CN109175764A - A kind of method of graphene sponge middle layer assistant brazing - Google Patents
A kind of method of graphene sponge middle layer assistant brazing Download PDFInfo
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- CN109175764A CN109175764A CN201811101772.9A CN201811101772A CN109175764A CN 109175764 A CN109175764 A CN 109175764A CN 201811101772 A CN201811101772 A CN 201811101772A CN 109175764 A CN109175764 A CN 109175764A
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- middle layer
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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
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
-
- 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
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- Mechanical Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
A kind of method of graphene sponge middle layer assistant brazing, the present invention relates to the method fields of soldering C/C composite material.The invention solves the technical problems that in existing C/C composite material soldering connection, residual stress causes greatly reliability low.Method: one, C/C composite material, cleaning are cut；Two, graphene sponge is thinly sliced along the direction for being parallel to cross section；Three, AgCuTi powder brazing alloy is subjected to compressing tablet process；Four, combination assembly compresses；Five, it is brazed.The present invention is generated equally distributed TiC reinforced phase in brazed seam, is refined and enhance brazed seam matrix, while hindering brittleness Cu by Ti reaction in-situ in graphene sponge middle layer and solder2Ti is formed in brazed seam, and then improves the mechanical property of gained connector, and shearing strength can reach 55MPa.The method of the present invention is in C/C composite material soldering connection field.
Description
Technical field
The present invention relates to the method fields of soldering C/C composite material.
Background technique
With the rapid development of space technology, people are increasingly frequent to the exploration and development in cosmic space, deliver various skies
Between station, space probe rocket performance and quantity continue to develop therewith.Jet pipe rises in the energy conversion of rocket engine
To important function, generally require to bear harsh service condition in rocket tube work.Firstly, in service condition
Under, jet pipe is in 2000 DEG C to 3500 DEG C of hot environment, and to bear violent thermal shock.In addition, the Service Environment of high temperature
Often bringing higher has thermal stress caused by thermal gradient.The corrosive gas of high speed is but also its Service Environment is more harsh.
Refractory metal is a kind of traditional rocket nozzle material, but the disadvantage of metal material increases it is also obvious that essentially consisting in it
The weight of rocket engine and its heat-resisting ability are poor.Therefore, high-strength, lightweight novel jet pipe structural material compared to
Traditional metal materials have great advantages, it is considered to be instead of the ideal jet pipe material of certain common metal structural members.
C/C composite material is using carbon as matrix, is a kind of new structural material using continuous carbon fibre as reinforced phase, compared to
Graphite material, it improves intensity and thermal shock resistance, and has lower density, lower thermal expansion coefficient, excellent high temperature
Performance and good resistance to ablation ability.Therefore, C/C composite material has very big excellent as rocket tube material
Gesture.However, due to the molding not easy to be processed of C/C composite material.The jet pipe of complicated shape is difficult to carry out one using C/C composite material
Chemical conversion type, it is therefore desirable to which exploitation is suitable for the connection method of C/C composite material, to realize the processing and manufacturing of complicated shape jet pipe.
C/C composite material is a kind of high-temperature structural material haveing excellent performance.However, because prepared by C/C composite material itself
Complex procedures, the production cycle is long, with high costs, largely constrains further applying for C/C composite material；Meanwhile C/C
Some applications of the composite material in the fields such as aerospace and nuclear energy, it is often necessary to connected with metal to meet certain performances
Demand.Therefore, C/C composite material is applied in practice, is unavoidably related to connectivity problem.For example, passing through small size
C/C composite material itself connection, can solve the difficulty for directly preparing complex-shaped, larger-size C/C composite material；It will
C/C composite material is attached with other metal materials or nonmetallic materials, available to be provided simultaneously with two kinds of material advantages again
The insufficient ideal structures of the person of can overcome the disadvantages that, and production efficiency can also be improved, reduce cost.But, it is generally the case that it is related to C/C
The connection of composite material, and the connection of metal is all unavoidable problem, because requiring C/ during realizing connection
C composite and metal (solder or middle layer) obtain good interface cohesion.
Currently, the connection of C/C composite material, there are difficulty, difficulty is it is on the one hand that liquid metal solder is multiple to C/C
Condensation material wettability of the surface problem, common solder is difficult to soak C/C composite material, and solder can be good on base material surface
Wetting and spreading is to form the premise being reliably connected；On the other hand be due to C/C composite material and metal solder or metallic matrix it
Between thermal expansion coefficient and elasticity modulus there are larger differences, residual thermal stress can be generated in connector, it is serious to reduce joint quality very
It cracks to causing connection rear joint to be destroyed.
