CN106346100A - Method for assisting brazing by carbon nanotube reinforced type three-dimensional middle layer - Google Patents
Method for assisting brazing by carbon nanotube reinforced type three-dimensional middle layer Download PDFInfo
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- CN106346100A CN106346100A CN201611081818.6A CN201611081818A CN106346100A CN 106346100 A CN106346100 A CN 106346100A CN 201611081818 A CN201611081818 A CN 201611081818A CN 106346100 A CN106346100 A CN 106346100A
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- 238000005219 brazing Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000002041 carbon nanotube Substances 0.000 title abstract description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 title abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 88
- 239000002184 metal Substances 0.000 claims abstract description 88
- 239000006260 foam Substances 0.000 claims abstract description 51
- 239000011888 foil Substances 0.000 claims abstract description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 47
- 229910000679 solder Inorganic materials 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000012535 impurity Substances 0.000 claims description 30
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 22
- 230000033228 biological regulation Effects 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 14
- 150000002431 hydrogen Chemical class 0.000 claims description 12
- 238000005086 pumping Methods 0.000 claims description 11
- 229960004756 ethanol Drugs 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 230000002708 enhancing effect Effects 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002071 nanotube Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 8
- 239000012071 phase Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000002905 metal composite material Substances 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 239000011324 bead Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 241001274660 Modulus Species 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- -1 arc discharge method Chemical compound 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- 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
- B23K1/206—Cleaning
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a method for assisting brazing by a carbon nanotube reinforced type three-dimensional middle layer, and relates to a method for brazing ceramic and metal, which aims at solving the problems of larger residual stress and insufficient high-temperature property in the existing ceramic and metal brazing connection process. The method comprises the following steps of 1, preparing soaked foam metal; 2, putting the soaked foam metal into a plasma reinforced type chemical vapor depositing vacuum device, and increasing temperature at certain pressure and hydrogen atmosphere; 3, preparing nanotube reinforced type foam metal; 4, preparing surface impurity-removed metal, surface impurity-removed brazing material foil and surface impurity-removed ceramic; 5, sequentially overlapping the surface impurity-removed to-be-brazed metal, the carbon nanotube reinforced type foam metal, the surface impurity-removed brazing material foil and the surface impurity-removed ceramic, so as to obtain a to-be-brazed part; brazing the to-be-brazed part, and cooling to room temperature. The method disclosed by the invention is used for assisting the brazing by the carbon nanotube reinforced type three-dimensional middle layer.
Description
Technical field
The present invention relates to the method for ceramic soldering and metal.
Background technology
Ceramic material is that in current engineering material, rigidity is best, hardness highest material, simultaneously the linear expansion coefficient of pottery
Lower than metal, when the temperature varies, pottery has good dimensional stability；Ceramic material typically has high fusing point
(mostly more than 2000 DEG C), not oxidizable at high temperature, and to acid, alkali, salt, there is good resistance to corrosion, have stable
Corrosion resistance, and its heat conductivity is less than metal material, is good heat-barrier material, and pottery has many excellent high temperatures
Energy.Pottery can be divided into several functions pottery according to its manufacture method, has been widely used in Aero-Space, energy traffic, electricity
Power electronics, biomedicine, chemical industry, the optically and mechanically field such as engineering.
Although pottery has above premium properties, its plasticity, toughness are relatively low, and its mouldability is bad to answer it is difficult to be processed into
Miscellaneous structure, therefore adopt is connected with metal more, realizes the complementation in aspect of performance with metal, has pottery with metal each to obtain
The ceramic-metal composite members of excellent properties.The ceramic-metal composite members applied in fields such as space flight and aviation many in high temperature load
Work under environment, selected pottery all can tolerate hot environment with metal, and pottery is often attached using method for welding with metal,
This undoubtedly causes huge challenge to soldered fitting, and the soldered fitting obtained by conventional method can occur molten under high temperature load
The phenomenon changed, ftracture.The soldering connection problem encountered of ceramic-metal composite members is as follows: on the one hand, the two chemical bond is not
With crystal structure is different, and physical and chemical composition difference is big, welding residual stress usually greatly, reacts insufficient, brittlement phase mistake
Many the problems such as, cause the decline of strength of joint；On the other hand, common method for welding resistance to elevated temperatures difference is it is impossible to meet high temperature work
Make demand.A kind of therefore guarantee Ceramic and metal joining intensity need to be developed, and the method that hot operation demand can be met.
