti, Zr, Cr, Mo, W copper alloy, are improved by solid-state reaction in carbon surface one layer of carbide thin layer of generation
Copper realizes the connection of carbon material and oxygen-free copper in the wetability of carbon/carbon surface.Using it is most be Ti and Cr come the carbon substrate that is modified
Material surface, due to the effect of transition metal carburization zone, the Mean Shear shearing stress of the pure Cu joints of CFC/ reaches more than 30MPa, far
Higher than the interlaminar shear strength of CFC materials.
Further, it is also possible to using direct soldering connection carbon-based material and copper alloy, the solder that welding process needs needs to contain
There are the element that there is wetability with carbon, such as Ti, Zr, Cr, Si；Removal vacuum environment obsolete Cd, Zn, Ag etc. are needed simultaneously
Element；Brazing temperature is also required to control on the running temperature of part；In order to alleviate the thermal stress of boundary layer, anaerobic fine copper is fitted
It is also essential to answer layer.JAEA such as Japan connects CFC and anaerobic fine copper using NiCrP solders, then again by heat etc.
Static pressure connects anaerobic fine copper and copper alloy heat sink material at 500 DEG C；Italy use commercialization Gemco alloys (87.75wt%Cu,
12wt%Ge and 0.25wt%Ni) welding CFC-Cu strength of joints be about 34MPa.
The content of the invention
For above-mentioned prior art, it is an object of the invention to provide a kind of carbon-based material and the soldering connecting method of copper,
The connectivity problem of carbon-based material and copper-based material is solved, the metallurgical junction of carbon-based material and copper-based material is realized by vacuum brazing
Close.
In order to achieve the above object, the present invention uses following technical scheme.
It is an object of the invention to provide a kind of carbon-based material and the soldering connecting method of copper, comprise the following steps：
Step one, carbon-based material surface metalation；
(1) carbon-based material is pre-processed, including surface sand-blasting process, ultrasonic wave clean and dehydrate step；
(2) one layer of Cr metal paste is deposited on carbon-based material surface by method for printing screen, after dried process, in vacuum
It is sintered in heating furnace, working vacuum degree is less than 1 × 10-2Pa, 1300-1400 DEG C of sintering temperature, sintering time 0.5-1h is raw
Into one layer of carbonization layers of chrome of densification；
Step 2, vacuum casting fine copper；
(1) carbon-based material of surface metalation is put into mould with anaerobic fine copper and is assembled, anaerobic fine copper block upper,
Carbon-based material is under, and carbon-based material metalized surface is relative with anaerobic fine copper block upward；It is then placed in being cast in vacuum furnace,
Working vacuum degree is less than 1 × 10-2Pa, cast temperature is 1150-1200 DEG C, is incubated 15-30min；
(2) after the completion of casting, 1000 DEG C are cooled in 30min, then 600 DEG C is cooled to by 40-60min, finally in stove
Inside it is cooled to room temperature；
(3) by machining after taking out, the anaerobic fine copper thickness that will cast in carbon-based material surface is machined to 1-3mm thickness；
Step 3, vacuum brazing；
The carbon-based material of casting anaerobic fine copper, copper base solder, copper-based material dock assembled successively, carbon-based material casting
Anaerobic fine copper face is relative with copper base solder；
It is then placed in being welded in vacuum brazing furnace, in temperature-rise period, 100 DEG C or so insulation 1-2h, 400 DEG C or so guarantors
Warm 10-20min, then heats to welding temperature soldering；After soldering is finished, room temperature is cooled in stove；Working vacuum degree less than 1 ×
10-2Pa。
Further, the welding temperature of step 3 vacuum brazing is 700-800 DEG C, and pricker soaking time is 10-30min.
Further, the carbon-based material is high purity graphite or carbon fiber reinforced carbon matrix composite.
Further, the copper-based material includes fine copper or copper alloy.
Further, the copper alloy is CuCrZr alloys.
Further, the copper base solder is CuP base solders.
Further, the CuP bases solder is the solder paper tinsel of amorphous state or crystalline state, and thickness is 50-200 microns.
Further, the oxidation of material surface is removed before the assembling of carbon-based material anaerobic fine copper face, copper base solder and copper-based material
Layer.
