CN105397344A - Preparation method of in-situ growth graphene/carbon nano tube reinforced Ti-based brazing filler metal - Google Patents
Preparation method of in-situ growth graphene/carbon nano tube reinforced Ti-based brazing filler metal Download PDFInfo
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- CN105397344A CN105397344A CN201510980691.0A CN201510980691A CN105397344A CN 105397344 A CN105397344 A CN 105397344A CN 201510980691 A CN201510980691 A CN 201510980691A CN 105397344 A CN105397344 A CN 105397344A
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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Abstract
The invention relates to a preparation method of Ti-based brazing filler metal, in particular to a preparation method of in-situ growth graphene/carbon nano tube reinforced Ti-based brazing filler metal, so as to solve the problems that the conventional graphene and carbon nano tubes can not be dispersed easily or uniformly in the Ti-based brazing filler metal and the traditional Ti-based brazing filler metal is high in thermal expansion coefficient and poor in high temperature mechanical properties. The preparation method of the in-situ growth graphene/carbon nano tube reinforced Ti-based brazing filler metal comprises the steps that firstly, TiH2 powder is mixed with Ni(NO3)2.6H2O by taking alcohol as a solvent, magnetic stirring and heating are conducted till absolute ethyl alcohol is volatilized and Ni(NO3)2/TiH2 composite powder is obtained; secondly, graphene/carbon nano tube reinforced TiH2 powder is prepared by adopting a plasma-enhanced chemical vapor deposition method; and thirdly, the prepared graphene/carbon nano tube reinforced TiH2 powder is mixed with metal powder and abraded sufficiently, and the graphene/carbon nano tube reinforced Ti-based brazing filler metal is obtained. The above scheme is applied to the preparation method of the in-situ growth graphene/carbon nano tube reinforced Ti-based brazing filler metal.
Description
Technical field
The present invention relates to the preparation method of Ti base solder.
Background technology
All the time, pottery and the connectivity problem of metal are all the emphasis of welding technology field research, and in numerous methods of attachment, soldering, because technique is simple and joint mechanical property is good, becomes the current main method connecting pottery and metal.Current, in many cases, Ceramic and metal joining component needs to use in high temperature environments, there are some researches show, the applied at elevated temperature of Ceramic and metal joining component, key depends on the mechanical behavior under high temperature of solder, but due to the thermal expansion coefficient difference of pottery and metal comparatively large, significantly can reduce the mechanical behavior under high temperature of component in the larger residual stress of joint generation; In addition, the interfacial reaction problem of solder and mother metal also can have a strong impact on the mechanical behavior under high temperature of joint.Traditional solder is difficult to solve the problem, and therefore reasonably adopts reinforcement to improve the mechanical behavior under high temperature of solder very necessary.
In recent years, Novel Carbon Nanomaterials research is very burning hot, and they often have the characteristics such as excellent thermal property, electric property and mechanical performance, have very wide application prospect in fields such as Aero-Space, photoelectric device, electrochemical capacitors.Graphene and CNT have high intensity, toughness, excellent heat endurance, and in addition, they have extremely low linear expansion coefficient, are respectively-8.0 × 10
-6k
-1,-5.86 × 10
-9k
-1, be used to the desirable reinforcement reducing conventional solder linear expansion coefficient.But it is current, the graphene/carbon nano-tube reinforced composite Measures compare adopting conventional method to prepare is complicated, and Graphene and the CNT dispersiveness in composite soldering is poor and easily reunite, result in the decline of their physical and chemical performances, thus have a strong impact on the mechanical behavior under high temperature of solder.
Summary of the invention
The present invention will solve existing Graphene and CNT is difficult to dispersed and that conventional Ti base solder thermal coefficient of expansion is higher and mechanical behavior under high temperature is poor problem in Ti base solder, and provides growth in situ graphene/carbon nano-tube to strengthen the method for Ti base solder.
