CN104625283A - Auxiliary brazing method for grapheme composite middle layer of three-dimensional structure - Google Patents
Auxiliary brazing method for grapheme composite middle layer of three-dimensional structure Download PDFInfo
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- CN104625283A CN104625283A CN201410828186.XA CN201410828186A CN104625283A CN 104625283 A CN104625283 A CN 104625283A CN 201410828186 A CN201410828186 A CN 201410828186A CN 104625283 A CN104625283 A CN 104625283A
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- dimensional structure
- structure graphene
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- graphene composite
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Classifications
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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
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
Abstract
The invention relates to the field of material welding, in particular to an auxiliary brazing method for a grapheme composite middle layer of a three-dimensional structure. The problem that in the existing brazing process, a connector is prone to generating large residual stress to lead to the poor mechanical property of the brazing connector is solved. The method includes the steps that impurities on the surface of foam metal are removed, the foam metal is placed in a chemical vapor deposition device, argon is injected into the device, the gas flow and pressure are adjusted, then temperature is made to rise, methane is injected, the gas flow and pressure are adjusted to carry out deposition, and the grapheme composite middle layer of the three-dimensional structure is obtained after deposition is completed; the grapheme composite middle layer of the three-dimensional structure is placed between two materials to be welded, brazing filler metal is placed between faces to be welded, the combination is placed in a vacuum brazing furnace, the vacuum brazing furnace is vacuumized, the heat is preserved at high temperature, and then the vacuum brazing furnace is cooled to complete the auxiliary brazing process of the grapheme composite middle layer of the three-dimensional structure. The method is used for auxiliary brazing for the grapheme composite middle layer of the three-dimensional structure.
Description
Technical field
The present invention relates to material welding field.
Background technology
Following two hang-ups are mainly faced in material braze process.First, between material, thermal expansion coefficient difference is large, and the process center tap of soldering very easily produces larger residual stress.Residual stress can seriously undermine the mechanical property of joint, even causes the joint connected to destroy.At present, joint residual stress can be alleviated by preferred solder and adjustment soldering interlayer structure, improve soldered fitting performance.Secondly, the wettability contrast of different materials surface and solder is comparatively large, and then generation interfacial reaction is insufficient and conversion zone is discontinuous etc., and problem all can butt joint performance produce serious influence.Graphene, is often referred to single-layer graphene, is by sp
2the carbon atom of hydridization links the two-dimensional nano material with carbon element with conjugated structure obtained by hexagon, can be regarded as one deck of graphite.The performance of the many uniquenesses of Graphene, because density is low, intensity is high, elastic modelling quantity high, is a kind of ideal Material reinforcement body.
Summary of the invention
The process center tap that the present invention will solve existing soldering very easily produces larger residual stress and causes the problem of soldered fitting poor mechanical property, and provides the method for three-dimensional structure Graphene composite interlayer assistant brazing.
The method of three-dimensional structure Graphene composite interlayer assistant brazing, specifically carry out according to following steps:
One, by ultrasonic for foam metal acetone pretreatment 10min ~ 20min, the foam metal of surface removal impurity is obtained;
Described foam metal is foam Ni or foam Cu;
Two, the foam metal of surface removal impurity is placed in chemical vapor deposition unit, being evacuated to pressure is below 20Pa, pass into argon gas, adjustment argon gas flow is 10sccm ~ 50sccm, pressure in chemical vapor deposition unit is regulated to be 50Pa ~ 300Pa, and under pressure is 50Pa ~ 300Pa and argon gas atmosphere, by temperature most 800 DEG C ~ 1200 DEG C;
Three, pass into methane, the gas flow regulating methane is 5sccm ~ 40sccm, the gas flow regulating argon gas is 60sccm ~ 95sccm, pressure in chemical vapor deposition unit is regulated to be 200Pa ~ 800Pa, then deposit under be 200Pa ~ 800Pa and temperature being the condition of 800 DEG C ~ 1000 DEG C at pressure, sedimentation time is 5min ~ 35min, after deposition terminates, close heating power supply, stop passing into methane, under an argon atmosphere, with cooling velocity be 5 DEG C/temperature is cooled to room temperature by min ~ 30 DEG C/min, namely three-dimensional structure Graphene metal composite intermediate layer is obtained,
The summation of described methane and the gas flow of argon gas is 100sccm;
Four, three-dimensional structure Graphene metal composite intermediate layer is placed between two materials to be welded, then solder is placed between three-dimensional structure Graphene metal composite intermediate layer and the junction to be welded of two materials to be welded, and be positioned in vacuum brazing furnace, to vacuum brazing stove evacuation, then at temperature is 500 DEG C ~ 1200 DEG C, 2min ~ 30min is incubated, finally with cooling rate be 2 DEG C/temperature is cooled to room temperature by 500 DEG C ~ 1200 DEG C, namely completes three-dimensional structure Graphene composite interlayer assistant brazing process by min ~ 30 DEG C/min.
