CN108274086B - Method for brazing carbon fiber reinforced carbon-based composite material at high temperature by two-step method - Google Patents

Method for brazing carbon fiber reinforced carbon-based composite material at high temperature by two-step method Download PDF

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CN108274086B
CN108274086B CN201810068104.4A CN201810068104A CN108274086B CN 108274086 B CN108274086 B CN 108274086B CN 201810068104 A CN201810068104 A CN 201810068104A CN 108274086 B CN108274086 B CN 108274086B
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composite material
brazing
temperature
vacuum
protective atmosphere
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CN108274086A (en
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曹健
贺宗晶
李淳
董士博
亓钧雷
冯吉才
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Harbin Institute of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/008—Soldering within a furnace
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • 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

Abstract

Two-step high-temperature drill rodA method for welding carbon fiber reinforced carbon-based composite material relates to a method for brazing carbon fiber reinforced carbon-based composite material. The invention aims to solve the problem of the prior art CfThe high-temperature brazing of the/C composite material has poor mechanical property. The invention comprises the following steps: firstly, preparing eutectic Ti-Si brazing filler metal; secondly, preparing brazing filler metal sheets; thirdly, preparation of CfA melt-infiltrated layer of the/C composite; IV, CfAnd (3) brazing the/C composite material. The invention adopts the 14Ti-86Si eutectic solder to realize the pressureless brazing connection of the carbon fiber reinforced carbon-based composite material at high temperature, and the two-step brazing method effectively improves the C contentfThe quality of the connection of the/C composite material. The invention is applied to the field of welding.

Description

Method for brazing carbon fiber reinforced carbon-based composite material at high temperature by two-step method
Technical Field
The invention relates to a method for brazing a carbon fiber reinforced carbon-based composite material.
Background
With the rapid development of science and technology, the requirements for thermal structures and thermal protection materials for spacecrafts at home and abroad are becoming stricter. Carbon fiber reinforced carbon-based composite material (C)fthe/C composite material) has the characteristics of low density, high specific strength, low thermal expansion coefficient, excellent high temperature resistance, excellent ablation resistance and the like, and is widely applied to the field of aerospace, and developed countries such as Europe and America adopt ultra-high temperature components of spacecrafts and solid rocket engines of various types as CfAnd preparing the/C composite material. In order to meet special service environment, the preparation of large-size C with complex shape is urgently neededfthe/C composite material member is limited by a prefabricated body weaving technology and a CVI (chemical vapor infiltration) process, and large and complex C is difficult to directly prepare at low costfa/C composite member. Tong (Chinese character of 'tong')Often, a feasible approach is to secondarily join C of simple shapefthe/C composite material is used for obtaining the required member.
Related to CfThe connection of the/C composite material comprises vacuum hot-pressing sintering, electric field auxiliary sintering, instantaneous liquid phase connection, brazing, diffusion welding, self-propagating reaction and the like. Compared with other connection methods, the brazing reaction time is short, the pressure applied to the base material is small, and the thermal expansion coefficient of the connection material can be regulated and controlled to form CfThe conventional connection methods for the/C composite materials. In the existing report, the solders of Ag-Cu, Ag-Cu-Ti, Ti-Cu-Ni, Ti-Zr-Ni-Cu and the like all realize CfThe medium-low temperature braze welding connection of the/C composite material is not common to the development of the high-temperature braze welding connection, and only Dadras and Salvo et al respectively adopt TiSi2And the Si sheet gives a reliable joint. Ti-Si based material has realized CfThe connection of the vacuum hot-pressing sintering and electric field auxiliary sintering of the/C composite material and other methods has good wettability of titanium to carbon, and the silicon carbide and C generated by the reaction of silicon and carbonfThe thermal expansion coefficient of the/C composite material is approximate, and the Ti-Si material is connected with C at high temperaturefthe/C composite material can obtain a joint with good welding quality. Therefore, the titanium-silicon-based brazing filler metal is adopted to develop the suitable CfA method for high-temperature brazing connection of the/C composite material is necessary.
Disclosure of Invention
The invention aims to solve the problem of the prior art CfThe technical problem of poor mechanical property of high-temperature brazing of the/C composite material is solved, and the method for brazing the carbon fiber reinforced carbon-based composite material at high temperature by the two-step method is provided.
