CN105397344B - Growth in situ graphene and CNT strengthen the method for Ti base solders - Google Patents
Growth in situ graphene and CNT strengthen the method for Ti base solders Download PDFInfo
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- CN105397344B CN105397344B CN201510980691.0A CN201510980691A CN105397344B CN 105397344 B CN105397344 B CN 105397344B CN 201510980691 A CN201510980691 A CN 201510980691A CN 105397344 B CN105397344 B CN 105397344B
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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
Growth in situ graphene and CNT strengthen the method for Ti base solders, and the present invention relates to the preparation method of Ti base solders.The invention solves the problems that the problem of existing graphene is difficult to higher dispersed and conventional Ti base solder thermal coefficient of expansion and poor mechanical behavior under high temperature with CNT in Ti base solders.The method of the present invention：First, by solvent of ethanol by TiH2Powder and Ni (NO3)2·6H2O mix, magnetic agitation and be heated to absolute ethyl alcohol volatilization obtain Ni (NO3)2And TiH2Composite powder；2nd, using plasma enhancing process for preparing graphenes by chemical vapour deposition and CNT enhancing TiH2Powder；3rd, the graphene of preparation and CNT are strengthened into TiH2Powder is mixed with metal dust, and graphene and CNT enhancing Ti base solders are obtained after being fully ground.The present invention strengthens the method for Ti base solders for growth in situ graphene and CNT.
Description
Technical field
The present invention relates to the preparation method of Ti base solders.
Background technology
All the time, the connectivity problem of ceramics and metal is all the emphasis of welding technology field research, in numerous connections
In method, soldering is because technique is simple and joint mechanical property is good, the main method as current connection ceramics with metal.Currently,
In many cases, Ceramic and metal joining component needs to use in high temperature environments, and there are some researches show ceramics and metal
The applied at elevated temperature of connecting elements, is critically depend on the mechanical behavior under high temperature of solder, but due to the thermal expansion system of ceramics and metal
Number differs greatly, and the mechanical behavior under high temperature of component can be greatly reduced in the larger residual stress produced in joint；In addition, solder and mother
The interfacial reaction problem of material can also have a strong impact on the mechanical behavior under high temperature of joint.Traditional solder is difficult to solve the above problems, because
The mechanical behavior under high temperature that this reasonably improves solder using reinforcement is very necessary.
In recent years, Novel Carbon Nanomaterials research is very burning hot, and they often have excellent thermal property, electric property
And the characteristic such as mechanical performance, have in fields such as Aero-Space, photoelectric device, electrochemical capacitors before very wide application
Scape.Graphene and CNT have high intensity, toughness, excellent heat endurance, in addition, they have extremely low line swollen
Swollen coefficient, is respectively -8.0 × 10-6K-1、-5.86×10-9K-1, it is for reducing the preferable enhancing of conventional solder linear expansion coefficient
Body.But it is current, the graphene and Carbon Nanotubes Reinforced Composites method prepared using conventional method is more complicated, and graphite
Dispersed poor in composite soldering of alkene and CNT is simultaneously easily reunited, and result in the decline of their physical and chemical performances,
So as to have a strong impact on the mechanical behavior under high temperature of solder.
The content of the invention
The invention solves the problems that existing graphene is difficult to dispersed and conventional Ti base with CNT in Ti base solders
Solder thermal coefficient of expansion is higher and the problem of poor mechanical behavior under high temperature, and provides growth in situ graphene and CNT enhancing Ti
The method of base solder.