CNT is the hollow tubular structure being wound by certain spiral angle by one or more layers graphene layer,
Find, the Young's moduluss of single-layer carbon nano-tube are up to 1tpa, suitable with diamond, about steel according to Theoretical Calculation and experiment measurement
5 times of material；Its tensile strength, in the range of 11～63gpa, 1000 times of about steel, has high rigidity and intensity；
And it has relatively low linear expansion coefficient, it is possible to decrease soldered fitting stress；CNT has higher fusing point, can lift pricker
Material fusion temperature, therefore it is widely used in reinforcement material.The advantage of CNT is that the one-dimension of its structure, reunion
The performance of impact CNT performance, therefore the dispersed of CNT has vital effect to the performance that it acts on.
Traditional preparation method of carbon nano-tube such as arc discharge method, laser ablation method, solid-phase pyrolysis, electric glow discharge method, polymerization is anti-
Answer synthetic method etc., the CNT producing unsetting carbon, reuniting that all can be different degrees of is it is difficult to be used for reinforcement material.
Content of the invention
The invention solves the problems that during existing ceramic material is connected with solder bonding metal, residual stress is larger and high-temperature behavior is not enough
Problem, and provide a kind of method that CNT strengthens three dimensional structure intermediate layer assistant brazing.
A kind of method that CNT strengthens three dimensional structure intermediate layer assistant brazing follows the steps below:
First, hydrochloric acid, acetone, dehydrated alcohol and the deionized water being 1mol/l～3mol/l with concentration successively by foam metal
It is respectively washed 10min, then naturally dries, obtain pretreated foam metal, catalyst is added in dehydrated alcohol, obtains
To the ethanol solution of the catalyst for 0.001mol/l～1mol/l for the concentration, pretreated foam metal is immersed in dense
Spend in the ethanol solution of the catalyst for 0.001mol/l～1mol/l, stand 1h, then naturally dry, after being soaked
Foam metal；
2nd, the foam metal after soaking is placed in plasma enhanced chemical vapor deposition vacuum equipment, is evacuated to
Pressure is 20pa～below 100pa, is passed through hydrogen, and regulation hydrogen gas flow is 20sccm～60sccm, adjusts evacuation speed
Pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled to 100pa～300pa by degree, and is 100pa in pressure
Under～300pa and hydrogen atmosphere, in 30min, temperature is heated up most 300 DEG C～800 DEG C；
3rd, it is passed through carbon-source gas, regulation carbon-source gas gas flow is 10sccm～100sccm, adjusts hydrogen gas stream
Measure as 1sccm～40sccm, adjust vacuum pumping rate and pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled
For 100pa～1000pa, then depositing system radio-frequency power be 50w～200w, pressure be 100pa～1000pa, carbon source gas
Body gas flow is 10sccm～100sccm, hydrogen gas flow is 1sccm～40sccm and temperature is 300 DEG C～800 DEG C bars
Deposited under part, sedimentation time is 1min～60min, after deposition terminates, close radio-frequency power supply and heating power supply, stop being passed through
Carbon-source gas and hydrogen, are cooled to room temperature, obtain the enhanced foam metal of CNT；
4th, by metal to be welded, pottery with solder paillon foil successively with 200 mesh, 400 mesh, 600 mesh and 800 mesh sand paperings, so
Use acetone ultrasonic pretreatment 10min～20min afterwards, obtain the metal to be welded removing surface impurity, the pottery removing surface impurity
With the solder paillon foil removing surface impurity；
5th, the metal to be welded of surface impurity, the enhanced foam metal of CNT will be removed, remove the solder of surface impurity
The pottery of paillon foil and removal surface impurity stacks successively, obtains part to be welded, part to be welded is placed in vacuum brazing furnace, in pressure is
1×10-4Pa～5 × 10-3Pa and brazing temperature are for, under conditions of 700 DEG C～1200 DEG C, insulation 1min～20min, then to drop
Warm speed is 2 DEG C/min～10 DEG C/min, and temperature is cooled to room temperature by 700 DEG C～1200 DEG C, that is, complete CNT and strengthen
The method of three dimensional structure intermediate layer assistant brazing.