The method for brazing the carbon fiber reinforced carbon-based composite material at high temperature by the two-step method is carried out according to the following steps:
firstly, preparing eutectic Ti-Si brazing filler metal: polishing the surface of the Ti sheet to remove oxide skin, then placing the Ti sheet and the Si block with the oxide skin removed in a copper pot, repeatedly smelting for 5-7 times by adopting vacuum arc smelting equipment, and naturally cooling to room temperature under a vacuum condition to obtain 14Ti-86Si brazing filler metal; the atomic percentage content ratio of the Ti sheet and the Si block for removing the oxide skin is 7: 43;
secondly, preparing brazing filler metal sheets: cutting the 14Ti-86Si brazing filler metal prepared in the first step into sheets by adopting linear cutting equipment, polishing to remove oxide skin, then placing the sheets in absolute ethyl alcohol for ultrasonic cleaning for 5-10 min, and drying to obtain 14Ti-86Si brazing filler metal sheets;
thirdly, preparation of CfInfiltration layer of/C composite: c to be weldedfPlacing the/C composite material in absolute ethyl alcohol for ultrasonic cleaning for 5-10 min, drying, and fixing the 14Ti-86Si brazing filler metal sheet prepared in the step two on the C to be welded by adopting an organic binderfThe surface to be welded of the/C composite material; fixing C to be welded by graphite diefPlacing the/C composite material in a vacuum brazing furnace or an atmosphere furnace, heating to 300 ℃ at the speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 10-30 min under the conditions of vacuum or protective atmosphere and 300 ℃, heating to 1380-1440 ℃ at the speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 10min under the conditions of vacuum or protective atmosphere and 1380-1440 ℃, cooling to 300 ℃ at the speed of 5 ℃/min under vacuum or protective atmosphere, and furnace-cooling to room temperature under vacuum or protective atmosphere to obtain the C with the infiltration layer on the surface to be weldedfa/C composite material;
IV, CfBrazing of the/C composite material: c with two-step three-to-be-welded surface having infiltration layerfthe/C composite material is used as a base material, the 14Ti-86Si brazing filler metal sheet prepared in the step two is fixed between the two base materials by adopting an organic binder, and a sandwich structure is assembled; fixing the base material of the sandwich structure by a graphite mould, placing the base material in a vacuum brazing furnace or an atmosphere furnace, heating to 300 ℃ at a speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 10-30 min under vacuum or protective atmosphere and at a temperature of 300 ℃, heating to 1380-1440 ℃ at a speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 5-120 min under vacuum or protective atmosphere and at a temperature of 1380-1440 ℃, cooling to 300 ℃ at a speed of 5 ℃/min under vacuum or protective atmosphere, and furnace-cooling to room temperature under vacuum or protective atmosphere to finish CfAnd (3) carrying out the whole brazing process of the/C composite material.
The invention has the following beneficial effects:
the invention adopts 14Ti-86Si eutectic solder to realize the carbon fiber reinforced carbon-based composite material (C) at 1380-1440 DEG Cfthe/C composite material) solves the problem of the prior CfThe problem that the/C composite material lacks a high-temperature brazing connection technology is solved, and C is expandedfThe application of the/C composite material in the high temperature field avoids the condition that diffusion welding can not connect complicated Cfcomposite/C material member and vacuum thermocompression sintering pair Cfthe/C composite material causes damage. The two-step brazing method effectively improves CfThe connection quality of the/C composite material (the room temperature strength of the joint is 20.5 MPa-40.8 MPa, the high-temperature shear strength of the joint measured under the vacuum condition of 1200 ℃ is 49.2MPa), and the preparation of the infiltration layer realizes C on one handfAlloying of the surface of the/C composite material, in one aspect to Cfthe/C base material plays a role in hole sealing treatment, and the brazing filler metal is prevented from excessively infiltrating into the base material under the capillary action to cause connection failure.
Drawings
FIG. 1 shows C in which brazing was completed in the fourth step of test onefThe structure picture of the whole soldered joint of the/C composite material;
FIG. 2 shows C in which brazing was completed in the fourth step of test IfPhase analysis diagram of the whole soldered joint shear fracture of the/C composite material.