The invention has the beneficial effects as follows:
1, the present invention adopts chemical vapour deposition (CVD) CVD method, and foam Cu or foam Ni are prepared three-dimensional structure Graphene composite interlayer, can control the growth of Graphenes by changing the experiment parameter such as sedimentation time, simple to operate and by force repeated.
2, the present invention utilizes three-dimensional structure Graphene, can improve the dispersiveness of Graphene in solder, reduces solder thermal coefficient of expansion, alleviates the stress in joint, is conducive to improving soldered fitting performance.
3, the present invention makes to utilize three-dimensional structure Graphene, the Graphene that conventional method can be avoided to prepare is reunited in brazed seam, utilize three-dimensional structure substrate can improve the deployment conditions of Graphene significantly, and then give full play to the excellent properties of Graphene, improve the overall performance of soldered fitting.
4, the CVD method of the present invention's employing is simple, efficiently, is convenient to prepare composite interlayer in enormous quantities.
The present invention is used for the method for three-dimensional structure Graphene composite interlayer assistant brazing.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscopic picture in three-dimensional structure Graphene metal composite intermediate layer prepared by embodiment step 3.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: the method for the three-dimensional structure Graphene composite interlayer assistant brazing described in present embodiment, specifically carry out according to following steps:
One, by ultrasonic for foam metal acetone pretreatment 10min ~ 20min, the foam metal of surface removal impurity is obtained;
Described foam metal is foam Ni or foam Cu;
Two, the foam metal of surface removal impurity is placed in chemical vapor deposition unit, being evacuated to pressure is below 20Pa, pass into argon gas, adjustment argon gas flow is 10sccm ~ 50sccm, pressure in chemical vapor deposition unit is regulated to be 50Pa ~ 300Pa, and under pressure is 50Pa ~ 300Pa and argon gas atmosphere, by temperature most 800 DEG C ~ 1200 DEG C;
Three, pass into methane, the gas flow regulating methane is 5sccm ~ 40sccm, the gas flow regulating argon gas is 60sccm ~ 95sccm, pressure in chemical vapor deposition unit is regulated to be 200Pa ~ 800Pa, then deposit under be 200Pa ~ 800Pa and temperature being the condition of 800 DEG C ~ 1000 DEG C at pressure, sedimentation time is 5min ~ 35min, after deposition terminates, close heating power supply, stop passing into methane, under an argon atmosphere, with cooling velocity be 5 DEG C/temperature is cooled to room temperature by min ~ 30 DEG C/min, namely three-dimensional structure Graphene metal composite intermediate layer is obtained,
The summation of described methane and the gas flow of argon gas is 100sccm;
Four, three-dimensional structure Graphene metal composite intermediate layer is placed between two materials to be welded, then solder is placed between three-dimensional structure Graphene metal composite intermediate layer and the junction to be welded of two materials to be welded, and be positioned in vacuum brazing furnace, to vacuum brazing stove evacuation, then at temperature is 500 DEG C ~ 1200 DEG C, 2min ~ 30min is incubated, finally with cooling rate be 2 DEG C/temperature is cooled to room temperature by 500 DEG C ~ 1200 DEG C, namely completes three-dimensional structure Graphene composite interlayer assistant brazing process by min ~ 30 DEG C/min.
Namely three-dimensional structure Graphene metal composite intermediate layer described in this detailed description of the invention step 3 forms three-dimensional structure Graphene on foam metal surface.
