CN110270729B - Method for brazing Ti-Al alloy and ceramic with graphene barrier layer - Google Patents

Method for brazing Ti-Al alloy and ceramic with graphene barrier layer Download PDF

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CN110270729B
CN110270729B CN201910659487.7A CN201910659487A CN110270729B CN 110270729 B CN110270729 B CN 110270729B CN 201910659487 A CN201910659487 A CN 201910659487A CN 110270729 B CN110270729 B CN 110270729B
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brazing
graphene
alloy
ceramic
pmma
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CN110270729A (en
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孙湛
马迎凯
张丽霞
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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • B23K1/206—Cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • 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
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3601—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
    • 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
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/08—Non-ferrous metals or alloys
    • B23K2103/10—Aluminium or alloys thereof
    • 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
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/08—Non-ferrous metals or alloys
    • B23K2103/14—Titanium or alloys thereof
    • 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
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
    • B23K2103/52—Ceramics

Abstract

A method for brazing Ti-Al series alloy and ceramic with the assistance of a graphene barrier layer relates to a method for brazing Ti-Al series alloy and ceramic. Aims to solve the problem that when the Ti-Al series alloy and the ceramic are brazed and connected by adopting the brazing filler metal containing copper, the shearing strength of the joint is low due to the brittle phase generated in the joint. The method comprises the following steps: preparing a graphene barrier layer on the to-be-welded surface of the Ti-Al alloy by adopting a liquid phase transfer method, then placing a copper-containing brazing filler metal foil between the to-be-welded surface of the Ti-Al alloy and the to-be-welded surface of the ceramic, and finally performing brazing. According to the invention, the layered graphene is introduced as the barrier layer in the brazing process, so that the reaction between the Ti-Al alloy and the ceramic brazing rod and the dissolution of the Ti-Al alloy are effectively weakened, the generation of brittle phases in joints is avoided, the thickness of a reaction layer is ensured, and the mechanical property is excellent. The invention is suitable for brazing Ti-Al series alloy and ceramics.