Summary of the invention
The invention solves in existing C/C composite material soldering connection, the technology that residual stress causes greatly reliability low is asked
Topic, to provide a kind of method of graphene sponge middle layer assistant brazing.
A kind of method of graphene sponge middle layer assistant brazing, specifically sequentially includes the following steps:
One, C/C composite material is cut into the thin slice with a thickness of 2~3mm, then position to be welded is beaten with sand paper
Mill, places into acetone soln and is cleaned by ultrasonic, obtain C/C composite material to be welded；
Two, graphene sponge is thinly sliced along the direction for being parallel to cross section, obtains graphene sponge middle layer；
Three, AgCuTi powder brazing alloy is subjected to compressing tablet process at room temperature, obtains the button shape solder that diameter is 8~12mm
Piece；
Four, the graphene sponge middle layer that step 2 obtains and the solder piece that step 3 obtains are overlayed into two panels step 1
It is combined assembly between obtained C/C composite material to be welded, and is compressed with graphite block, sample to be welded is obtained；
Five, the sample to be welded for obtaining step 4 is put on the warm table of vacuum brazing furnace, is evacuated down to 5 × 10-3Pa
Heating soldering is carried out, control brazing temperature is 830 DEG C~920 DEG C, and soaking time is 10min~40min, then with 5 DEG C/min
Cooling rate be cooled to room temperature, that is, complete the method for the graphene sponge middle layer assistant brazing.
When cutting in step 2 to graphene sponge, the integrality of guarantee graphene sponge and surface is smooth as far as possible
Property.
When being compressed in step 4 with graphite block, it is ensured that each layer is closely contacted with each other.
The beneficial effects of the present invention are:
A kind of method that the present invention proposes graphene sponge middle layer assistant brazing introduces graphene sea in brazing process
Silk floss is used as middle layer, and connection method is simple and effective, and graphene sponge middle layer preparation process is efficiently feasible.By with AgCuTi pricker
Material occur reaction in-situ generate in brazed seam equally distributed TiC phase, due to TiC phase have lower linear expansion coefficient and preferably
Plastic deformation ability, therefore the thermal expansion coefficient of brazed seam can be adjusted, refine and enhance brazed seam matrix, while can be with
Alleviate connector residual stress by plastic deformation.
After present invention introduces graphene sponges as middle layer, brittleness Cu can be hindered2Ti is formed in brazed seam, conversion zone
Continuous and thickness is moderate, significantly reduces connector stress and concentrates, to improve the mechanical property of gained connector, shearing strength be can reach
55MPa。
The method of the present invention is in C/C composite material soldering connection field.
Detailed description of the invention
Fig. 1 is that embodiment one introduces the jointing after the C/C composite material soldering that graphene sponge middle layer obtains
Microstructure back scattering picture；
Fig. 2 is the jointing that comparative test is not introduced into after the C/C composite material soldering that graphene sponge middle layer obtains
Microstructure back scattering picture.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between any combination.
Specific embodiment 1: a kind of method of graphene sponge middle layer assistant brazing of present embodiment, it is specific by with
Lower step carries out:
One, C/C composite material is cut into the thin slice with a thickness of 2~3mm, then position to be welded is beaten with sand paper
Mill, places into acetone soln and is cleaned by ultrasonic, obtain C/C composite material to be welded；
Two, graphene sponge is thinly sliced along the direction for being parallel to cross section, obtains graphene sponge middle layer；
Three, AgCuTi powder brazing alloy is subjected to compressing tablet process at room temperature, obtains the button shape solder that diameter is 8~12mm
Piece；
Four, the graphene sponge middle layer that step 2 obtains and the solder piece that step 3 obtains are overlayed into two panels step 1
It is combined assembly between obtained C/C composite material to be welded, and is compressed with graphite block, sample to be welded is obtained；
Five, the sample to be welded for obtaining step 4 is put on the warm table of vacuum brazing furnace, is evacuated down to 5 × 10-3Pa
Heating soldering is carried out, control brazing temperature is 830 DEG C~920 DEG C, and soaking time is 10min~40min, then with 5 DEG C/min
Cooling rate be cooled to room temperature, that is, complete the method for the graphene sponge middle layer assistant brazing.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: electric spark is used in step 1
Wire cutting machine cuts C/C composite material.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: it is successively adopted in step 1
It is polished with 240#, 600# and 1000# sand paper position to be welded.It is other same as the specific embodiment one.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: in step 1
It is cleaned by ultrasonic 20min in acetone soln.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: being adopted in step 2
Graphene sponge is cut with stainless steel blade.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: stone in step 2
Black alkene sponge middle layer with a thickness of 0.3~6mm.It is other identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: being adopted in step 3
Compressing tablet process is carried out with tablet press machine.It is other identical as one of specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: in step 3
The quality of AgCuTi powder brazing alloy is 0.2g.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: being pressed in step 3
When piece, it is 2MPa that control, which applies pressure, keeps 2~3min.It is other identical as one of specific embodiment one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: will in step 1
C/C composite material is cut into having a size of 5mm × 5mm × 3mm and 10mm × 10mm × 3mm two panels C/C composite material to be welded, step
Graphene sponge middle layer, the step that will be obtained having a size of 10mm × 10mm × 3mm C/C composite material to be welded, step 2 in four
Three obtained solder pieces and having a size of 5mm × 5mm × 3mm C/C composite material to be welded, successively stack and are combined assembly, be used in combination
Graphite block compresses.It is other identical as one of specific embodiment one to nine.