Growth in situ graphene and CNT strengthen the method for Ti base solders, specifically follow the steps below：
First, by Ni (NO3)2·6H2O and TiH2Powder is placed in absolute ethyl alcohol and mixed, and is then 80 DEG C~100 in temperature
Under conditions of DEG C, magnetic agitation to absolute ethyl alcohol is all volatilized, then ground, obtains Ni (NO3)2·TiH2Composite powder；
Described Ni (NO3)2·6H2O and TiH2The mass ratio of powder is 1:(1~10)；
2nd, by Ni (NO3)2·TiH2Composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, takes out true
Sky is passed through hydrogen by 10sccm~40sccm of gas flow to below 5Pa, and regulation plasma enhanced chemical vapor deposition is true
Pressure is 100Pa~400Pa in empty device, and in the case where pressure is 100Pa~400Pa and hydrogen atmosphere, with 20 DEG C/min liter
Temperature is warming up to 500 DEG C~560 DEG C by warm speed；
3rd, be passed through methane gas by 10sccm~80sccm of gas flow, the gas flow of regulation hydrogen for 5sccm~
Pressure is 200Pa~800Pa in 20sccm, regulation plasma enhanced chemical vapor deposition vacuum plant, then in radio frequency work(
Rate is that 100W~300W, pressure are 200Pa~800Pa and temperature is to be deposited under conditions of 500 DEG C~560 DEG C, during deposition
Between be 15min~45min；
4th, stop being passed through hydrogen, argon gas is passed through by 15sccm~45sccm of gas flow, regulation methane gas flow is
Pressure is 500Pa~1000Pa in 5sccm~50sccm, regulation plasma enhanced chemical vapor deposition vacuum plant, then
It is that 100W~300W, pressure are 500Pa~1000Pa and temperature is to be sunk under conditions of 500 DEG C~560 DEG C in radio-frequency power
Product, sedimentation time is 15min~45min, after deposition terminates, and stopping is passed through methane gas, cools down under an argon atmosphere, obtains stone
Black alkene and CNT strengthen TiH2Composite powder；
5th, graphene and CNT are strengthened into TiH2Composite powder, TiH2Powder and metal dust are mixed and ground, and are obtained
To growth in situ graphene and CNT enhancing Ti base solders, that is, complete growth in situ graphene and CNT enhancing Ti bases
The method of solder；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiZrCuNi solders, described metal dust is Zr metal dusts, Cu metal dusts and Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiZrCu solders, described metal dust is Zr metal dusts and Cu metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens AgCuTi solders, described metal dust is Cu metal dusts and Ag metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiCuNi solders, described metal dust is Cu metal dusts and Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiNi solders, described metal dust is Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiNiNb solders, described metal dust is Ni metal dusts and Nb metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiCuCo solders, described metal dust is Cu metal dusts and Co metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens SnCuTi solders, described metal dust is Sn metal dusts and Cu metal dusts.
The beneficial effects of the invention are as follows：
The method that growth in situ graphene and CNT of the present invention strengthen Ti base solders, passes through plasma enhanced chemical
CVD method, under conditions of low temperature, in TiH2On be prepared for dispersed graphene and CNT, graphene and
CNT is respectively provided with excellent elevated temperature strength and extremely low linear expansion coefficient, can play dual invigoration effect, Jin Erke
The linear expansion coefficient of Ti base solders is reduced, the mechanical behavior under high temperature of solder is effectively improved.Meanwhile, prepared graphene and carbon is received
Mitron has three-dimensional hybrid structure, can further strengthen the performance of composite soldering.
To sum up the method for growth in situ graphene and CNT enhancing Ti base solders of the present invention has advantages below：
1st, using plasma enhancing chemical gaseous phase depositing process of the present invention, more traditional chemical gaseous phase depositing process can
Operating temperature is greatly reduced.
2nd, graphene and CNT are respectively provided with excellent elevated temperature strength and extremely low linear expansion coefficient in the present invention, can
To play dual invigoration effect, and then the linear expansion coefficient of Ti base solders can be reduced, effectively improve the mechanical behavior under high temperature of solder.
3rd, the present invention is in TiH2Upper in-situ preparation of carbon nanotube and graphene simultaneously, dispersed graphene and carbon nanometer
Pipe has three-dimensional hybrid structure, can strengthen the performance of composite soldering.
The method that the present invention is used is simple, efficient, is adapted to industrial production.