CNT of the present invention strengthens the ultimate principle of three dimensional structure intermediate layer assistant brazing: is existed using chemical vapor deposition
On foamed materialss, in-situ preparation CNT is as intermediate layer, introduces CNT in weld seam, uniform due to CNT
Distribution plays one's part to the full, and dispersion-strengtherning, slows down residual stress thus improving strength of joint, reduces continuous brittlement phase and generates, and
Improve the high-temperature behavior of joint using the high-temperature behavior of itself, according to the good plasticity of selected foamed materialss, form plasticity good
Solid solution, intermetallic compound, thus alleviate larger residual stress between pottery and metal.
Beneficial effects of the present invention:
1st, in weld seam, the CNT of high intensity is uniformly distributed, and plays the effect of dispersion-strengtherning.
2nd, CNT thermal coefficient of expansion is low, the thermal coefficient of expansion of scalable solder, and selected foamed materialss plasticity is preferably
Plastic property of weld bead can be improved, thus reducing the residual stress of pottery and metal joint.
3rd, CNT and active element react, product Dispersed precipitate, do not form continuous brittlement phase, adjust conversion zone
Thickness, thus improve strength of joint.
4th, the good high-temperature behavior of CNT, can significantly improve the high-temperature behavior of soldered fitting.
5th, the CNT of plasma enhanced chemical vapor deposition method synthesis, introduces weld seam by intermediate layer, it is right to be not required to
Mother metal is processed, and mother metal structure, property are not affected.
The present invention is used for a kind of method that CNT strengthens three dimensional structure intermediate layer assistant brazing.
Brief description
Fig. 1 is the scanning electron microscope (SEM) photograph of the enhanced foam metal of CNT of embodiment one step 3 preparation.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, also include each specific embodiment it
Between combination in any.
Specific embodiment one: a kind of CNT described in present embodiment strengthens three dimensional structure intermediate layer assistant brazing
Method follow the steps below:
First, hydrochloric acid, acetone, dehydrated alcohol and the deionized water being 1mol/l～3mol/l with concentration successively by foam metal
It is respectively washed 10min, then naturally dries, obtain pretreated foam metal, catalyst is added in dehydrated alcohol, obtains
To the ethanol solution of the catalyst for 0.001mol/l～1mol/l for the concentration, pretreated foam metal is immersed in dense
Spend in the ethanol solution of the catalyst for 0.001mol/l～1mol/l, stand 1h, then naturally dry, after being soaked
Foam metal；
2nd, the foam metal after soaking is placed in plasma enhanced chemical vapor deposition vacuum equipment, is evacuated to
Pressure is 20pa～below 100pa, is passed through hydrogen, and regulation hydrogen gas flow is 20sccm～60sccm, adjusts evacuation speed
Pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled to 100pa～300pa by degree, and is 100pa in pressure
Under～300pa and hydrogen atmosphere, in 30min, temperature is heated up most 300 DEG C～800 DEG C；
3rd, it is passed through carbon-source gas, regulation carbon-source gas gas flow is 10sccm～100sccm, adjusts hydrogen gas stream
Measure as 1sccm～40sccm, adjust vacuum pumping rate and pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled
For 100pa～1000pa, then depositing system radio-frequency power be 50w～200w, pressure be 100pa～1000pa, carbon source gas
Body gas flow is 10sccm～100sccm, hydrogen gas flow is 1sccm～40sccm and temperature is 300 DEG C～800 DEG C bars
Deposited under part, sedimentation time is 1min～60min, after deposition terminates, close radio-frequency power supply and heating power supply, stop being passed through
Carbon-source gas and hydrogen, are cooled to room temperature, obtain the enhanced foam metal of CNT；
4th, by metal to be welded, pottery with solder paillon foil successively with 200 mesh, 400 mesh, 600 mesh and 800 mesh sand paperings, so
Use acetone ultrasonic pretreatment 10min～20min afterwards, obtain the metal to be welded removing surface impurity, the pottery removing surface impurity
With the solder paillon foil removing surface impurity；
5th, the metal to be welded of surface impurity, the enhanced foam metal of CNT will be removed, remove the solder of surface impurity
The pottery of paillon foil and removal surface impurity stacks successively, obtains part to be welded, part to be welded is placed in vacuum brazing furnace, in pressure is
1×10-4Pa～5 × 10-3Pa and brazing temperature are for, under conditions of 700 DEG C～1200 DEG C, insulation 1min～20min, then to drop
Warm speed is 2 DEG C/min～10 DEG C/min, and temperature is cooled to room temperature by 700 DEG C～1200 DEG C, that is, complete CNT and strengthen
The method of three dimensional structure intermediate layer assistant brazing.