Specific embodiment 11: unlike one of present embodiment and specific embodiment one to ten: in step 5
Controlling brazing temperature is 890 DEG C, soaking time 20min.It is other identical as one of specific embodiment one to ten.
Specific embodiment 12: present embodiment is unlike specific embodiment one to one of 11: step 5
Middle control brazing temperature is 830 DEG C, soaking time 20min.It is other identical as specific embodiment one to one of 11.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
A kind of method of graphene sponge middle layer assistant brazing of the present embodiment, specifically sequentially includes the following steps:
One, C/C composite material is cut into having a size of 5mm × 5mm × 3mm and 10mm using electric spark wire cutting machine ×
Then two plate sheet of 10mm × 3mm successively polishes to position to be welded using 240#, 600# and 1000# sand paper, places into third
Ultrasonic cleaning 20min is carried out in ketone solution, obtains C/C composite material to be welded；
Two, graphene sponge is cut into along the direction for being parallel to cross section with a thickness of the thin of 3mm using stainless steel blade
Piece obtains graphene sponge middle layer；
Three, 0.2g AgCuTi powder brazing alloy is carried out at room temperature by compressing tablet process using tablet press machine, control applies pressure and is
2MPa keeps 2min, obtains the button shape solder piece that diameter is 10mm；
Four, among the graphene sponge that will be obtained having a size of 10mm × 10mm × 3mm C/C composite material to be welded, step 2
Layer, the obtained solder piece of step 3 and having a size of 5mm × 5mm × 3mm C/C composite material to be welded, successively stack and are combined dress
Match, and compressed with graphite block, obtains sample to be welded；
Five, the sample to be welded for obtaining step 4 is put on the warm table of vacuum brazing furnace, is evacuated down to 5 × 10-3Pa
Heating soldering is carried out, control brazing temperature is 890 DEG C, soaking time 20min, then cooling with the cooling rate of 5 DEG C/min
To room temperature, that is, complete the method for the graphene sponge middle layer assistant brazing.
The present embodiment introduces microcosmic group of the jointing after the C/C composite material soldering that graphene sponge middle layer obtains
It is as shown in Figure 1 to knit back scattering picture；
Comparative experiments:
This comparative experiments specifically sequentially includes the following steps:
One, C/C composite material is cut into having a size of 5mm × 5mm × 3mm and 10mm using electric spark wire cutting machine ×
Then two plate sheet of 10mm × 3mm successively polishes to position to be welded using 240#, 600# and 1000# sand paper, places into third
Ultrasonic cleaning 20min is carried out in ketone solution, obtains C/C composite material to be welded；
Two, 0.2g AgCuTi powder brazing alloy is carried out at room temperature by compressing tablet process using tablet press machine, control applies pressure and is
2MPa keeps 2min, obtains the button shape solder piece that diameter is 10mm；
Three, will having a size of the solder piece that 10mm × 10mm × 3mm C/C composite material to be welded, step 2 obtain and having a size of
5mm × 5mm × 3mm C/C composite material to be welded, successively stacks and is combined assembly, and compressed with graphite block, obtain examination to be welded
Sample；
Four, the sample to be welded for obtaining step 3 is put on the warm table of vacuum brazing furnace, is evacuated down to 5 × 10-3Pa
Heating soldering is carried out, control brazing temperature is 890 DEG C, soaking time 20min, then cooling with the cooling rate of 5 DEG C/min
To room temperature, soldering is completed.