Growth in situ graphene/carbon nano-tube strengthens the method for Ti base solder, specifically carries out according to following steps:
One, by Ni (NO
3)
26H
2o and TiH
2powder is placed in absolute ethyl alcohol and mixes, and is then that under the condition of 80 DEG C ~ 100 DEG C, magnetic agitation is all volatilized to absolute ethyl alcohol in temperature, then through grinding, obtains Ni (NO
3)
2tiH
2composite powder;
Described Ni (NO
3)
26H
2o and TiH
2the mass ratio of powder is 1:(1 ~ 10);
Two, by Ni (NO
3)
2tiH
2composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, be evacuated to below 5Pa, be that 10sccm ~ 40sccm passes into hydrogen with gas flow, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 100Pa ~ 400Pa, and under pressure is 100Pa ~ 400Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 500 DEG C ~ 560 DEG C;
Three, be that 10sccm ~ 80sccm passes into methane gas with gas flow, the gas flow regulating hydrogen is 5sccm ~ 20sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa ~ 800Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 200Pa ~ 800Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 15min ~ 45min;
Four, stop passing into hydrogen, be that 15sccm ~ 45sccm passes into argon gas with gas flow, methane gas flow is regulated to be 5sccm ~ 50sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 500Pa ~ 1000Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 500Pa ~ 1000Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 15min ~ 45min, after deposition terminates, stop passing into methane gas, cool under an argon atmosphere, obtain graphene/carbon nano-tube and strengthen TiH
2composite powder;
Five, graphene/carbon nano-tube is strengthened TiH
2composite powder, TiH
2powder and metal dust mix and grind, and obtain growth in situ graphene/carbon nano-tube and strengthen Ti base solder, namely complete the method that growth in situ graphene/carbon nano-tube strengthens Ti base solder;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiZrCuNi solder, described metal dust is Zr metal dust, Cu metal dust and Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiZrCu solder, described metal dust is Zr metal dust and Cu metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing AgCuTi solder, described metal dust is Cu metal dust and Ag metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiCuNi solder, described metal dust is Cu metal dust and Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiNi solder, described metal dust is Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiNiNb solder, described metal dust is Ni metal dust and Nb metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiCuCo solder, described metal dust is Cu metal dust and Co metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing SnCuTi solder, described metal dust is Sn metal dust and Cu metal dust.
The invention has the beneficial effects as follows:
Growth in situ graphene/carbon nano-tube of the present invention strengthens the method for Ti base solder, by plasma enhanced chemical vapor deposition method, under the condition of low temperature, in TiH
2on prepared homodisperse Graphene and CNT, Graphene and CNT all have excellent elevated temperature strength and extremely low linear expansion coefficient, dual invigoration effect can be played, and then the linear expansion coefficient of Ti base solder can be reduced, effectively improve the mechanical behavior under high temperature of solder.Meanwhile, prepared graphene/carbon nano-tube has three-dimensional hybrid structure, can strengthen the performance of composite soldering further.
To sum up the method for growth in situ graphene/carbon nano-tube enhancing Ti base solder of the present invention has the following advantages:
1, using plasma of the present invention strengthens chemical gaseous phase depositing process, and more traditional chemical gaseous phase depositing process significantly can reduce operating temperature.
2, in the present invention, Graphene and CNT all have excellent elevated temperature strength and extremely low linear expansion coefficient, can play dual invigoration effect, and then can reduce the linear expansion coefficient of Ti base solder, effectively improve the mechanical behavior under high temperature of solder.
3, the present invention is at TiH
2in-situ preparation of carbon nanotube and Graphene while of upper, homodisperse graphene/carbon nano-tube has three-dimensional hybrid structure, can strengthen the performance of composite soldering.
The method that the present invention adopts is simple, efficient, is applicable to industrial production.
The present invention is used for the method that growth in situ graphene/carbon nano-tube strengthens Ti base solder.