The CNT being generated by plasma enhanced chemical vapor deposition method not only grows uniformly, the not group of generation
Poly- it might even be possible to directive growth；Plasma enhanced chemical vapor deposition method need not be processed to mother metal simultaneously, can
Directly CNT can be introduced among weld seam by the use of foam metal as intermediate layer, the property of mother metal, structure are not produced
Raw impact is so that mother metal is more stable in high temperature environments.
This specific embodiment CNT strengthens the ultimate principle of three dimensional structure intermediate layer assistant brazing: using chemical gas
Mutually it is deposited on in-situ preparation CNT on foamed materialss and, as intermediate layer, introduce CNT in weld seam, due to carbon nanometer
Being uniformly distributed of pipe plays one's part to the full, and dispersion-strengtherning, slows down residual stress thus improving strength of joint, reduces continuous brittlement phase
Generate, and improve the high-temperature behavior of joint using the high-temperature behavior of itself, according to the good plasticity of selected foamed materialss, formation is moulded
The good solid solution of property, intermetallic compound, thus alleviate larger residual stress between pottery and metal.
The beneficial effect of this specific embodiment:
1st, in weld seam, the CNT of high intensity is uniformly distributed, and plays the effect of dispersion-strengtherning.
2nd, CNT thermal coefficient of expansion is low, the thermal coefficient of expansion of scalable solder, and selected foamed materialss plasticity is preferably
Plastic property of weld bead can be improved, thus reducing the residual stress of pottery and metal joint.
3rd, CNT and active element react, product Dispersed precipitate, do not form continuous brittlement phase, adjust conversion zone
Thickness, thus improve strength of joint.
4th, the good high-temperature behavior of CNT, can significantly improve the high-temperature behavior of soldered fitting.
5th, the CNT of plasma enhanced chemical vapor deposition method synthesis, introduces weld seam by intermediate layer, it is right to be not required to
Mother metal is processed, and mother metal structure, property are not affected.
Specific embodiment two: present embodiment from unlike specific embodiment one: the foam described in step one
Metal is foam copper or nickel foam.Other identical with specific embodiment one.
Specific embodiment three: unlike one of present embodiment and specific embodiment one or two: institute in step one
The catalyst stated is six water nickel nitrates, ferric nitrate, cobalt nitrate, nickel sulfate, iron sulfate or cobaltous sulfate.Other and specific embodiment
One or two is identical.
Specific embodiment four: unlike one of present embodiment and specific embodiment one to three: institute in step 3
The carbon-source gas stated are methane, acetylene or ethanol.Other identical with specific embodiment one to three.
Specific embodiment five: unlike one of present embodiment and specific embodiment one to four: institute in step 4
The metal to be welded stated is tc4 titanium alloy, tc10 titanium alloy, tial alloy, rustless steel or gh99 alloy.Other and specific embodiment party
Formula one to four is identical.