The present invention strengthens the method for Ti base solders for growth in situ graphene and CNT.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：Growth in situ graphene and CNT described in present embodiment strengthen Ti base solders
Method, is specifically followed the steps below：
First, by Ni (NO3)2·6H2O and TiH2Powder is placed in absolute ethyl alcohol and mixed, and is then 80 DEG C~100 in temperature
Under conditions of DEG C, magnetic agitation to absolute ethyl alcohol is all volatilized, then ground, obtains Ni (NO3)2·TiH2Composite powder；
Described Ni (NO3)2·6H2O and TiH2The mass ratio of powder is 1:(1~10)；
2nd, by Ni (NO3)2·TiH2Composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, takes out true
Sky is passed through hydrogen by 10sccm~40sccm of gas flow to below 5Pa, and regulation plasma enhanced chemical vapor deposition is true
Pressure is 100Pa~400Pa in empty device, and in the case where pressure is 100Pa~400Pa and hydrogen atmosphere, with 20 DEG C/min liter
Temperature is warming up to 500 DEG C~560 DEG C by warm speed；
3rd, be passed through methane gas by 10sccm~80sccm of gas flow, the gas flow of regulation hydrogen for 5sccm~
Pressure is 200Pa~800Pa in 20sccm, regulation plasma enhanced chemical vapor deposition vacuum plant, then in radio frequency work(
Rate is that 100W~300W, pressure are 200Pa~800Pa and temperature is to be deposited under conditions of 500 DEG C~560 DEG C, during deposition
Between be 15min~45min；
4th, stop being passed through hydrogen, argon gas is passed through by 15sccm~45sccm of gas flow, regulation methane gas flow is
Pressure is 500Pa~1000Pa in 5sccm~50sccm, regulation plasma enhanced chemical vapor deposition vacuum plant, then
It is that 100W~300W, pressure are 500Pa~1000Pa and temperature is to be sunk under conditions of 500 DEG C~560 DEG C in radio-frequency power
Product, sedimentation time is 15min~45min, after deposition terminates, and stopping is passed through methane gas, cools down under an argon atmosphere, obtains stone
Black alkene and CNT strengthen TiH2Composite powder；
5th, graphene and CNT are strengthened into TiH2Composite powder, TiH2Powder and metal dust are mixed and ground, and are obtained
To growth in situ graphene and CNT enhancing Ti base solders, that is, complete growth in situ graphene and CNT enhancing Ti bases
The method of solder；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiZrCuNi solders, described metal dust is Zr metal dusts, Cu metal dusts and Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiZrCu solders, described metal dust is Zr metal dusts and Cu metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens AgCuTi solders, described metal dust is Cu metal dusts and Ag metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiCuNi solders, described metal dust is Cu metal dusts and Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiNi solders, described metal dust is Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiNiNb solders, described metal dust is Ni metal dusts and Nb metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens TiCuCo solders, described metal dust is Cu metal dusts and Co metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 be growth in situ graphene and
When CNT strengthens SnCuTi solders, described metal dust is Sn metal dusts and Cu metal dusts.
The beneficial effect of present embodiment is：
1st, present embodiment using plasma enhancing chemical gaseous phase depositing process, more traditional chemical gaseous phase depositing process
Operating temperature can be greatly reduced.
2nd, graphene and CNT are respectively provided with excellent elevated temperature strength and extremely low line expansion system in present embodiment
Number, can play dual invigoration effect, and then can reduce the linear expansion coefficient of Ti base solders, effectively improve the high-temperature mechanics of solder
Performance.
3rd, present embodiment is in TiH2Upper in-situ preparation of carbon nanotube and graphene, dispersed graphene and carbon simultaneously
Nanotube has three-dimensional hybrid structure, can strengthen the performance of composite soldering.
The method that present embodiment is used is simple, efficient, is adapted to industrial production.
Embodiment two：Present embodiment from unlike embodiment one：With gas flow in step 2
It is 300Pa to be passed through pressure in hydrogen, regulation plasma enhanced chemical vapor deposition vacuum plant for 20sccm, and is in pressure
Under 300Pa and hydrogen atmosphere, temperature is warming up to 520 DEG C with 20 DEG C/min heating rate.Other and embodiment one
It is identical.
Embodiment three：Unlike one of present embodiment and embodiment one or two：In step 2 with
Gas flow is that 25sccm is passed through hydrogen, and it is 200Pa to adjust pressure in plasma enhanced chemical vapor deposition vacuum plant, and
In the case where pressure is 200Pa and hydrogen atmosphere, temperature is warming up to 550 DEG C with 20 DEG C/min heating rate.Other and specific reality
Apply mode one or two identical.