This comparative test is not introduced into the micro- of the jointing after the C/C composite material soldering that graphene sponge middle layer obtains
It is as shown in Figure 2 to see tissue back scattering picture.
By Fig. 1 and Fig. 2 comparison it can be found that the addition of graphene interlayers effectively inhibits brittleness Cu in brazed seam2Tiization
The generation of object is closed, while the TiC striped generated after graphene interlayers is added mutually to have the function of refining brazing seam structure, makes brazed seam
Microstructure homogenization is effectively improved joint performance.
Shearing test, loading velocity 0.5mm/min are carried out using electronic universal tester, the present embodiment uses graphene
The resulting jointing room temperature shear strength of sponge middle layer assisted brazing method reaches 55MPa.And under identical parameters, it is not introduced into
Middle layer is directly brazed resulting jointing room temperature shear strength and there was only 35MPa.
Embodiment two:
A kind of method of graphene sponge middle layer assistant brazing of the present embodiment, specifically sequentially includes the following steps:
One, C/C composite material is cut into having a size of 5mm × 5mm × 3mm and 10mm using electric spark wire cutting machine ×
Then two plate sheet of 10mm × 3mm successively polishes to position to be welded using 240#, 600# and 1000# sand paper, places into third
Ultrasonic cleaning 20min is carried out in ketone solution, obtains C/C composite material to be welded；
Two, graphene sponge is cut into along the direction for being parallel to cross section with a thickness of the thin of 3mm using stainless steel blade
Piece obtains graphene sponge middle layer；
Three, 0.2g AgCuTi powder brazing alloy is carried out at room temperature by compressing tablet process using tablet press machine, control applies pressure and is
2MPa keeps 2min, obtains the button shape solder piece that diameter is 10mm；
Four, among the graphene sponge that will be obtained having a size of 10mm × 10mm × 3mm C/C composite material to be welded, step 2
Layer, the obtained solder piece of step 3 and having a size of 5mm × 5mm × 3mm C/C composite material to be welded, successively stack and are combined dress
Match, and compressed with graphite block, obtains sample to be welded；
Five, the sample to be welded for obtaining step 4 is put on the warm table of vacuum brazing furnace, is evacuated down to 5 × 10-3Pa
Heating soldering is carried out, control brazing temperature is 830 DEG C, soaking time 20min, then cooling with the cooling rate of 5 DEG C/min
To room temperature, that is, complete the method for the graphene sponge middle layer assistant brazing.
Shearing test, loading velocity 0.5mm/min are carried out using electronic universal tester, the present embodiment uses graphene
The resulting jointing room temperature shear strength of sponge middle layer assisted brazing method reaches 36MPa.And under identical parameters, it is not introduced into
Middle layer is directly brazed resulting jointing room temperature shear strength and there was only 24MPa.
Embodiment three:
A kind of method of graphene sponge middle layer assistant brazing of the present embodiment, specifically sequentially includes the following steps:
One, C/C composite material is cut into having a size of 5mm × 5mm × 3mm and 10mm using electric spark wire cutting machine ×
Then two plate sheet of 10mm × 3mm successively polishes to position to be welded using 240#, 600# and 1000# sand paper, places into third
Ultrasonic cleaning 20min is carried out in ketone solution, obtains C/C composite material to be welded；
Two, graphene sponge is cut into along the direction for being parallel to cross section with a thickness of the thin of 3mm using stainless steel blade
Piece obtains graphene sponge middle layer；
Three, 0.2g AgCuTi powder brazing alloy is carried out at room temperature by compressing tablet process using tablet press machine, control applies pressure and is
2MPa keeps 2min, obtains the button shape solder piece that diameter is 10mm；
Four, among the graphene sponge that will be obtained having a size of 10mm × 10mm × 3mm C/C composite material to be welded, step 2
Layer, the obtained solder piece of step 3 and having a size of 5mm × 5mm × 3mm C/C composite material to be welded, successively stack and are combined dress
Match, and compressed with graphite block, obtains sample to be welded；
Five, the sample to be welded for obtaining step 4 is put on the warm table of vacuum brazing furnace, is evacuated down to 5 × 10-3Pa
Heating soldering is carried out, control brazing temperature is 890 DEG C, soaking time 40min, then cooling with the cooling rate of 5 DEG C/min
To room temperature, that is, complete the method for the graphene sponge middle layer assistant brazing.