Specific embodiment six: unlike one of present embodiment and specific embodiment one to five: institute in step 4
The pottery stated is cf/ c composite ceramicses, c/sic pottery, sio2- bn composite ceramicses, sio2Pottery or sio2f/sio2Pottery.Other
Identical with specific embodiment one to five.
Specific embodiment seven: unlike one of present embodiment and specific embodiment one to six: institute in step 4
The solder paillon foil stated is tizrnicu solder paillon foil, ti-cu solder paillon foil, ti-ni solder paillon foil, cu-zr solder paillon foil, agcu
Solder paillon foil or agcuti solder paillon foil.Other identical with specific embodiment one to six.
Specific embodiment eight: unlike one of present embodiment and specific embodiment one to seven: will in step 2
Foam metal after immersion is placed in plasma enhanced chemical vapor deposition vacuum equipment, be evacuated to pressure be 30pa with
Under, it is passed through hydrogen, regulation hydrogen gas flow is 40sccm, adjust vacuum pumping rate by plasma enhanced chemical vapor deposition
In vacuum equipment, pressure is controlled to 200pa, and in pressure for, under 200pa and hydrogen atmosphere, temperature heating up most in 30min
570℃.Other identical with specific embodiment one to seven.
Specific embodiment nine: unlike one of present embodiment and specific embodiment one to eight: logical in step 3
Enter carbon-source gas, regulation carbon-source gas gas flow is 40sccm, regulation hydrogen gas flow is 10sccm, adjust evacuation speed
Pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled to 700pa, then in depositing system radio-frequency power by degree
For 175w, pressure be 700pa, carbon-source gas gas flow be 40sccm, hydrogen gas flow be that 10sccm and temperature are 570 DEG C
Under the conditions of deposited, sedimentation time is 30min, after deposition terminates, closes radio-frequency power supply and heating power supply, stops being passed through carbon source
Gas and hydrogen, are cooled to room temperature, obtain the enhanced foam metal of CNT.Other and specific embodiment one to eight phase
With.
Specific embodiment ten: unlike one of present embodiment and specific embodiment one to nine: will in step 5
Remove metal to be welded, the enhanced foam metal of CNT, the solder paillon foil removing surface impurity and the removal table of surface impurity
The pottery of face impurity stacks successively, obtains part to be welded, and part to be welded is placed in vacuum brazing furnace, is 3 × 10 in pressure-3Pa and pricker
Under conditions of weldering temperature is 930 DEG C, it is incubated 10min, then with cooling rate for 5 DEG C/min, temperature is cooled to room by 930 DEG C
Temperature.Other identical with specific embodiment one to nine.
Specific embodiment 11: unlike one of present embodiment and specific embodiment one to ten: in step 2
Being evacuated to pressure is 25pa～below 70pa.Other identical with specific embodiment one to ten.
Specific embodiment 12: unlike one of present embodiment and specific embodiment one to ten one: step 2
Middle regulation hydrogen gas flow is 30sccm～50sccm.Other identical with specific embodiment one to ten one.
Specific embodiment 13: unlike one of present embodiment and specific embodiment one to ten two: step 2
Pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled to 150pa～270pa by middle regulation vacuum pumping rate.Its
It is identical with specific embodiment one to ten two.
Specific embodiment 14: unlike one of present embodiment and specific embodiment one to ten three: step 2
In and in pressure under 100pa～300pa and hydrogen atmosphere, in 30min, temperature is heated up most 400 DEG C～700 DEG C.Other
Identical with specific embodiment one to ten three.
Specific embodiment 15: unlike one of present embodiment and specific embodiment one to ten four: step 3
In be passed through carbon-source gas, regulation carbon-source gas gas flow be 20sccm～80sccm.Other and specific embodiment one to ten
Four is identical.
Specific embodiment 16: unlike one of present embodiment and specific embodiment one to ten five: step 3
Middle regulation hydrogen gas flow is 5sccm～30sccm.Other identical with specific embodiment one to ten five.
Specific embodiment 17: unlike one of present embodiment and specific embodiment one to ten six: step 3
Pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled to 270pa～850pa by middle regulation vacuum pumping rate.Its
It is identical with specific embodiment one to ten six.