Embodiment four：Unlike one of present embodiment and embodiment one to three：In step 3 with
Gas flow is that 20sccm is passed through methane gas, and the gas flow of regulation hydrogen is 10sccm.Other and embodiment one
It is identical to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Adjusted in step 3
It is 300Pa to save pressure in plasma enhanced chemical vapor deposition vacuum plant, is then that 200W, pressure are in radio-frequency power
300Pa and temperature is are deposited under conditions of 500 DEG C~560 DEG C, sedimentation time is 20min.Other and embodiment
One to four is identical.
Embodiment six：Unlike one of present embodiment and embodiment one to five：In step 3 with
Gas flow is that 50sccm is passed through methane gas, and the gas flow of regulation hydrogen is 10sccm.Other and embodiment one
It is identical to five.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：Adjusted in step 3
It is 300Pa to save pressure in plasma enhanced chemical vapor deposition vacuum plant, is then that 175W, pressure are in radio-frequency power
300Pa and temperature is are deposited under conditions of 550 DEG C, sedimentation time is 30min.It is other with the phase of embodiment one to six
Together.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：In step 4 with
Gas flow is that 30sccm is passed through argon gas, and regulation methane gas flow is 45sccm.It is other with the phase of embodiment one to seven
Together.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：Adjusted in step 4
Save plasma enhanced chemical vapor deposition vacuum plant in pressure be 1000Pa, then radio-frequency power be 100W~300W,
Pressure is 1000Pa and temperature is to be deposited under conditions of 500 DEG C~560 DEG C, and sedimentation time is 20min.Other and specific reality
Apply mode one to eight identical.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：In step 4 with
Gas flow is that 40sccm is passed through argon gas, and regulation methane gas flow is 50sccm, and regulation PECVD sinks
Pressure is 750Pa in product vacuum plant, then radio-frequency power be 100W~300W, pressure be 750Pa and temperature be 500 DEG C~
Deposited under conditions of 560 DEG C, sedimentation time is 25min.It is other identical with embodiment one to nine.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
Growth in situ graphene described in the present embodiment and CNT strengthen the method for Ti base solders, be specifically according to
What lower step was carried out：
First, by Ni (NO3)2·6H2O and TiH2Powder is placed in absolute ethyl alcohol and mixed, then in the bar that temperature is 100 DEG C
Under part, magnetic agitation to absolute ethyl alcohol is all volatilized, then ground, obtains Ni (NO3)2·TiH2Composite powder；
Described Ni (NO3)2·6H2O and TiH2The mass ratio of powder is 1:5；
2nd, by Ni (NO3)2·TiH2Composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, takes out true
Sky is passed through in hydrogen, regulation plasma enhanced chemical vapor deposition vacuum plant to below 5Pa by 25sccm of gas flow
Pressure is 200Pa, and in the case where pressure is 200Pa and hydrogen atmosphere, temperature is warming up into 550 with 20 DEG C/min heating rate
℃；
3rd, be passed through methane gas by 50sccm of gas flow, the gas flow of regulation hydrogen is 10sccm, regulation etc. from
Pressure is 300Pa in daughter enhancing chemical vapor deposition vacuum plant, then radio-frequency power be 175W, pressure be 300Pa and
Temperature is is deposited under conditions of 550 DEG C, sedimentation time is 30min；
4th, stop being passed through hydrogen, argon gas be passed through by 25sccm of gas flow, regulation methane gas flow is 50sccm,
It is 1000Pa to adjust pressure in plasma enhanced chemical vapor deposition vacuum plant, is then 175W, pressure in radio-frequency power
It is to be deposited under conditions of 550 DEG C for 1000Pa and temperature, sedimentation time is 30min, after deposition terminates, stopping is passed through methane
Gas, is cooled down under an argon atmosphere, obtains graphene and CNT enhancing TiH2Composite powder；
5th, graphene and CNT are strengthened into TiH2Composite powder, TiH2Powder and metal dust are mixed and ground, and are obtained
To growth in situ graphene and CNT enhancing TiNi solders, that is, complete growth in situ graphene and CNT enhancing Ti bases
The method of solder；
Described graphene and CNT enhancing TiH2Composite powder and TiH2The mass ratio of powder is 1:1；Described stone
Black alkene and CNT strengthen TiH2The mass ratio of composite powder and metal dust is 2:3；
Metal dust described in step 5 is Ni metal dusts.