Composite soldering intermediate layer directly adds or utilize reaction in brazing process to form the wild phase of low thermal coefficient of expansion, high elastic modulus in original solder system, realizes designing the Composite of soldered fitting.The method of composite interlayer is adopted to connect same material or foreign material, this method had both suppressed the formation of frangible compounds completely and had obtained soft solid solution tissue, change again thermal coefficient of expansion and the elastic modelling quantity of the addition regulation and control joint intermediate layer tissue of wild phase, the adjustable boundary's tissue of thermal coefficient of expansion is formed at material interface, be conducive to reducing solder thermal coefficient of expansion, alleviate the stress in joint.
The square ratio juris of present embodiment three-dimensional structure Graphene composite interlayer assistant brazing is: utilize chemical vapour deposition (CVD) (CVD) method to prepare three-dimensional structure Graphene composite interlayer, then utilize composite interlayer to carry out assistant brazing.Utilize three-dimensional structure Graphene, improve the dispersiveness of Graphene in solder, alleviate the residual stress of brazing process median surface, improve the overall performance of soldered fitting.
The beneficial effect of present embodiment is:
1, present embodiment adopts chemical vapour deposition (CVD) CVD method, and foam Cu or foam Ni are prepared three-dimensional structure Graphene composite interlayer, can control the growth of Graphenes by changing the experiment parameters such as sedimentation time, simple to operate and by force repeated.
2, present embodiment utilizes three-dimensional structure Graphene, can improve the dispersiveness of Graphene in solder, reduces solder thermal coefficient of expansion, alleviates the stress in joint, is conducive to improving soldered fitting performance.
3, present embodiment makes to utilize three-dimensional structure Graphene, the Graphene of traditional lamella can be avoided to reunite in brazed seam, utilize three-dimensional structure substrate can improve the deployment conditions of Graphene significantly, and then give full play to the excellent properties of Graphene, improve the overall performance of soldered fitting.
4, the CVD method of present embodiment employing is simple, efficiently, is convenient to prepare composite interlayer in enormous quantities.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: the material to be welded described in step 4 is metal material or ceramic material; Described material sand papering to be welded, then ultrasonic pretreatment 5min ~ 10min in acetone.Other is identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one or two unlike: the solder described in step 4 is AgCuTi solder or TiNi solder.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: by temperature most 800 DEG C in step 2.Other is identical with detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike: by temperature most 1000 DEG C in step 2.Other is identical with detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five unlike: regulate the gas flow of methane to be 10sccm in step 3, regulate the gas flow of argon gas to be 90sccm.Other is identical with detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six unlike: regulate the gas flow of methane to be 20sccm in step 3, regulate the gas flow of argon gas to be 80sccm.Other is identical with detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven unlike: regulate pressure in chemical vapor deposition unit to be 500Pa in step 3.Other is identical with detailed description of the invention one to seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention one to eight unlike: regulate pressure in chemical vapor deposition unit to be 800Pa in step 3.Other is identical with detailed description of the invention one to eight.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention one to nine unlike: in step 3, sedimentation time is 15min.Other is identical with detailed description of the invention one to nine.
Detailed description of the invention 11: one of present embodiment and detailed description of the invention one to ten unlike: the material to be welded described in step 4 is metal Nb; Described Nb sand papering, then ultrasonic pretreatment 5min ~ 10min in acetone.Other is identical with detailed description of the invention one to ten.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment:
The method of the three-dimensional structure Graphene composite interlayer assistant brazing described in the present embodiment, specifically carry out according to following steps:
One, by ultrasonic for foam Cu acetone pretreatment 10min, the foam Cu of surface removal impurity is obtained;
Two, the foam Cu of surface removal impurity is placed in chemical vapor deposition unit, being evacuated to pressure is below 20Pa, pass into argon gas, adjustment argon gas flow is 20sccm, pressure in chemical vapor deposition unit is regulated to be 100Pa, and under pressure is 100Pa and argon gas atmosphere, by temperature most 900 DEG C;
Three, methane is passed into, the gas flow regulating methane is 10sccm, and the gas flow regulating argon gas is 90sccm, regulates pressure in chemical vapor deposition unit to be 800Pa, then deposit under be 800Pa and temperature being the condition of 900 DEG C at pressure, sedimentation time is 5min, after deposition terminates, closes heating power supply, stop passing into methane, under an argon atmosphere, be that temperature is cooled to room temperature by 5 DEG C/min with cooling velocity, obtain three-dimensional structure Graphene metal composite intermediate layer;
Four, three-dimensional structure Graphene metal composite intermediate layer is placed between two Nb, then AgCuTi solder is placed between three-dimensional structure Graphene metal composite intermediate layer and the junction to be welded of two Nb, and be positioned in vacuum brazing furnace, to vacuum brazing stove evacuation, then at temperature is 750 DEG C, 5min is incubated, last is that temperature is cooled to room temperature by 750 DEG C by 10 DEG C/min with cooling rate, namely completes three-dimensional structure Graphene composite interlayer assistant brazing process;
Two described Nb sand paperings, then ultrasonic pretreatment 5min in acetone.