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 growth in situ graphene/carbon nano-tube described in present embodiment strengthens the method for Ti base solder, specifically carries out according to following steps:
One, by Ni (NO
3)
26H
2o and TiH
2powder is placed in absolute ethyl alcohol and mixes, and is then that under the condition of 80 DEG C ~ 100 DEG C, magnetic agitation is all volatilized to absolute ethyl alcohol in temperature, then through grinding, obtains Ni (NO
3)
2tiH
2composite powder;
Described Ni (NO
3)
26H
2o and TiH
2the mass ratio of powder is 1:(1 ~ 10);
Two, by Ni (NO
3)
2tiH
2composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, be evacuated to below 5Pa, be that 10sccm ~ 40sccm passes into hydrogen with gas flow, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 100Pa ~ 400Pa, and under pressure is 100Pa ~ 400Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 500 DEG C ~ 560 DEG C;
Three, be that 10sccm ~ 80sccm passes into methane gas with gas flow, the gas flow regulating hydrogen is 5sccm ~ 20sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa ~ 800Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 200Pa ~ 800Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 15min ~ 45min;
Four, stop passing into hydrogen, be that 15sccm ~ 45sccm passes into argon gas with gas flow, methane gas flow is regulated to be 5sccm ~ 50sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 500Pa ~ 1000Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 500Pa ~ 1000Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 15min ~ 45min, after deposition terminates, stop passing into methane gas, cool under an argon atmosphere, obtain graphene/carbon nano-tube and strengthen TiH
2composite powder;
Five, graphene/carbon nano-tube is strengthened TiH
2composite powder, TiH
2powder and metal dust mix and grind, and obtain growth in situ graphene/carbon nano-tube and strengthen Ti base solder, namely complete the method that growth in situ graphene/carbon nano-tube strengthens Ti base solder;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiZrCuNi solder, described metal dust is Zr metal dust, Cu metal dust and Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiZrCu solder, described metal dust is Zr metal dust and Cu metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing AgCuTi solder, described metal dust is Cu metal dust and Ag metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiCuNi solder, described metal dust is Cu metal dust and Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiNi solder, described metal dust is Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiNiNb solder, described metal dust is Ni metal dust and Nb metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiCuCo solder, described metal dust is Cu metal dust and Co metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing SnCuTi solder, described metal dust is Sn metal dust and Cu metal dust.
The beneficial effect of present embodiment is:
1, present embodiment using plasma strengthens chemical gaseous phase depositing process, and more traditional chemical gaseous phase depositing process significantly can reduce operating temperature.
2, in present embodiment, Graphene and CNT all have excellent elevated temperature strength and extremely low linear expansion coefficient, can play dual invigoration effect, and then can reduce the linear expansion coefficient of Ti base solder, effectively improve the mechanical behavior under high temperature of solder.
3, present embodiment is at TiH
2in-situ preparation of carbon nanotube and Graphene while of upper, homodisperse graphene/carbon nano-tube has three-dimensional hybrid structure, can strengthen the performance of composite soldering.
The method that present embodiment adopts is simple, efficient, is applicable to industrial production.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: be that 20sccm passes into hydrogen with gas flow in step 2, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 300Pa, and under pressure is 300Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 520 DEG C.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: be that 25sccm passes into hydrogen with gas flow in step 2, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa, and under pressure is 200Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 550 DEG C.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: be that 20sccm passes into methane gas with gas flow in step 3, regulate the gas flow of hydrogen to be 10sccm.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: regulate pressure in plasma enhanced chemical vapor deposition vacuum plant to be 300Pa in step 3, then radio-frequency power be 200W, pressure deposits under be 300Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 20min.