Detailed Description
The first embodiment is as follows: the embodiment is a method for brazing a carbon fiber reinforced carbon-based composite material at high temperature by a two-step method, which comprises the following steps:
firstly, preparing eutectic Ti-Si brazing filler metal: polishing the surface of the Ti sheet to remove oxide skin, then placing the Ti sheet and the Si block with the oxide skin removed in a copper pot, repeatedly smelting for 5-7 times by adopting vacuum arc smelting equipment, and naturally cooling to room temperature under a vacuum condition to obtain 14Ti-86Si brazing filler metal; the atomic percentage content ratio of the Ti sheet and the Si block for removing the oxide skin is 7: 43;
secondly, preparing brazing filler metal sheets: cutting the 14Ti-86Si brazing filler metal prepared in the first step into sheets by adopting linear cutting equipment, polishing to remove oxide skin, then placing the sheets in absolute ethyl alcohol for ultrasonic cleaning for 5-10 min, and drying to obtain 14Ti-86Si brazing filler metal sheets;
thirdly, preparation of CfInfiltration layer of/C composite: c to be weldedfPlacing the/C composite material in absolute ethyl alcohol for ultrasonic cleaning for 5-10 min, drying, and fixing the 14Ti-86Si brazing filler metal sheet prepared in the step two on the C to be welded by adopting an organic binderfThe surface to be welded of the/C composite material; fixing C to be welded by graphite diefPlacing the/C composite material in a vacuum brazing furnace or an atmosphere furnace, heating to 300 ℃ at the speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 10-30 min under the conditions of vacuum or protective atmosphere and 300 ℃, heating to 1380-1440 ℃ at the speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 10min under the conditions of vacuum or protective atmosphere and 1380-1440 ℃, cooling to 300 ℃ at the speed of 5 ℃/min under vacuum or protective atmosphere, and furnace-cooling to room temperature under vacuum or protective atmosphere to obtain the C with the infiltration layer on the surface to be weldedfa/C composite material;
IV, CfBrazing of the/C composite material: c with two-step three-to-be-welded surface having infiltration layerfthe/C composite material is used as a base material, the 14Ti-86Si brazing filler metal sheet prepared in the step two is fixed between the two base materials by adopting an organic binder, and a sandwich structure is assembled; fixing the base material of the sandwich structure by a graphite mould, placing the base material in a vacuum brazing furnace or an atmosphere furnace, heating to 300 ℃ at a speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 10-30 min under vacuum or protective atmosphere and at a temperature of 300 ℃, heating to 1380-1440 ℃ at a speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 5-120 min under vacuum or protective atmosphere and at a temperature of 1380-1440 ℃, cooling to 300 ℃ at a speed of 5 ℃/min under vacuum or protective atmosphere, and furnace-cooling to room temperature under vacuum or protective atmosphere to finish CfAnd (3) carrying out the whole brazing process of the/C composite material.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the organic binder in the third step is 101 glue. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the organic binder described in step three is 502 glue. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the organic binder in the fourth step is 101 glue. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the organic binder described in step four is 502 glue. The rest is the same as one of the first to fourth embodiments.
The invention was verified with the following tests:
test one: the test is a method for brazing a carbon fiber reinforced carbon-based composite material at high temperature by a two-step method, and the method is specifically carried out according to the following steps:
firstly, preparing eutectic Ti-Si brazing filler metal: polishing the surface of the Ti sheet to remove oxide skin, then placing the Ti sheet and the Si block with the oxide skin removed in a copper pot, repeatedly smelting for 5-7 times by adopting vacuum arc smelting equipment, and naturally cooling to room temperature under a vacuum condition to obtain 14Ti-86Si brazing filler metal; the atomic percentage content ratio of the Ti sheet and the Si block for removing the oxide skin is 7: 43;
secondly, preparing brazing filler metal sheets: cutting the 14Ti-86Si brazing filler metal prepared in the first step into sheets by adopting linear cutting equipment, polishing to remove oxide skin, then placing the sheets in absolute ethyl alcohol for ultrasonic cleaning for 10min, and drying to obtain 14Ti-86Si brazing filler metal sheets;