Namely described three-dimensional structure Graphene metal composite intermediate layer forms three-dimensional structure Graphene on foam Cu surface.
Fig. 1 is the scanning electron microscopic picture in three-dimensional structure Graphene metal composite intermediate layer prepared by embodiment step 3, as seen from the figure, foam Cu has unique three-dimensional structure as we know from the figure, its surface of graphene coated after growth, there is unique three-dimensional structure equally, be conducive to the dispersion of Graphene in composite soldering like this, and then avoid the reunion of Graphene, the excellent properties of Graphene can be given full play to.
The metal Nb of use three-dimensional structure Graphene composite interlayer assistant brazing that the present embodiment obtains and the connector shearing strength at room temperature of metal Nb are 75MPa.
Claims (10)
1. the method for three-dimensional structure Graphene composite interlayer assistant brazing, is characterized in that the method for three-dimensional structure Graphene composite interlayer assistant brazing is carried out according to following steps:
One, by ultrasonic for foam metal acetone pretreatment 10min ~ 20min, the foam metal of surface removal impurity is obtained;
Described foam metal is foam Ni or foam Cu;
Two, the foam metal of surface removal impurity is placed in chemical vapor deposition unit, being evacuated to pressure is below 20Pa, pass into argon gas, adjustment argon gas flow is 10sccm ~ 50sccm, pressure in chemical vapor deposition unit is regulated to be 50Pa ~ 300Pa, and under pressure is 50Pa ~ 300Pa and argon gas atmosphere, by temperature most 800 DEG C ~ 1200 DEG C;
Three, pass into methane, the gas flow regulating methane is 5sccm ~ 40sccm, the gas flow regulating argon gas is 60sccm ~ 95sccm, pressure in chemical vapor deposition unit is regulated to be 200Pa ~ 800Pa, then deposit under be 200Pa ~ 800Pa and temperature being the condition of 800 DEG C ~ 1000 DEG C at pressure, sedimentation time is 5min ~ 35min, after deposition terminates, close heating power supply, stop passing into methane, under an argon atmosphere, with cooling velocity be 5 DEG C/temperature is cooled to room temperature by min ~ 30 DEG C/min, namely three-dimensional structure Graphene metal composite intermediate layer is obtained,
The summation of described methane and the gas flow of argon gas is 100sccm;
Four, three-dimensional structure Graphene metal composite intermediate layer is placed between two materials to be welded, then solder is placed between three-dimensional structure Graphene metal composite intermediate layer and the junction to be welded of two materials to be welded, and be positioned in vacuum brazing furnace, to vacuum brazing stove evacuation, then at temperature is 500 DEG C ~ 1200 DEG C, 2min ~ 30min is incubated, finally with cooling rate be 2 DEG C/temperature is cooled to room temperature by 500 DEG C ~ 1200 DEG C, namely completes three-dimensional structure Graphene composite interlayer assistant brazing process by min ~ 30 DEG C/min.
2. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that the material to be welded described in step 4 is metal material or ceramic material; Described material sand papering to be welded, then ultrasonic pretreatment 5min ~ 10min in acetone.
3. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that the solder described in step 4 is AgCuTi solder or TiNi solder.
4. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that temperature most 800 DEG C in step 2.
5. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that temperature most 1000 DEG C in step 2.
6. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that regulating in step 3 the gas flow of methane to be 10sccm, and the gas flow regulating argon gas is 90sccm.
7. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that regulating in step 3 the gas flow of methane to be 20sccm, and the gas flow regulating argon gas is 80sccm.
8. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that regulating in step 3 pressure in chemical vapor deposition unit to be 500Pa.
9. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that regulating in step 3 pressure in chemical vapor deposition unit to be 800Pa.
10. the method for three-dimensional structure Graphene composite interlayer assistant brazing according to claim 1, is characterized in that in step 3, sedimentation time is 15min.
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| CN105081502A (en) * | 2015-09-14 | 2015-11-25 | 哈尔滨工业大学 | Method for brazing ceramic matrix composite material by being assisted through nitrogen treatment |
| CN105345195A (en) * | 2015-12-02 | 2016-02-24 | 哈尔滨工业大学 | Method for brazing aluminum or aluminum alloy and other metals |
| CN105397224A (en) * | 2015-12-28 | 2016-03-16 | 哈尔滨工业大学 | Method for brazing hard alloy and steel by utilizing foam metal interlayer |
| CN105420530A (en) * | 2015-12-09 | 2016-03-23 | 哈尔滨工业大学 | Preparation method for graphene-reinforced nickel-based composite materials |
| CN108069416A (en) * | 2016-11-14 | 2018-05-25 | 北京大学 | Ultra-clean graphene and preparation method thereof |
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| CN105081502A (en) * | 2015-09-14 | 2015-11-25 | 哈尔滨工业大学 | Method for brazing ceramic matrix composite material by being assisted through nitrogen treatment |
| CN105345195A (en) * | 2015-12-02 | 2016-02-24 | 哈尔滨工业大学 | Method for brazing aluminum or aluminum alloy and other metals |
| CN105345195B (en) * | 2015-12-02 | 2017-06-23 | 哈尔滨工业大学 | A kind of method of aluminum or aluminum alloy and other solder bonding metals |
| CN105420530A (en) * | 2015-12-09 | 2016-03-23 | 哈尔滨工业大学 | Preparation method for graphene-reinforced nickel-based composite materials |
| CN105397224A (en) * | 2015-12-28 | 2016-03-16 | 哈尔滨工业大学 | Method for brazing hard alloy and steel by utilizing foam metal interlayer |
| CN108069416B (en) * | 2016-11-14 | 2020-01-07 | 北京大学 | Ultra-clean graphene and preparation method thereof |
| CN108069416A (en) * | 2016-11-14 | 2018-05-25 | 北京大学 | Ultra-clean graphene and preparation method thereof |
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| CN109175764A (en) * | 2018-09-20 | 2019-01-11 | 哈尔滨工业大学 | A kind of method of graphene sponge middle layer assistant brazing |
| CN109175764B (en) * | 2018-09-20 | 2020-07-07 | 哈尔滨工业大学 | Method for auxiliary brazing of graphene sponge middle layer |
| CN110270729A (en) * | 2019-07-19 | 2019-09-24 | 哈尔滨工业大学 | A method of with graphene barrier layer assistant brazing Ti-Al system's alloy and ceramics |
| CN110497116A (en) * | 2019-08-06 | 2019-11-26 | 华北水利水电大学 | A kind of mutative scale boron nitrogen graphene modified layer solder, Preparation method and use |
| CN111136361A (en) * | 2019-12-31 | 2020-05-12 | 陕西斯瑞新材料股份有限公司 | Method for vacuum brazing of dispersed copper |
| CN111136361B (en) * | 2019-12-31 | 2021-07-30 | 陕西斯瑞新材料股份有限公司 | Method for vacuum brazing of dispersed copper |
| CN112756727A (en) * | 2020-12-29 | 2021-05-07 | 哈尔滨工业大学 | Method for enhancing reduction resistance of brazed joint by graphene sponge barrier layer |
| CN112756727B (en) * | 2020-12-29 | 2022-08-02 | 哈尔滨工业大学 | Method for enhancing reduction resistance of brazed joint by graphene sponge barrier layer |
| CN113231706A (en) * | 2021-06-25 | 2021-08-10 | 哈尔滨工业大学 | Method for assisting in brazing dissimilar materials by using three-dimensional negative expansion network composite interlayer material |
| CN113857603A (en) * | 2021-09-29 | 2021-12-31 | 江苏科技大学 | Method for assisting in brazing ceramic matrix composite material and metal |
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