Specific embodiment 18: unlike one of present embodiment and specific embodiment one to ten seven: step 3
In then depositing system radio-frequency power be 125w～190w, pressure be that 100pa～1000pa, carbon-source gas gas flow are
10sccm～100sccm, hydrogen gas flow are 1sccm～40sccm and temperature is sunk under the conditions of 300 DEG C～800 DEG C
Long-pending, sedimentation time is 1min～60min.Other identical with specific embodiment one to ten seven.
Specific embodiment 19: unlike one of present embodiment and specific embodiment one to ten eight: step 3
In then depositing system radio-frequency power be 50w～200w, pressure be that 100pa～1000pa, carbon-source gas gas flow are
10sccm～100sccm, hydrogen gas flow are 1sccm～40sccm and temperature is sunk under the conditions of 300 DEG C～800 DEG C
Long-pending, sedimentation time is 1min～40min.Other identical with specific embodiment one to ten eight.
Specific embodiment 20: unlike one of present embodiment and specific embodiment one to ten nine: step 5
Middle part to be welded is placed in vacuum brazing furnace, pressure be 1 × 10-4Pa～5 × 10-3Pa and brazing temperature are 800 DEG C～1000
Under conditions of DEG C, it is incubated 1min～20min.Other identical with specific embodiment one to ten nine.
Specific embodiment 21: unlike one of present embodiment and specific embodiment one to two ten: step
In five, part to be welded is placed in vacuum brazing furnace, is 1 × 10 in pressure-4Pa～5 × 10-3Pa and brazing temperature be 700 DEG C～
Under conditions of 1200 DEG C, it is incubated 5min～15min.Other identical with specific embodiment one to two ten.
Specific embodiment 22: unlike one of present embodiment and specific embodiment one to two 11: step
In rapid five and then with cooling rate for 4 DEG C/min～8 DEG C/min, temperature is cooled to room temperature by 700 DEG C～1200 DEG C.Other with
Specific embodiment one to two 11 is identical.
Using following examples checking beneficial effects of the present invention:
Embodiment one:
The method that a kind of CNT described in the present embodiment strengthens three dimensional structure intermediate layer assistant brazing is according to following
Step is carried out:
First, hydrochloric acid, acetone, dehydrated alcohol and deionized water that foam metal is 2mol/l with concentration successively are respectively washed
10min, then dries naturally, obtains pretreated foam metal, and catalyst is added in dehydrated alcohol, obtains concentration and is
The ethanol solution of the catalyst of 0.1mol/l, pretreated foam metal is immersed in the catalysis that concentration is 0.1mol/l
In the ethanol solution of agent, stand 1h, then naturally dry, the foam metal after being soaked；
2nd, the foam metal after soaking is placed in plasma enhanced chemical vapor deposition vacuum equipment, is evacuated to
Pressure is below 30pa, is passed through hydrogen, and regulations hydrogen gas flow is 40sccm, and regulation vacuum pumping rate is by plasma enhancing
In chemical vapor deposition vacuum equipment, pressure is controlled to 200pa, and in pressure for, under 200pa and hydrogen atmosphere, inciting somebody to action in 30min
Temperature heats up most 570 DEG C；
3rd, it is passed through carbon-source gas, regulation carbon-source gas gas flow is 40sccm, adjusting hydrogen gas flow is
10sccm, adjusts vacuum pumping rate and pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled to 700pa, then
Depositing system radio-frequency power be 175w, pressure be 700pa, carbon-source gas gas flow be that 40sccm, hydrogen gas flow are
10sccm and temperature are deposited under the conditions of 570 DEG C, and sedimentation time is 30min, after deposition terminates, close radio-frequency power supply and add
Thermoelectric generator, stops being passed through carbon-source gas and hydrogen, is cooled to room temperature, obtains the enhanced foam metal of CNT；
4th, by metal to be welded, pottery with solder paillon foil successively with 200 mesh, 400 mesh, 600 mesh and 800 mesh sand paperings, so
Use acetone ultrasonic pretreatment 15min afterwards, obtain the metal to be welded removing surface impurity, the pottery removing surface impurity and removal table
The solder paillon foil of face impurity；
5th, the metal to be welded of surface impurity, the enhanced foam metal of CNT will be removed, remove the solder of surface impurity
The pottery of paillon foil and removal surface impurity stacks successively, obtains part to be welded, part to be welded is placed in vacuum brazing furnace, in pressure is
3×10-3Under conditions of pa and brazing temperature are 930 DEG C, be incubated 10min, then with cooling rate for 5 DEG C/min, by temperature by
930 DEG C are cooled to room temperature, that is, complete the method that CNT strengthens three dimensional structure intermediate layer assistant brazing；
Foam metal described in step one is foam copper；
Catalyst described in step one is six water nickel nitrates；
Carbon-source gas described in step 3 are methane；
Metal to be welded described in step 4 is tc4 titanium alloy；
Pottery described in step 4 is cf/ c composite ceramicses；
Solder paillon foil described in step 4 is tizrnicu solder paillon foil.