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: be that 50sccm passes into methane gas with gas flow in step 3, regulate the gas flow of hydrogen to be 10sccm.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 pressure in plasma enhanced chemical vapor deposition vacuum plant to be 300Pa in step 3, then radio-frequency power be 175W, pressure deposits under be 300Pa and temperature being the condition of 550 DEG C, sedimentation time is 30min.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: be that 30sccm passes into argon gas with gas flow in step 4, regulate methane gas flow to be 45sccm.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 plasma enhanced chemical vapor deposition vacuum plant to be 1000Pa in step 4, then radio-frequency power be 100W ~ 300W, pressure deposits under be 1000Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 20min.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: be that 40sccm passes into argon gas with gas flow in step 4, methane gas flow is regulated to be 50sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 750Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 750Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 25min.Other is identical with detailed description of the invention one to nine.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
Growth in situ graphene/carbon nano-tube described in the present embodiment strengthens the method for Ti base solder, specifically carries out according to following steps:
One, by Ni (NO
3)
26H
2o and TiH
2powder is placed in absolute ethyl alcohol and mixes, and is then that under the condition of 100 DEG C, magnetic agitation is all volatilized to absolute ethyl alcohol in temperature, then through grinding, obtains Ni (NO
3)
2tiH
2composite powder;
Described Ni (NO
3)
26H
2o and TiH
2the mass ratio of powder is 1:5;
Two, by Ni (NO
3)
2tiH
2composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, be evacuated to below 5Pa, be that 25sccm passes into hydrogen with gas flow, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa, and under pressure is 200Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 550 DEG C;
Three, be that 50sccm passes into methane gas with gas flow, the gas flow regulating hydrogen is 10sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 300Pa, then radio-frequency power be 175W, pressure deposits under be 300Pa and temperature being the condition of 550 DEG C, sedimentation time is 30min;
Four, stop passing into hydrogen, be that 25sccm passes into argon gas with gas flow, methane gas flow is regulated to be 50sccm, regulate pressure in plasma enhanced chemical vapor deposition vacuum plant to be 1000Pa, then radio-frequency power be 175W, pressure deposits under be 1000Pa and temperature being the condition of 550 DEG C, sedimentation time is 30min, after deposition terminates, stop passing into methane gas, cool under an argon atmosphere, obtain graphene/carbon nano-tube and strengthen TiH
2composite powder;
Five, graphene/carbon nano-tube is strengthened TiH
2composite powder, TiH
2powder and metal dust mix and grind, and obtain growth in situ graphene/carbon nano-tube and strengthen TiNi solder, namely complete the method that growth in situ graphene/carbon nano-tube strengthens Ti base solder;
Described graphene/carbon nano-tube strengthens TiH
2composite powder and TiH
2the mass ratio of powder is 1:1; Described graphene/carbon nano-tube strengthens TiH
2the mass ratio of composite powder and metal dust is 2:3;
Metal dust described in step 5 is Ni metal dust.
The present embodiment using plasma strengthens chemical gaseous phase depositing process, under the condition of low temperature, in TiH
2on prepared homodisperse Graphene and CNT, Graphene and CNT all have excellent elevated temperature strength and extremely low linear expansion coefficient, dual invigoration effect can be played, and then the linear expansion coefficient of Ti base solder can be reduced, effectively improve the mechanical behavior under high temperature of solder.Meanwhile, prepared graphene/carbon nano-tube has three-dimensional hybrid structure, can strengthen the performance of composite soldering further.
Growth in situ graphene/carbon nano-tube prepared by the present embodiment strengthens TiNi solder brazing SiO
2-BN pottery and metal Nb, obtain high-quality soldered fitting, joint is 89MPa in the shearing strength of room temperature, and the high temperature shearing strength at 600 DEG C and 800 DEG C reaches 82MPa and 61MPa respectively.The thermal coefficient of expansion that growth in situ graphene/carbon nano-tube prepared by embodiment strengthens TiNi solder is 7.3 × 10
-6k
-1.