The present embodiment using plasma strengthens chemical gaseous phase depositing process, under conditions of low temperature, in TiH2It is upper to prepare
Dispersed graphene and CNT, graphene and CNT be respectively provided with excellent elevated temperature strength and extremely low line
The coefficient of expansion, can play dual invigoration effect, and then can reduce the linear expansion coefficient of Ti base solders, effectively improve the height of solder
Warm mechanical property.Meanwhile, prepared graphene and CNT has three-dimensional hybrid structure, can further strengthen compound pricker
The performance of material.
Growth in situ graphene and CNT enhancing TiNi solder brazings SiO manufactured in the present embodiment2- BN ceramics and gold
Belong to Nb, obtain high-quality soldered fitting, joint is 89MPa, the high temperature at 600 DEG C and 800 DEG C in the shearing strength of room temperature
Shearing strength respectively reaches 82MPa and 61MPa.Growth in situ graphene and CNT enhancing TiNi solders prepared by embodiment
Thermal coefficient of expansion be 7.3 × 10-6K-1。
Claims (10)
1. growth in situ graphene and CNT strengthen the method for Ti base solders, it is characterised in that it is entered according to following steps
Capable：
First, by Ni (NO3)2·6H2O and TiH2Powder is placed in absolute ethyl alcohol and mixed, then in the bar that temperature is 80 DEG C~100 DEG C
Under part, magnetic agitation to absolute ethyl alcohol is all volatilized, then ground, obtains Ni (NO3)2·TiH2Composite powder；
Described Ni (NO3)2·6H2O and TiH2The mass ratio of powder is 1:(1~10)；
2nd, by Ni (NO3)2·TiH2Composite powder is placed in plasma enhanced chemical vapor deposition vacuum plant, is evacuated to
Below 5Pa, hydrogen is passed through by 10sccm~40sccm of gas flow, adjusts plasma enhanced chemical vapor deposition vacuum holding
Middle pressure is put for 100Pa~400Pa, and in the case where pressure is 100Pa~400Pa and hydrogen atmosphere, with 20 DEG C/min heating speed
Temperature is warming up to 500 DEG C~560 DEG C by rate；
3rd, be passed through methane gas by 10sccm~80sccm of gas flow, the gas flow of regulation hydrogen for 5sccm~
Pressure is 200Pa~800Pa in 20sccm, regulation plasma enhanced chemical vapor deposition vacuum plant, then in radio frequency work(
Rate is that 100W~300W, pressure are 200Pa~800Pa and temperature is to be deposited under conditions of 500 DEG C~560 DEG C, during deposition
Between be 15min~45min；
4th, stop being passed through hydrogen, argon gas is passed through by 15sccm~45sccm of gas flow, regulation methane gas flow is
Pressure is 500Pa~1000Pa in 5sccm~50sccm, regulation plasma enhanced chemical vapor deposition vacuum plant, then
It is that 100W~300W, pressure are 500Pa~1000Pa and temperature is to be sunk under conditions of 500 DEG C~560 DEG C in radio-frequency power
Product, sedimentation time is 15min~45min, after deposition terminates, and stopping is passed through methane gas, cools down under an argon atmosphere, obtains stone
Black alkene and CNT strengthen TiH2Composite powder；
5th, graphene and CNT are strengthened into TiH2Composite powder, TiH2Powder and metal dust are mixed and ground, and obtain original
Position growth graphene and CNT enhancing Ti base solders, that is, complete growth in situ graphene and CNT enhancing Ti base solders
Method；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens TiZrCuNi solders, described metal dust is Zr metal dusts, Cu metal dusts and Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens TiZrCu solders, described metal dust is Zr metal dusts and Cu metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens AgCuTi solders, described metal dust is Cu metal dusts and Ag metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens TiCuNi solders, described metal dust is Cu metal dusts and Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens TiNi solders, described metal dust is Ni metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens TiNiNb solders, described metal dust is Ni metal dusts and Nb metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens TiCuCo solders, described metal dust is Cu metal dusts and Co metal dusts；
Growth in situ graphene and CNT the enhancing Ti bases solder obtained in step 5 is that growth in situ graphene and carbon are received
When mitron strengthens SnCuTi solders, described metal dust is Sn metal dusts and Cu metal dusts.
2. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
It is passed through in hydrogen, regulation plasma enhanced chemical vapor deposition vacuum plant and presses by 20sccm of gas flow in step 2
It is 300Pa by force, and in the case where pressure is 300Pa and hydrogen atmosphere, temperature is warming up to 520 DEG C with 20 DEG C/min heating rate.
3. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
It is passed through in hydrogen, regulation plasma enhanced chemical vapor deposition vacuum plant and presses by 25sccm of gas flow in step 2
It is 200Pa by force, and in the case where pressure is 200Pa and hydrogen atmosphere, temperature is warming up to 550 DEG C with 20 DEG C/min heating rate.
4. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
Methane gas is passed through by 20sccm of gas flow in step 3, the gas flow of regulation hydrogen is 10sccm.
5. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
It is 300Pa that pressure in plasma enhanced chemical vapor deposition vacuum plant is adjusted in step 3, is then in radio-frequency power
200W, pressure are 300Pa and temperature is to be deposited under conditions of 500 DEG C~560 DEG C, and sedimentation time is 20min.
6. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
Methane gas is passed through by 50sccm of gas flow in step 3, the gas flow of regulation hydrogen is 10sccm.
7. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
It is 300Pa that pressure in plasma enhanced chemical vapor deposition vacuum plant is adjusted in step 3, is then in radio-frequency power
175W, pressure are 300Pa and temperature is to be deposited under conditions of 550 DEG C, and sedimentation time is 30min.
8. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
Argon gas is passed through by 30sccm of gas flow in step 4, regulation methane gas flow is 45sccm.
9. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
It is 1000Pa that pressure in plasma enhanced chemical vapor deposition vacuum plant is adjusted in step 4, is then in radio-frequency power
100W~300W, pressure are 1000Pa and temperature is to be deposited under conditions of 500 DEG C~560 DEG C, and sedimentation time is 20min.
10. growth in situ graphene according to claim 1 and CNT strengthen the method for Ti base solders, its feature exists
Argon gas is passed through by 40sccm of gas flow in step 4, regulation methane gas flow is 50sccm, and regulation plasma increases
Pressure is 750Pa in extensive chemical vapour deposition vacuum plant, then radio-frequency power be 100W~300W, pressure be 750Pa and
Temperature is is deposited under conditions of 500 DEG C~560 DEG C, sedimentation time is 25min.
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| 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 |
| CN112427759B (en) * | 2020-10-27 | 2022-08-26 | 哈尔滨工业大学 | ZrC-SiC ceramic and TC4 titanium alloy brazing method |
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| EP2396442B1 (en) * | 2009-02-16 | 2012-11-14 | Bayer International SA | An engine or engine part and a method of manufacturing the same |
| CN102383071B (en) * | 2011-11-09 | 2013-01-16 | 哈尔滨工业大学 | Method for preparing carbon nano tube enhanced titanium-base compound material by in-suit reaction |
| CN102534300B (en) * | 2012-02-08 | 2013-04-24 | 哈尔滨工业大学 | Method for preparing in-situ growing carbon nano tube reinforcing TiNi high-temperature solders |
| CN103276322B (en) * | 2013-06-17 | 2015-10-07 | 哈尔滨工业大学 | A kind of preparation method of In-situ grown carbon-nanotube-reinaluminum-base aluminum-base solder |
| CN103831549A (en) * | 2014-03-19 | 2014-06-04 | 哈尔滨工业大学 | Method for preparing carbon nano tube reinforced copper-based composite brazing filler metal based on in-situ reaction |
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