Further, the anaerobic fine copper leads anaerobic fine copper for height, and purity is more than 99.9999%.
The beneficial effect that technical scheme provided in an embodiment of the present invention is brought is：
A kind of carbon-based material of the present invention and the soldering connecting method of copper, gold is carried out by slurry method to the surface of carbon-based material
Categoryization, increases the wetability of copper and carbon.
A kind of carbon-based material of the present invention and the soldering connecting method of copper, carbon can be effectively reduced by being segmented insulation cooling
Due to internal stress caused by thermal expansion coefficient difference between sill and anaerobic fine copper.
A kind of carbon-based material of the present invention and the soldering connecting method of copper, because vacuum brazing temperature is low, can effectively slacken
Copper alloy crystal grain is grown up, hydraulic performance decline the problems such as.
The soldering connecting method of a kind of carbon-based material of the present invention and copper, efficiency high is suitable for mass production, the weld seam for obtaining
Be well combined, no hole, be mingled with, the defect such as crackle；The shear strength of preparation-obtained connector is more than 30MPa, prepares
Water-cooled module can bear heat flux more than 10MW/m2Stable state thermic load without occur fail.
Specific embodiment
A kind of carbon-based material of the invention and the soldering connecting method of copper are elaborated with reference to specific embodiment.
Embodiment 1：
The soldering connecting method of a kind of carbon-based material of the present invention and copper, the method is comprised the following steps：
Step one, carbon-based material surface metalation；
(1) carbon-based material is pre-processed, including surface sand-blasting process, ultrasonic wave are cleaned and dehydrated；
(2) one layer of Cr metal paste is deposited on carbon-based material surface by method for printing screen, after dried process, in vacuum
It is sintered in heating furnace, working vacuum degree is better than 1 × 10-2Pa, 1300-1400 DEG C of sintering temperature, sintering time 0.5-1h is raw
Into one layer of carbonization layers of chrome of densification；
The carbon-based material is high purity graphite or carbon fiber reinforced carbon matrix composite；
Step 2, vacuum casting fine copper；
(1) carbon-based material of surface metalation is put into mould with anaerobic fine copper and is assembled, anaerobic fine copper block upper,
Carbon-based material is under, and carbon-based material metalized surface is relative with anaerobic fine copper block upward；It is put into vacuum furnace, working vacuum
Degree is better than 1 × 10-2Pa, cast temperature is 1150-1200 DEG C, is incubated 15-30min；
(2) after the completion of casting, 1000 DEG C are cooled in 30min, then 600 DEG C is cooled to by 40-60min, finally in stove
Inside it is cooled to room temperature；
(3) by machining after taking out, the anaerobic fine copper thickness that will cast in carbon-based material surface is machined to 1-3mm thickness；
Step 3, vacuum brazing；
The carbon-based material of casting anaerobic fine copper, copper base solder, copper-based material dock assembled successively, carbon-based material casting
Anaerobic fine copper face is relative with copper base solder, is then placed in being welded in vacuum brazing furnace, in temperature-rise period, 100 DEG C or so guarantors
Warm 1-2h, 400 DEG C or so insulation 10-20min, then heats to welding temperature welding；After soldering is finished, room is cooled in stove
Temperature；Working vacuum degree is better than 1 × 10-2Pa, welding temperature is 700-800 DEG C, and pricker soaking time is 10-30min；
The copper-based material includes fine copper or copper alloy.
The copper base solder is CuP base solders, preferably the solder paper tinsel of amorphous state or crystalline state, and thickness is 50-200 microns.
Carbon-based material anaerobic fine copper face, copper base solder, copper-based material surface oxide layer are removed before assembling.