Claims (10)
1. growth in situ graphene/carbon nano-tube strengthens the method for Ti base solder, it is characterized in that it carries out according to following steps:
One, by Ni (NO
3)
26H
2o and TiH
2powder is placed in absolute ethyl alcohol and mixes, and is then that under the condition of 80 DEG C ~ 100 DEG C, magnetic agitation is all volatilized to absolute ethyl alcohol in temperature, then through grinding, obtains Ni (NO
3)
2tiH
2composite powder;
Described Ni (NO
3)
26H
2o and TiH
2the mass ratio of powder is 1:(1 ~ 10);
Two, by Ni (NO
3)
2tiH
2composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, be evacuated to below 5Pa, be that 10sccm ~ 40sccm passes into hydrogen with gas flow, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 100Pa ~ 400Pa, and under pressure is 100Pa ~ 400Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 500 DEG C ~ 560 DEG C;
Three, be that 10sccm ~ 80sccm passes into methane gas with gas flow, the gas flow regulating hydrogen is 5sccm ~ 20sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa ~ 800Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 200Pa ~ 800Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 15min ~ 45min;
Four, stop passing into hydrogen, be that 15sccm ~ 45sccm passes into argon gas with gas flow, methane gas flow is regulated to be 5sccm ~ 50sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 500Pa ~ 1000Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 500Pa ~ 1000Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 15min ~ 45min, after deposition terminates, stop passing into methane gas, cool under an argon atmosphere, obtain graphene/carbon nano-tube and strengthen TiH
2composite powder;
Five, graphene/carbon nano-tube is strengthened TiH
2composite powder, TiH
2powder and metal dust mix and grind, and obtain growth in situ graphene/carbon nano-tube and strengthen Ti base solder, namely complete the method that growth in situ graphene/carbon nano-tube strengthens Ti base solder;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiZrCuNi solder, described metal dust is Zr metal dust, Cu metal dust and Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiZrCu solder, described metal dust is Zr metal dust and Cu metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing AgCuTi solder, described metal dust is Cu metal dust and Ag metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiCuNi solder, described metal dust is Cu metal dust and Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiNi solder, described metal dust is Ni metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiNiNb solder, described metal dust is Ni metal dust and Nb metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing TiCuCo solder, described metal dust is Cu metal dust and Co metal dust;
When the growth in situ graphene/carbon nano-tube enhancing Ti base solder obtained in step 5 is growth in situ graphene/carbon nano-tube enhancing SnCuTi solder, described metal dust is Sn metal dust and Cu metal dust.
2. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that being that 20sccm passes into hydrogen with gas flow in step 2, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 300Pa, and under pressure is 300Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 520 DEG C.
3. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that being that 25sccm passes into hydrogen with gas flow in step 2, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa, and under pressure is 200Pa and hydrogen atmosphere, with the heating rate of 20 DEG C/min by temperature to 550 DEG C.
4. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that being that 20sccm passes into methane gas with gas flow in step 3, and the gas flow regulating hydrogen is 10sccm.
5. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that regulating in step 3 pressure in plasma enhanced chemical vapor deposition vacuum plant to be 300Pa, then radio-frequency power be 200W, pressure deposits under be 300Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 20min.
6. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that being that 50sccm passes into methane gas with gas flow in step 3, and the gas flow regulating hydrogen is 10sccm.
7. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that regulating in step 3 pressure in plasma enhanced chemical vapor deposition vacuum plant to be 300Pa, then radio-frequency power be 175W, pressure deposits under be 300Pa and temperature being the condition of 550 DEG C, sedimentation time is 30min.
8. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that being that 30sccm passes into argon gas with gas flow in step 4, regulates methane gas flow to be 45sccm.
9. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that regulating in step 4 pressure in plasma enhanced chemical vapor deposition vacuum plant to be 1000Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 1000Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 20min.
10. growth in situ graphene/carbon nano-tube according to claim 1 strengthens the method for Ti base solder, it is characterized in that being that 40sccm passes into argon gas with gas flow in step 4, methane gas flow is regulated to be 50sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 750Pa, then radio-frequency power be 100W ~ 300W, pressure deposits under be 750Pa and temperature being the condition of 500 DEG C ~ 560 DEG C, sedimentation time is 25min.
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| CN108620767A (en) * | 2018-05-08 | 2018-10-09 | 哈尔滨工业大学 | A kind of composite soldering and preparation method thereof for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys |
| CN110252030A (en) * | 2019-05-30 | 2019-09-20 | 辽宁兰晶科技有限公司 | A kind of preparation method and application of quantum graphene automobile filter filter material |
| CN110576187A (en) * | 2019-09-19 | 2019-12-17 | 天津大学 | preparation method for in-situ synthesis of three-dimensional graphene/one-dimensional carbon nanotube loaded copper nanoparticle material |
| CN112427759A (en) * | 2020-10-27 | 2021-03-02 | 哈尔滨工业大学 | ZrC-SiC ceramic and TC4 titanium alloy brazing method |
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