Description

Method for brazing Ti-Al alloy and ceramic with graphene barrier layer
Technical Field
The present invention relates to a method for brazing a Ti-Al alloy and a ceramic.
Background
The Cu-containing brazing filler metal can solve the problem of low joint strength caused by large difference of thermal expansion coefficients of base materials on two sides when the Ti-Al alloy and the ceramic are brazed, but in the brazing process, the dissolved Ti-Al alloy and the Cu-containing brazing filler metal can react with the ceramic to generate excessive brittle phases such as Cu in the brazed joint2Ti or TiSiCu, brittle phase may lead to a decrease in the shear strength of the braze joint.
Disclosure of Invention
The invention aims to solve the problem of low joint shear strength caused by brittle phases generated in joints when a copper-containing brazing filler metal is used for brazing and connecting Ti-Al series alloy and ceramic, and provides a method for brazing Ti-Al series alloy and ceramic by using a graphene barrier layer.
The method for brazing the Ti-Al alloy and the ceramic with the graphene barrier layer in an auxiliary mode comprises the following steps:
firstly, preparing a graphene layer on a to-be-welded surface of a Ti-Al alloy by adopting a liquid phase transfer method, then placing a copper-containing brazing filler metal foil between the to-be-welded surface of the Ti-Al alloy and the to-be-welded surface of a ceramic, and finally performing brazing to finish the process.
Further, before the graphene barrier layer is prepared on the surface to be welded of the Ti-Al alloy, the surface to be welded is polished and cleaned by adopting different types of abrasive paper during polishing, and the surface to be welded of the Ti-Al alloy is cleaned after polishing; cleaning liquid adopted during cleaning is ethanol solution, and the cleaning mode is ultrasonic cleaning; the ultrasonic cleaning time is 15-25 min.
Further, before brazing, sequentially polishing and cleaning the to-be-brazed surface of the ceramic; when in polishing, different types of abrasive paper are adopted to polish the surfaces to be polished of the ceramics, and the surfaces to be polished are cleaned; cleaning liquid adopted during cleaning is ethanol solution, and the cleaning mode is ultrasonic cleaning; the ultrasonic cleaning time is 15-25 min.
Further, before brazing, a graphite block is adopted to compact the Ti-Al series alloy, the copper-containing brazing filler metal foil and the ceramic.
Further, the brazing specific process comprises the following steps: in a vacuum brazing furnace, the vacuum degree during brazing is 5X 10-3Pa above, the brazing temperature is 800-880 ℃, and the heat preservation time is 8-12 min; and cooling to room temperature after brazing, wherein the cooling speed is 4-6 ℃/min during cooling.
Further, the method for preparing the graphene layer on the to-be-welded surface of the Ti-Al alloy by adopting the liquid phase transfer method comprises the following steps:
step 1, firstly, coating a layer of PMMA solution on the surface of a metal substrate in a graphene/metal substrate laminated sample, and heating and curing;
further, the graphene/metal substrate laminated sample in the step 1 is composed of a metal substrate and a graphene layer attached to the surface of the metal substrate; graphene/metal base laminate samples were purchased from Chongqing graphene technologies, Inc. under the trade name graphene film on a copper foil substrate.
Further, the solvent of the PMMA solution in step 1 is acetone, and the concentration of the PMMA solution is 4 wt.%.
Further, in the step 1, the curing temperature is 150-200 ℃, and the curing time is 4-5 min.
Step 2, corroding the metal substrate by using corrosive liquid to obtain a PMMA/graphene laminated sample;
further, in the step 2, the corrosive liquid is FeCl with the concentration of 1-4 mol/L3A solution; when a metal substrate is corroded by corrosive liquid, immersing the graphene/metal substrate laminated sample into the corrosive liquid; the corrosive liquid is soaked to remove the metal substrate;
step 3, transferring the PMMA/graphene laminated sample to a surface to be welded of the Ti-Al alloy, wherein one side of graphene in the PMMA/graphene laminated sample faces to the surface to be welded of the Ti-Al alloy, and carrying out heat treatment;
further, the heat treatment temperature of the step 3 is 100-140 ℃, and the time is 1-2 min.
Step 4, removing PMMA in the PMMA/graphene laminated sample after heat treatment to obtain a Ti-Al alloy with one layer of graphene;
further, in the step 4, when the PMMA in the PMMA/graphene laminated sample after the heat treatment is removed, the sample is immersed in acetone for soaking for 6-8 hours, and then is washed by deionized water after the soaking is finished.
And 5, repeating the step 1 to the step 4 to obtain the Ti-Al alloy with the multilayer graphene.
The principle and the beneficial effects of the invention are as follows:
according to the invention, graphene is introduced as the barrier layer in the brazing process, so that the reaction between the Ti-Al alloy and the ceramic brazing filler metal and the dissolution of the Ti-Al alloy are effectively weakened, the generation of brittle phases in joints is avoided, and the thickness of a reaction layer is ensured, so that the mechanical property is excellent. The shearing strength of the brazed joint of the invention after the Ti-Al series alloy and the ceramics are brazed reaches more than 110 MPa. The method is used for connecting the Ti-Al alloy and the ceramic brazing filler metal.
The patent CN201811101772.9 generates TiC phase uniformly distributed in the brazing seam through the in-situ reaction of graphene sponge and AgCuTi brazing filler metal, and because the TiC phase has lower linear expansion coefficient and better plastic deformation capability, the TiC phase can adjust the thermal expansion coefficient of the brazing seam, refine and strengthen the matrix structure of the brazing seam, and simultaneously relieve the residual stress of the joint through plastic deformation. The difference points are that: according to the invention, a plurality of layers of graphene are transferred to the to-be-welded surface of the hard alloy and are parallel to the to-be-welded surface of the hard alloy, so that the purpose of inhibiting the hard alloy from being excessively dissolved into the brazing filler metal is achieved; on the other hand, patent CN201811101772.9 is sponge-like graphene, which is placed between two layers of brazing filler metal, not between the brazing filler metal and the object to be welded, and thus dissolution of the cemented carbide into the brazing filler metal cannot be suppressed. Patent CN201811101772.9 aims to reduce the content of Ti element in the brazing seam by compounding and reacting with the brazing filler metal, and finally to suppress the generation of brittle compounds in the brazing seam, and this patent fails to solve the problem of dissolution of base metal elements such as cemented carbide into the brazing seam.
The patent CN201510980623.4 successfully prepares the graphene/aluminum-based solder by using a reduction method of graphene oxide, thereby realizing the enhancement effect of the graphene on the aluminum-based solder. The patent CN201510980623.4 aims to enhance the comprehensive performance of the aluminum-based brazing filler metal by adding graphene, and the invention aims to transfer graphene to inhibit the dissolution of hard alloy into a brazing seam, so the aim is different. The patent CN201510980623.4 cannot solve the problem of dissolution of base metal elements such as cemented carbide into the brazing seams.
Patent CN201410828186.X introduces a three-dimensional structure graphene composite interlayer in the brazing process, and adopts a chemical vapor deposition CVD method to prepare the three-dimensional structure graphene composite interlayer on foam Cu or foam Ni, so that the dispersibility of graphene in the brazing filler metal is improved, the thermal expansion coefficient of the brazing filler metal is reduced, the stress in a joint is relieved, and the performance of the brazed joint is improved. The foam Cu or the foam Ni are porous materials, and the deposited graphene is still porous, so the patent CN201410828186.X cannot solve the problem that the hard alloy is excessively dissolved into a brazing seam.
Drawings
FIG. 1 shows Ti in example 12AlNb alloy and Ti3SiC2Back scattering pictures of the microstructure of the ceramic soldered joint;
FIG. 2 shows Ti without graphene barrier layer introduced in comparative example 12AlNb alloy and Ti3SiC2Back scattering picture of microstructure of ceramic soldered joint.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1: in this example, the ceramic is Ti3SiC2Ceramics, the Ti-Al alloy being Ti2The copper-containing brazing filler metal foil is AgCu brazing filler metal foil; the method of the embodiment is carried out according to the following steps:
firstly, preparing a graphene layer on a to-be-welded surface of a Ti-Al alloy by adopting a liquid phase transfer method, then placing a copper-containing brazing filler metal foil with the thickness of 50 mu m between the to-be-welded surface of the Ti-Al alloy and the to-be-welded surface of a ceramic, and finally brazing to finish the process.
Further, before the graphene barrier layer is prepared on the to-be-welded surface of the Ti-Al alloy, polishing and cleaning the to-be-welded surface are also included, wherein 240# and 600# abrasive paper are sequentially adopted to polish the to-be-welded surface of the Ti-Al alloy during polishing, and cleaning is performed after polishing; cleaning liquid adopted during cleaning is ethanol solution, and the cleaning mode is ultrasonic cleaning; the ultrasonic cleaning time is 20 min.
Further, before brazing, sequentially polishing and cleaning the to-be-brazed surface of the ceramic; when in polishing, different types of abrasive paper are adopted to polish the surfaces to be polished of the ceramics, and the surfaces to be polished are cleaned; cleaning liquid adopted during cleaning is ethanol solution, and the cleaning mode is ultrasonic cleaning; the ultrasonic cleaning time is 20 min.
Further, before brazing, a graphite block is adopted to compact the Ti-Al series alloy, the copper-containing brazing filler metal foil and the ceramic.