Embodiment 2：
The soldering connecting method of a kind of carbon-based material of the present invention and copper, the method is comprised the following steps：
Step one, the metallization of carbon fiber reinforced carbon matrix composite material surface；
Carbon fiber reinforced carbon matrix composite is pre-processed, including surface sand-blasting process, ultrasonic wave are cleaned and de-
Water is dried；
One layer of Cr metal paste is deposited in carbon fiber reinforced carbon matrix composite material surface by method for printing screen, at drying
After reason, sintered in vacuum drying oven, 1300 DEG C of sintering temperature, sintering time 1h；Vacuum drying oven working vacuum degree is better than 1 × 10-2Pa；
Step 2, vacuum casting fine copper；
The carbon fiber reinforced carbon matrix composite of surface metalation is put into mould with anaerobic fine copper block and is assembled, nothing
Oxygen fine copper block upper, the carbon fiber reinforced carbon matrix composite of surface metalation under, metalized surface upward with anaerobic fine copper
Block is relative；
It is then placed in vacuum furnace, cast temperature is 1200 DEG C, soaking time 15min.After heating is finished, 30min
Inside it is cooled to 1000 DEG C；600 DEG C are cooled to by 60min again, room temperature is finally cooled in stove；
Sample is taken out, by machining, the anaerobic fine copper thickness of casting 1mm is machined to thick；
The anaerobic fine copper leads anaerobic fine copper for height, and purity is more than 99.9999%；
Step 3, vacuum brazing；
Cast the carbon fiber reinforced carbon matrix composite of anaerobic fine copper, CuP bases solder, CuCrZr alloys are docked successively carries out
Assembling, carbon fiber reinforced carbon matrix composite anaerobic fine copper face CuP base solders are relative；It is then placed in being welded in vacuum brazing furnace
Connect, working vacuum degree is better than 1 × 10-2Pa, welding temperature is 700 DEG C；1h, 400 DEG C of left sides are incubated in temperature-rise period at 100 DEG C or so
20min is incubated when right；Holding time is 30min；Soldering is finished, and room temperature is cooled in stove.
The CuP bases solder is amorphous filler metal paper tinsel, and thickness is 50 μm.
Carbon fiber reinforced carbon matrix composite anaerobic fine copper face, CuP solders, the Surface Oxygen of CuCrZr alloys are removed before assembling
Change layer.
Embodiment 3：
The soldering connecting method of a kind of carbon-based material of the present invention and copper, the method is comprised the following steps：
Step one, the metallization of high purity graphite material surface；
High purity graphite material is pre-processed first, including surface sand-blasting process, ultrasonic wave are cleaned, dehydrated；
One layer of Cr metal paste is deposited in high purity graphite material surface by method for printing screen, after dried process, true
It is sintered in empty stove, 1400 DEG C of sintering temperature, sintering time 0.5h；Vacuum drying oven working vacuum degree is better than 1 × 10-2Pa；
Step 2, vacuum casting fine copper；
The high purity graphite material of surface metalation is put into mould with anaerobic fine copper block and is assembled, anaerobic fine copper block exists
On, under, wherein metalized surface is upward for the high purity graphite material of surface metalation；
It is then placed in vacuum furnace, cast temperature is 1150 DEG C, soaking time 30min；After heating is finished, 20min
Inside it is cooled to 1000 DEG C；600 DEG C are cooled to by 40min again, last stove is cooled to room temperature；
Sample is taken out, by machining, the anaerobic fine copper thickness of casting 3mm is machined to thick；
The anaerobic fine copper leads anaerobic fine copper for height, and purity is more than 99.9999%；
Step 3, vacuum brazing；
The high purity graphite material of casting anaerobic fine copper, CuP solders, CuCrZr alloys are assembled using docking mode；
It is then placed in being welded in vacuum brazing furnace, working vacuum degree is better than 1 × 10-2Pa, welding temperature is 800 DEG C；
1h is incubated in temperature-rise period at 100 DEG C or so, 20min is incubated at 400 DEG C or so；Holding time is 15min；Soldering is finished,
Room temperature is cooled in stove；
The CuP bases solder is amorphous filler metal paper tinsel, and thickness is 200 μm；
High purity graphite material anaerobic fine copper face, CuP solders, the surface oxide layer of CuCrZr alloys are removed before assembling.