thirdly, preparation of CfInfiltration layer of/C composite: c to be weldedfPlacing the/C composite material in absolute ethyl alcohol for ultrasonic cleaning for 10min, drying, and fixing the 14Ti-86Si brazing filler metal sheet prepared in the step two on the C to be welded by adopting an organic binderfThe surface to be welded of the/C composite material; fixing C to be welded by graphite diefPlacing the/C composite material in an atmosphere furnace, heating to 300 ℃ at a speed of 10 ℃/min under the protective atmosphere, preserving the heat for 30min under the protective atmosphere and at a temperature of 300 ℃, and preserving the heat for 30min under the protective atmosphereHeating to 1380 ℃ at 10 ℃/min under the atmosphere, preserving heat for 10min under the condition of protective atmosphere and 1380 ℃, cooling to 300 ℃ at 5 ℃/min under the protective atmosphere, and then furnace-cooling to room temperature under the protective atmosphere to obtain C with a infiltration layer on the surface to be weldedfa/C composite material;
IV, CfBrazing of the/C composite material: c with two-step three-to-be-welded surface having infiltration layerfthe/C composite material is used as a base material, the 14Ti-86Si brazing filler metal sheet prepared in the step two is fixed between the two base materials by adopting an organic binder, and a sandwich structure is assembled; fixing the base material of the sandwich structure by a graphite mold, placing the base material in an atmosphere furnace, heating to 300 ℃ at a speed of 10 ℃/min under a protective atmosphere, preserving heat for 30min under the protective atmosphere and at a temperature of 300 ℃, heating to 1400 ℃ at a speed of 10 ℃/min under the protective atmosphere, preserving heat for 5min under the protective atmosphere and at a temperature of 1400 ℃, cooling to 300 ℃ at a speed of 5 ℃/min under the protective atmosphere, and then furnace-cooling to room temperature under the protective atmosphere to finish CfAnd (3) carrying out the whole brazing process of the/C composite material.
The joint performance is evaluated by adopting the compressive shear strength, and the room temperature strength of the obtained joint is 20.5 MPa.
And (2) test II: this test differs from the test one in that: and step four, preserving the heat for 10min under the condition of the protective atmosphere and the temperature of 1400 ℃. The rest were the same as test one.
The joint performance is evaluated by adopting the compressive shear strength, and the room temperature strength of the obtained joint is 25.4 MPa.
And (3) test III: this test differs from the test one in that: and in the fourth step, the temperature is kept for 20min under the condition of the protective atmosphere and the temperature of 1400 ℃. The rest were the same as test one.
The joint performance is evaluated by adopting the compressive shear strength, and the room temperature strength of the obtained joint is 26.7 MPa.
And (4) testing: this test differs from the test one in that: and in the fourth step, the temperature is kept for 40min under the condition of the protective atmosphere and the temperature of 1400 ℃. The rest were the same as test one.
The joint performance is evaluated by adopting the compressive shear strength, and the room temperature strength of the obtained joint is 30.7 MPa.
And (5) testing: this test differs from the test one in that: and in the fourth step, the temperature is kept for 60min under the condition of the protective atmosphere and the temperature of 1400 ℃. The rest were the same as test one.
The joint performance is evaluated by adopting the compressive shear strength, and the room temperature strength of the obtained joint is 32.6 MPa.
And (6) test six: this test differs from the test one in that: and in the fourth step, the temperature is kept for 90min under the condition of the protective atmosphere and the temperature of 1400 ℃. The rest were the same as test one.
The joint performance is evaluated by adopting the compressive shear strength, the room temperature strength of the obtained joint is 40.8MPa, the high-temperature shear strength of the joint measured under the vacuum condition of 1200 ℃ is 49.2MPa, and the strength is obtained when the temperature is higher than the room temperature.
Test seven: this test differs from the test one in that: and in the fourth step, the temperature is kept for 120min under the condition of protective atmosphere and 1400 ℃. The rest were the same as test one.
The joint performance is evaluated by adopting the compressive shear strength, and the room temperature strength of the obtained joint is 26.1 MPa.
FIG. 1 shows C in which brazing was completed in the fourth step of test onefThe whole brazing joint structure photo of the/C composite material, the area A is the base material Cfthe/C composite material has welding seams in the area B, the quality of the soldered joint is good, and the brazing filler metal is infiltrated into the CfIn the pores of the/C composite, a favorable "pinning" effect is achieved for the joint connection. By combining the energy spectrum analysis in Table 1, it can be seen that the center of the brazing seam is formed by eutectic structure TiSi2The phase and the Si matrix form, and a compact SiC reaction layer is generated between the brazing filler metal and the base metal.