Further, the brazing specific process comprises the following steps: in a vacuum brazing furnace, the vacuum degree during brazing is 5X 10-3Pa above, the brazing temperature is 840 ℃, and the heat preservation time is 10 min; and cooling to room temperature after the brazing is finished, wherein the cooling speed is 5 ℃/min during cooling.
Further, the method for preparing the graphene layer on the to-be-welded surface of the Ti-Al alloy by adopting the liquid phase transfer method comprises the following steps:
step 1, firstly, coating a layer of PMMA solution on the surface of a metal substrate in a graphene/metal substrate laminated sample, and heating and curing;
further, the graphene/metal substrate laminated sample in the step 1 is composed of a metal substrate and a graphene layer attached to the surface of the metal substrate; graphene/metal base laminate samples were purchased from Chongqing graphene technologies, Inc. under the trade name graphene film on a copper foil substrate.
Further, the solvent of the PMMA solution in step 1 is acetone, and the concentration of the PMMA solution is 4 wt.%.
Further, in the step 1, the curing temperature is 180 ℃, and the curing time is 5 min.
Step 2, corroding the metal substrate by using corrosive liquid to obtain a PMMA/graphene laminated sample;
further, the corrosive liquid in the step 2 is FeCl with the concentration of 1mol/L3A solution; when a metal substrate is corroded by corrosive liquid, immersing the graphene/metal substrate laminated sample into the corrosive liquid; the corrosive liquid is soaked to remove the metal substrate;
step 3, transferring the PMMA/graphene laminated sample to a surface to be welded of the Ti-Al alloy, wherein one side of graphene in the PMMA/graphene laminated sample faces to the surface to be welded of the Ti-Al alloy, and carrying out heat treatment;
further, the heat treatment temperature in the step 3 is 120 ℃, and the time is 2 min.
Step 4, removing PMMA in the PMMA/graphene laminated sample after heat treatment to obtain a Ti-Al alloy with one layer of graphene;
further, when the PMMA is removed in the step 4, the sample is soaked in acetone for 7 hours, and is washed by deionized water after the soaking is finished.
And 5, repeating the step 1 to the step 4 to obtain the Ti-Al alloy with 3 layers of graphene.
Comparative example 1:
in this comparative example, the ceramic was Ti3SiC2Ceramics, the Ti-Al alloy being Ti2AlNb alloy, Cu-containing brazing filler metal foil is AgCu brazing filler metalA foil; the comparative example process was carried out according to the following steps: in Ti-Al based alloy (Ti)2AlNb alloy) and a copper-containing brazing filler metal foil with the thickness of 50 mu m is placed between the to-be-welded surface of the ceramic and the to-be-welded surface of the ceramic for brazing, and then the process is completed.
Further, before brazing, sequentially polishing and cleaning the surfaces to be welded of the ceramics and the Ti-Al alloy; when in polishing, 240# and 600# abrasive paper is adopted to polish the surfaces to be welded of the ceramics, and the surfaces to be welded are cleaned after polishing; the cleaning liquid adopted during cleaning is ethanol solution, and the cleaning mode is ultrasonic cleaning. The ultrasonic cleaning time is 20 min.
Further, before brazing, a graphite block is adopted to compact the Ti-Al series alloy, the copper-containing brazing filler metal foil and the ceramic.
Further, the brazing specific process comprises the following steps: in a vacuum brazing furnace, the vacuum degree during brazing is 5X 10-3Pa above, the brazing temperature is 840 ℃, and the heat preservation time is 10 min; and cooling to room temperature after the brazing is finished, wherein the cooling speed is 5 ℃/min during cooling.
FIG. 1 shows Ti in example I2AlNb alloy and Ti3SiC2Back scattering pictures of the microstructure of the ceramic soldered joint; FIG. 2 shows Ti without graphene barrier layer introduced in comparative example 12AlNb alloy and Ti3SiC2Back scattering picture of microstructure of ceramic soldered joint. As can be seen by comparing FIG. 1 with FIG. 2, Ti2Ti when graphene barrier layer is transferred on surface of AlNb alloy2The dissolution degree of AlNb alloy is obviously reduced, the reaction is fully carried out, the thickness of a reaction layer of a brittle compound is also obviously reduced, and the addition of a graphene barrier layer effectively inhibits the brittle Cu in a brazing seam2Ti and TiSiCu compounds are generated, and brazing seam tissues are more uniform after the graphene barrier layer is added, so that the performance of the joint is effectively improved.
An electronic universal testing machine is used for carrying out a shearing test, the loading speed is 0.5mm/min, and the room-temperature shearing strength of the connecting joint obtained by adopting the graphene barrier layer assisted brazing method in the embodiment 1 reaches 110 MPa. Under the same parameters, the room-temperature shear strength of the connecting joint (comparative example) obtained by direct brazing without introducing the barrier layer is only 82 MPa.