Claims (9)
1. the soldering connecting method of a kind of carbon-based material and copper, it is characterised in that the method is comprised the following steps：
Step one, carbon-based material surface metalation；
(1) carbon-based material is pre-processed, including surface sand-blasting process, ultrasonic wave clean and dehydrate step；
(2) one layer of Cr metal paste is deposited on carbon-based material surface by method for printing screen, after dried process, in heating in vacuum
It is sintered in stove, working vacuum degree is less than 1 × 10-2Pa, 1300-1400 DEG C of sintering temperature, sintering time 0.5-1h, generation one
The fine and close carbonization layers of chrome of layer；
Step 2, vacuum casting fine copper；
(1) carbon-based material of surface metalation is put into mould with anaerobic fine copper and is assembled, anaerobic fine copper block is carbon-based upper
Material is under, and carbon-based material metalized surface is relative with anaerobic fine copper block upward；It is then placed in being cast in vacuum furnace, work
Vacuum is less than 1 × 10-2Pa, cast temperature is 1150-1200 DEG C, is incubated 15-30min；
(2) after the completion of casting, 1000 DEG C are cooled in 30min, then 600 DEG C is cooled to by 40-60min, it is finally cold in stove
To room temperature；
(3) by machining after taking out, the anaerobic fine copper thickness that will cast in carbon-based material surface is machined to 1-3mm thickness；
Step 3, vacuum brazing；
The carbon-based material of casting anaerobic fine copper, copper base solder, copper-based material dock assembled successively, carbon-based material casting anaerobic
Fine copper face is relative with copper base solder；
It is then placed in being welded in vacuum brazing furnace, in temperature-rise period, 100 DEG C or so insulation 1-2h, 400 DEG C or so insulations
10-20min, then heats to welding temperature soldering；After soldering is finished, room temperature is cooled in stove；Working vacuum degree less than 1 ×
10-2Pa。
2. the soldering connecting method of a kind of carbon-based material according to claim 1 and copper, it is characterised in that step 3 vacuum
The welding temperature of soldering is 700-800 DEG C, and pricker soaking time is 10-30min.
3. the soldering connecting method of a kind of carbon-based material according to claim 1 and copper, it is characterised in that the carbon substrate
Expect to be high purity graphite or carbon fiber reinforced carbon matrix composite.
4. the soldering connecting method of a kind of carbon-based material according to claim 1 and copper, it is characterised in that the Copper base material
Material includes fine copper or copper alloy.
5. the soldering connecting method of a kind of carbon-based material according to claim 4 and copper, it is characterised in that the copper alloy
It is CuCrZr alloys.
6. the soldering connecting method of a kind of carbon-based material according to claim 1 and copper, it is characterised in that the copper-based pricker
Expect to be CuP base solders.
7. the soldering connecting method of a kind of carbon-based material according to claim 6 and copper, it is characterised in that the CuP bases
Solder is the solder paper tinsel of amorphous state or crystalline state, and thickness is 50-200 microns.
8. the soldering connecting method of a kind of carbon-based material according to claim 1 and copper, it is characterised in that carbon-based material without
The oxide layer of removal material surface before the assembling of oxygen fine copper face, copper base solder and copper-based material.
9. the soldering connecting method of a kind of carbon-based material according to claim 1 and copper, it is characterised in that the anaerobic is pure
Copper leads anaerobic fine copper for height, and purity is more than 99.9999%.
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Cited By (9)
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| CN107252942A (en) * | 2017-07-17 | 2017-10-17 | 中国科学技术大学 | A kind of metal surface forms the processing technology of micro-nano multi-level composite construction |
| CN108161156A (en) * | 2017-11-23 | 2018-06-15 | 安泰天龙钨钼科技有限公司 | A kind of vacuum brazing method of molybdenum alloy and graphite |
| CN109467456A (en) * | 2017-09-08 | 2019-03-15 | 核工业西南物理研究院 | A method of it is modified to carbon-based material surface using metal paste |
| CN109640586A (en) * | 2018-12-20 | 2019-04-16 | 有研工程技术研究院有限公司 | A kind of preparation method of light flexible graphite heat conducting rope |
| CN109913696A (en) * | 2019-04-30 | 2019-06-21 | 华侨大学 | A kind of method of graphite surface metallization |
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| CN107252942A (en) * | 2017-07-17 | 2017-10-17 | 中国科学技术大学 | A kind of metal surface forms the processing technology of micro-nano multi-level composite construction |
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| CN108161156B (en) * | 2017-11-23 | 2021-01-01 | 安泰天龙钨钼科技有限公司 | Vacuum brazing method for molybdenum alloy and graphite |
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