The enhanced foam metal of CNT of step 3 preparation passes through weight difference assay and measures, and CNT strengthens
Foam metal in CNT volume fraction be 4%.
The pottery that present embodiment obtains is good with titanium alloy strength of joint, and high-temperature behavior is good, is evident that
The defects such as crackle, up to 58mpa, at 600 DEG C, elevated temperature strength can reach 24mpa to shear strength.
Fig. 1 is the scanning electron microscope (SEM) photograph of the enhanced foam metal of CNT of embodiment one step 3 preparation.As seen from the figure,
The length of carbon nanotube generating is longer, is evenly distributed, medium density, using dispersion in solder connector for the CNT, therefore can
Give full play to its effect, solution Ceramic and metal joining center tap intensity is not high, the not enough problem of high-temperature behavior.
Claims (10)
1. a kind of CNT strengthens the method for three dimensional structure intermediate layer assistant brazing it is characterised in that a kind of CNT strengthens
The method of three dimensional structure intermediate layer assistant brazing follows the steps below:
First, hydrochloric acid, acetone, dehydrated alcohol and the deionized water difference being 1mol/l～3mol/l with concentration successively by foam metal
Cleaning 10min, then naturally dries, obtains pretreated foam metal, catalyst is added in dehydrated alcohol, obtain dense
Spend the ethanol solution of the catalyst for 0.001mol/l～1mol/l, pretreated foam metal is immersed in concentration is
In the ethanol solution of the catalyst of 0.001mol/l～1mol/l, stand 1h, then naturally dry, the bubble after being soaked
Foam metal；
2nd, the foam metal after soaking is placed in plasma enhanced chemical vapor deposition vacuum equipment, is evacuated to pressure
For 20pa～below 100pa, it is passed through hydrogen, regulation hydrogen gas flow is 20sccm～60sccm, adjusting vacuum pumping rate will
In plasma enhanced chemical vapor deposition vacuum equipment, pressure is controlled to 100pa～300pa, and pressure for 100pa～
Under 300pa and hydrogen atmosphere, in 30min, temperature is heated up most 300 DEG C～800 DEG C；
3rd, it is passed through carbon-source gas, regulation carbon-source gas gas flow is 10sccm～100sccm, adjusting hydrogen gas flow is
1sccm～40sccm, adjusts vacuum pumping rate and is controlled to pressure in plasma enhanced chemical vapor deposition vacuum equipment
100pa～1000pa, then depositing system radio-frequency power be 50w～200w, pressure be 100pa～1000pa, carbon-source gas
Gas flow is 10sccm～100sccm, hydrogen gas flow is 1sccm～40sccm and temperature is 300 DEG C～800 DEG C conditions
Under deposited, sedimentation time is 1min～60min, after deposition terminates, closes radio-frequency power supply and heating power supply, stops being passed through carbon
Source gas and hydrogen, are cooled to room temperature, obtain the enhanced foam metal of CNT；
4th, by metal to be welded, pottery and solder paillon foil successively with 200 mesh, 400 mesh, 600 mesh and 800 mesh sand paperings, Ran Houyong
Acetone ultrasonic pretreatment 10min～20min, obtains removing the metal to be welded of surface impurity, removes the pottery of surface impurity and go
Solder paillon foil except surface impurity；
5th, the metal to be welded of surface impurity, the enhanced foam metal of CNT will be removed, remove the solder paillon foil of surface impurity
And remove surface impurity pottery stack successively, obtain part to be welded, part to be welded be placed in vacuum brazing furnace, pressure be 1 ×
10-4Pa～5 × 10-3Pa and brazing temperature are for, under conditions of 700 DEG C～1200 DEG C, insulation 1min～20min, then to lower the temperature
Speed is 2 DEG C/min～10 DEG C/min, and temperature is cooled to room temperature by 700 DEG C～1200 DEG C, that is, complete CNT and strengthen three
The method of dimension structure intermediate layer assistant brazing.
2. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is that the foam metal described in step one is foam copper or nickel foam.
3. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is that the catalyst described in step one is six water nickel nitrates, ferric nitrate, cobalt nitrate, nickel sulfate, iron sulfate or cobaltous sulfate.
4. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is that the carbon-source gas described in step 3 are methane, acetylene or ethanol.
5. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is that the metal to be welded described in step 4 is tc4 titanium alloy, tc10 titanium alloy, tial alloy, rustless steel or gh99 alloy.
6. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is that the pottery described in step 4 is cf/ c composite ceramicses, c/sic pottery, sio2- bn composite ceramicses, sio2Pottery or sio2f/
sio2Pottery.
7. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is that the solder paillon foil described in step 4 is tizrnicu solder paillon foil, ti-cu solder paillon foil, ti-ni solder paillon foil, cu-
Zr solder paillon foil, agcu solder paillon foil or agcuti solder paillon foil.
8. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is in step 2, the foam metal after soaking to be placed in plasma enhanced chemical vapor deposition vacuum equipment, be evacuated to
Pressure is below 30pa, is passed through hydrogen, and regulations hydrogen gas flow is 40sccm, and regulation vacuum pumping rate is by plasma enhancing
In chemical vapor deposition vacuum equipment, pressure is controlled to 200pa, and in pressure for, under 200pa and hydrogen atmosphere, inciting somebody to action in 30min
Temperature heats up most 570 DEG C.
9. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is in step 3 to be passed through carbon-source gas, regulation carbon-source gas gas flow is 40sccm, adjusting hydrogen gas flow is
10sccm, adjusts vacuum pumping rate and pressure in plasma enhanced chemical vapor deposition vacuum equipment is controlled to 700pa, then
Depositing system radio-frequency power be 175w, pressure be 700pa, carbon-source gas gas flow be that 40sccm, hydrogen gas flow are
10sccm and temperature are deposited under the conditions of 570 DEG C, and sedimentation time is 30min, after deposition terminates, close radio-frequency power supply and add
Thermoelectric generator, stops being passed through carbon-source gas and hydrogen, is cooled to room temperature, obtains the enhanced foam metal of CNT.
10. the method that a kind of CNT according to claim 1 strengthens three dimensional structure intermediate layer assistant brazing, its feature
It is to remove the metal to be welded of surface impurity, the enhanced foam metal of CNT, remove the pricker of surface impurity in step 5
The pottery of material paillon foil and removal surface impurity stacks successively, obtains part to be welded, part to be welded is placed in vacuum brazing furnace, in pressure
For 3 × 10-3Pa and brazing temperature are for, under conditions of 930 DEG C, being incubated 10min, then with cooling rate for 5 DEG C/min, by temperature
It is cooled to room temperature by 930 DEG C.
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| CN112404631B (en) * | 2020-10-27 | 2022-06-07 | 哈尔滨工业大学 | Method for soldering dissimilar materials with assistance of carbon nanotube sponge intermediate layer |
| CN112894047A (en) * | 2021-01-15 | 2021-06-04 | 华中科技大学 | Method for improving dissimilar metal fusion soldering joint performance through carbon nano tube |
| 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 |
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