Claims (8)

1. A method for brazing Ti-Al alloy and ceramic with the assistance of a graphene barrier layer is characterized in that: the method comprises the following steps:
firstly, preparing a graphene layer on a to-be-welded surface of a Ti-Al alloy by adopting a liquid phase transfer method, then placing a copper-containing brazing filler metal foil between the to-be-welded surface of the Ti-Al alloy and the to-be-welded surface of a ceramic, and finally performing brazing to finish the process;
the method for preparing the graphene layer on the to-be-welded surface of the Ti-Al alloy by adopting the liquid phase transfer method comprises the following steps:
step 1, firstly, coating a layer of PMMA solution on the surface of a metal substrate in a graphene/metal substrate laminated sample, and heating and curing;
step 2, corroding the metal substrate by using corrosive liquid to obtain a PMMA/graphene laminated sample;
step 3, transferring the PMMA/graphene laminated sample to a surface to be welded of the Ti-Al alloy, wherein one side of graphene in the PMMA/graphene laminated sample faces to the surface to be welded of the Ti-Al alloy, and carrying out heat treatment;
step 4, removing PMMA in the PMMA/graphene laminated sample after heat treatment to obtain a Ti-Al alloy with one layer of graphene;
step 5, repeating the step 1 to the step 4 to obtain the Ti-Al alloy with the multilayer graphene;
the solvent of the PMMA solution in the step 1 is acetone, and the concentration of the PMMA solution is 4 wt.%;
step 1, the curing temperature is 150-200 ℃, and the curing time is 4-5 min;
and 3, the heat treatment temperature is 100-140 ℃, and the time is 1-2 min.
2. The method of brazing Ti-Al based alloys and ceramics with the assistance of graphene barrier according to claim 1, wherein: before the graphene barrier layer is prepared on the surface to be welded of the Ti-Al alloy, the surface to be welded is polished and cleaned by adopting different types of abrasive paper during polishing, and the surface to be welded of the Ti-Al alloy is cleaned after polishing; cleaning liquid adopted during cleaning is ethanol solution, and the cleaning mode is ultrasonic cleaning; the ultrasonic cleaning time is 15-25 min.
3. The method of assisted brazing of Ti-Al based alloys and ceramics with a graphene barrier layer according to claim 1 or 2, characterized in that: sequentially polishing and cleaning the to-be-welded surface of the ceramic before brazing; when in polishing, different types of abrasive paper are adopted to polish the surfaces to be polished of the ceramics, and the surfaces to be polished are cleaned; cleaning liquid adopted during cleaning is ethanol solution, and the cleaning mode is ultrasonic cleaning; the ultrasonic cleaning time is 15-25 min.
4. The method of brazing Ti-Al based alloys and ceramics with the assistance of graphene barrier according to claim 3, wherein: and before brazing, the Ti-Al alloy, the copper-containing brazing filler metal foil and the ceramic are compacted by a graphite block.
5. The method of assisted brazing of Ti-Al based alloys and ceramics with a graphene barrier according to claim 1, 2 or 4, characterized in that: the brazing specific process comprises the following steps: in a vacuum brazing furnace, the vacuum degree during brazing is 5X 10-3Pa above, the brazing temperature is 800-880 ℃, and the heat preservation time is 8-12 min; and cooling to room temperature after brazing, wherein the cooling speed is 4-6 ℃/min during cooling.
6. The method of brazing Ti-Al based alloys and ceramics with the assistance of graphene barrier according to claim 1, wherein: the graphene/metal substrate laminated sample in the step 1 is composed of a metal substrate and a graphene layer attached to the surface of the metal substrate.
7. The method of brazing Ti-Al based alloys and ceramics with the assistance of graphene barrier according to claim 6, wherein: step 2, the corrosive liquid is FeCl with the concentration of 1-4 mol/L3A solution; immersing a graphene/metal substrate laminated sample into corrosive liquid when corroding a metal substrateAnd etching the liquid.
8. The method of brazing Ti-Al based alloys and ceramics with the assistance of graphene barrier according to claim 6, wherein: and 4, when PMMA in the PMMA/graphene laminated sample after the heat treatment is removed, soaking the sample in acetone for 6-8 hours, and cleaning with deionized water after the soaking is finished.
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CN112756727B (en) * 2020-12-29 2022-08-02 哈尔滨工业大学 Method for enhancing reduction resistance of brazed joint by graphene sponge barrier layer
CN114178738A (en) * 2021-12-08 2022-03-15 浙江亚通焊材有限公司 Active solder for brazing ceramic and stainless steel and solder paste
CN115415656B (en) * 2022-09-19 2023-08-15 哈尔滨工业大学 Connection method of skutterudite thermoelectric material and copper electrode by using Fe-Cr-Mo/W as barrier layer

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