Table 1 is a table of EDS analysis data at points C, D and E in fig. 1.
TABLE 1
Figure BDA0001557853020000061
FIG. 2 shows C in which brazing was completed in the fourth step of test IfPhase separation of entire soldered joint shear fracture of/C composite materialMapping out, C at ●, SiC, Si,. TiSi-2As can be seen from the figure, the section is C, TiSi2Si and SiC phases, indicating that cracks cross C when the joint is subjected to shear loadsfthe/C matrix, reaction interface and braze center, which also demonstrates the phase analysis in Table 1.

Claims (5)

1. A method for brazing a carbon fiber reinforced carbon-based composite material at high temperature by a two-step method is characterized in that the method for brazing the carbon fiber reinforced carbon-based composite material at high temperature by the two-step method is carried out according to the following steps:
firstly, preparing eutectic Ti-Si brazing filler metal: polishing the surface of the Ti sheet to remove oxide skin, then placing the Ti sheet and the Si block with the oxide skin removed in a copper pot, repeatedly smelting for 5-7 times by adopting vacuum arc smelting equipment, and naturally cooling to room temperature under a vacuum condition to obtain 14Ti-86Si brazing filler metal; the atomic percentage content ratio of the Ti sheet and the Si block for removing the oxide skin is 7: 43;
secondly, preparing brazing filler metal sheets: cutting the 14Ti-86Si brazing filler metal prepared in the first step into sheets by adopting linear cutting equipment, polishing to remove oxide skin, then placing the sheets in absolute ethyl alcohol for ultrasonic cleaning for 5-10 min, and drying to obtain 14Ti-86Si brazing filler metal sheets;
thirdly, preparation of CfInfiltration layer of/C composite: c to be weldedfPlacing the/C composite material in absolute ethyl alcohol, ultrasonically cleaning for 5-10 min, drying, and fixing the 14Ti-86Si brazing filler metal sheet prepared in the step two on the C to be welded by adopting an organic binderfThe surface to be welded of the/C composite material; fixing C to be welded by graphite diefthe/C composite material is placed in a vacuum brazing furnace or an atmosphere furnace, the temperature is raised to 300 ℃ at the speed of 5-10 ℃/min under the vacuum or protective atmosphere, the temperature is kept for 10-30 min under the vacuum or protective atmosphere and at the temperature of 300 ℃, the temperature is raised to 1380-1440 ℃ at the speed of 5-10 ℃/min under the vacuum or protective atmosphere, the temperature is kept for 10min under the vacuum or protective atmosphere and at the temperature of 1380-1440 ℃, the temperature is lowered to 300 ℃ at the speed of 5 ℃/min under the vacuum or protective atmosphere, and then the temperature is cooled to room temperature along with the furnace under the vacuum or protective atmosphere to obtain the C with the infiltration layer on the surface to be weldedfa/C composite material; the infiltration layer can be opposite to Cfthe/C composite material has the function of hole sealing treatment;
IV, CfBrazing of the/C composite material: c with two-step three-to-be-welded surface having infiltration layerfthe/C composite material is used as a base material, the 14Ti-86Si brazing filler metal sheet prepared in the step two is fixed between the two base materials by adopting an organic binder, and a sandwich structure is assembled; fixing a base material of a sandwich structure by using a graphite mold, placing the base material in a vacuum brazing furnace or an atmosphere furnace, heating to 300 ℃ at a speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 10-30 min under vacuum or protective atmosphere and at a temperature of 300 ℃, heating to 1380-1440 ℃ at a speed of 5-10 ℃/min under vacuum or protective atmosphere, preserving heat for 5-120 min under vacuum or protective atmosphere and at a temperature of 1380-1440 ℃, cooling to 300 ℃ at a speed of 5 ℃/min under vacuum or protective atmosphere, and furnace-cooling to room temperature under vacuum or protective atmosphere to finish CfAnd (3) carrying out the whole brazing process of the/C composite material.
2. The method of claim 1, wherein the organic binder in step three is 101 glue.
3. The method of claim 1, wherein the organic binder in step three is 502 glue.
4. The method of claim 1, wherein the organic binder in step four is 101 glue.
5. The method of claim 1, wherein the organic binder in step four is 502 glue.
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