Shearing test, loading velocity 0.5mm/min are carried out using electronic universal tester, the present embodiment uses graphene
The resulting jointing room temperature shear strength of sponge middle layer assisted brazing method reaches 46MPa.And under identical parameters, it is not introduced into
Middle layer is directly brazed resulting jointing room temperature shear strength and there was only 37MPa.
Claims (10)
1. a kind of method of graphene sponge middle layer assistant brazing, it is characterised in that this method specifically sequentially includes the following steps:
One, C/C composite material is cut into the thin slice with a thickness of 2~3mm, is then polished with sand paper position to be welded, then
It is put into acetone soln and is cleaned by ultrasonic, obtain C/C composite material to be welded；
Two, graphene sponge is thinly sliced along the direction for being parallel to cross section, obtains graphene sponge middle layer；
Three, AgCuTi powder brazing alloy is subjected to compressing tablet process at room temperature, obtains the button shape solder piece that diameter is 8~12mm；
Four, the graphene sponge middle layer that step 2 obtains and the solder piece that step 3 obtains two panels step 1 is overlayed to obtain
C/C composite material to be welded between be combined assembly, and compressed with graphite block, obtain sample to be welded；
Five, the sample to be welded for obtaining step 4 is put on the warm table of vacuum brazing furnace, is evacuated down to 5 × 10-3Pa is carried out
Heating soldering, control brazing temperature are 830 DEG C~920 DEG C, and soaking time is 10min~40min, then with the drop of 5 DEG C/min
Warm speed is cooled to room temperature, that is, completes the method for the graphene sponge middle layer assistant brazing.
2. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 1
It is middle that C/C composite material is cut using electric spark wire cutting machine.
3. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 1
In successively polished position to be welded using 240#, 600# and 1000# sand paper.
4. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 1
In be cleaned by ultrasonic 20min in acetone soln.
5. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 2
Middle graphene sponge middle layer with a thickness of 0.3~6mm.
6. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 3
The quality of middle AgCuTi powder brazing alloy is 0.2g.
7. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 3
When middle tabletting, it is 2MPa that control, which applies pressure, keeps 2~3min.
8. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 1
It is middle that C/C composite material is cut into having a size of 5mm × 5mm × 3mm and 10mm × 10mm × 3mm two panels C/C composite material to be welded,
In step 4 will having a size of the graphene sponge middle layer that 10mm × 10mm × 3mm C/C composite material to be welded, step 2 obtain,
Solder piece that step 3 obtains and having a size of 5mm × 5mm × 3mm C/C composite material to be welded, successively stacks and is combined assembly,
And it is compressed with graphite block.
9. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 5
Middle control brazing temperature is 890 DEG C, soaking time 20min.
10. a kind of method of graphene sponge middle layer assistant brazing according to claim 1, it is characterised in that step 5
Middle control brazing temperature is 830 DEG C, soaking time 20min.
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| CN110315159A (en) * | 2019-07-19 | 2019-10-11 | 哈尔滨工业大学 | A kind of manufacturing method of hard alloy steel compound tool |
| CN112404631A (en) * | 2020-10-27 | 2021-02-26 | 哈尔滨工业大学 | Method for soldering dissimilar materials with assistance of carbon nanotube sponge intermediate layer |
| 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 |
| CN112935621A (en) * | 2021-01-20 | 2021-06-11 | 西安理工大学 | Welding wire for graphene-enhanced TA1-Q345 middle layer and preparation method |
| CN112935621B (en) * | 2021-01-20 | 2022-05-31 | 西安理工大学 | Welding wire for graphene-enhanced TA1-Q345 middle layer and preparation method |
| CN113430414A (en) * | 2021-06-25 | 2021-09-24 | 哈尔滨工业大学 | Method for improving high-temperature oxidation resistance of AgCu alloy by using three-dimensional network reinforcing phase |
| CN113430414B (en) * | 2021-06-25 | 2022-03-01 | 哈尔滨工业大学 | Method for improving high-temperature oxidation resistance of AgCu alloy by using three-dimensional network reinforcing phase |
| CN115556436A (en) * | 2022-12-07 | 2023-01-03 | 长沙威尔保新材料有限公司 | Preparation method of multilayer alloy wear-resistant composite material |
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