CN111069726B - Carbon-carbon composite material and metal brazing connection method based on electrophoretic deposition of SiC nanowires - Google Patents
Carbon-carbon composite material and metal brazing connection method based on electrophoretic deposition of SiC nanowires Download PDFInfo
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- CN111069726B CN111069726B CN201811224800.6A CN201811224800A CN111069726B CN 111069726 B CN111069726 B CN 111069726B CN 201811224800 A CN201811224800 A CN 201811224800A CN 111069726 B CN111069726 B CN 111069726B
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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
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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
- B23K1/20—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
- B23K35/24—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
- B23K35/3006—Ag as the principal constituent
Abstract
The invention discloses a method for braze welding of a carbon-carbon composite material and metal based on electrophoretic deposition of SiC nanowires. In addition, compared with chemical vapor deposition, electrophoretic deposition has the advantages of short period and low cost, and does not damage C fibers.
Description
Technical Field
The invention relates to the technical field of welding. More specifically, in the brazing process, when a layer of continuous brittle compound is formed on a connecting interface to influence the joint strength, the method of electrophoretic deposition of SiC nanowires (SiCNWs) is adopted to improve the interface structure and improve the joint strength.
Background
The C/C composite material has the characteristics of low density, higher strength at high temperature, excellent ablation resistance, low thermal expansion coefficient and the like, and is commonly used in the fields of aerospace, nuclear power and the like. In many cases, it is desirable to bond the C/C composite to the metal. At present, in the connection method of the C/C composite material and the metal, the research of brazing connection is wide. However, since the difference between the thermal expansion coefficients of the base metal and the brazing seam metal is large, large residual stress is likely to occur in the brazed joint, resulting in a reduction in the joint strength. Therefore, new processes are needed to reduce residual stress in the brazed joint and improve joint strength.
In order to improve the strength of the soldered joint, the general soldering process is to add a soft metal intermediate layer or use a composite solder mixed with a low thermal expansion coefficient additive phase, and the idea is to change the soldering seam structure and relieve the residual stress of the joint. However, the two methods cannot directionally regulate and control the interface tissue, and the added phase is easy to agglomerate and is easy to become a new weak phase. Under many brazing conditions, a continuous hard brittle phase forms in the braze joint, which becomes the weak phase in the joint. The document "M.Singh, T.P.Shpargel, G.N.Morscher, R.Asthana, Active metal brazing and catalysis of brazed joints in titanium to carbon composites, Mater.Sci.Eng.A.412(2005) 123-128. doi: 10.1016/j.msea.2005.08.179" indicates that a layer of brittle mesophase TiCu preferentially precipitates on the side close to the C/C composite when the C/C composite tube and Ti are subjected to Active brazing using three different solders Cu-ABA, TiCuNi and TiCuSil. When the AgCuTi brazing filler metal is used for brazing the C/C composite material and the Nb metal, a layer of continuous TiCu brittle compound is formed on the side close to the C/C, and the performance of a joint is influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a method for braze welding of a carbon-carbon composite material and a metal based on an electrophoretic deposition SiC nanowire, solves the problem that when a C/C composite material and a metal are connected by brazing through an active brazing filler metal, continuous brittle compounds appear on one side close to the C/C composite material to reduce the strength of a joint, deposits a layer of SiCNWs on the surface of the C/C composite material, reacts with active elements in the brazing filler metal to generate a new phase with a small size and is separated out, and TiCu is separated out in a non-uniform nucleation mode by taking the new phase as a nucleation mass point, so that the original continuous brittle TiCu compound is refined, the weak phase of the joint is improved, and the strength of the joint is improved.
The technical purpose of the invention is realized by the following technical scheme.
The brazing connection method of the carbon-carbon composite material and metal based on the electrophoretic deposition of the SiC nanowire comprises the following steps:
step 1, placing a carbon-carbon composite material serving as a negative electrode into a suspension containing SiC nanowires, and performing electrophoretic deposition by using direct current to deposit the SiC nanowires on the surface of the carbon-carbon composite material, wherein in the suspension containing the SiC nanowires, the concentration of the SiC nanowires is 0.4-0.7 g/L, the concentration of a dispersant, namely disodium methylene dinaphthalenesulfonate is 0.5-0.8 g/L, and the concentration of aluminum nitrate is 0.03-0.08 g/L;
in step 1, the copper plate is the anode, and the distance between the anode and the cathode is 10-20 mm.
In step 1, the SiC nanowires (i.e., SiCNWs) have a diameter of 100-500nm and a length of 50-100 μm, preferably a diameter of 200-300 nm and a length of 60-80 μm.
In step 1, the deposition voltage is 30-60V and the deposition time is 5-60 s, preferably the deposition voltage is 40-50V and the deposition time is 10-40 s.
In the step 1, in the suspension containing the SiC nanowires, the concentration of the SiC nanowires is 0.5-0.7 g/L, the concentration of the disodium methylene dinaphthalenesulfonate serving as a dispersant is 0.6-0.75 g/L, and the concentration of aluminum nitrate is 0.03-0.05 g/L; the carbon-carbon composite material is dispersed uniformly by adopting ultrasound, for example, for 1 hour, and then is placed in the carbon-carbon composite material for direct electrophoresis deposition.
Step 2, the carbon-carbon composite material processed in the step 1 is used as a piece to be welded, the piece to be welded is assembled with brazing filler metal and metal according to a sandwich structure to form a brazing piece, the brazing piece is clamped by a graphite plate to ensure tight contact, the brazing piece is placed in a vacuum brazing furnace and vacuumized, and the pressure in the furnace reaches 1 x 10-3When the temperature is lower than MPa, the temperature is increased from room temperature of 20-25 ℃ to a temperature which is 20-150 ℃ higher than the melting point of the brazing filler metal at a temperature rise rate of 5-10 ℃/min, the temperature is kept for brazing, and then the temperature is reduced to 20-25 ℃, so that the brazing connection of the carbon-carbon composite material and the metal is realized.
In step 2, an AgCuTi brazing filler metal is adopted, nominal components of the AgCuTi brazing filler metal are Ag-21Cu-4.5 Tiwt%, namely 21 wt% of Cu, 4.5 wt% of Ti and the balance of Ag, the total is 100 wt%, the brazing temperature is 850-900 ℃, and the heat preservation time is 10-15 min.
In the step 2, the pressure intensity in the furnace is preferably 8-9 multiplied by 10-4After MPa, the temperature risesAnd (5) performing line brazing.
In the step 2, heat preservation is carried out for 10-15 min at 700-750 ℃ in the temperature rising process so as to ensure that the temperature in the furnace is uniform; and (3) in the cooling process, the temperature is kept for 10-15 min at 400-450 ℃ so as to ensure that the temperature in the furnace is uniform, influence caused by sudden temperature drop is avoided, and finally the furnace is cooled to room temperature.
In step 2, the metal is pure Nb sheet with a purity > 99.9%.
In step 2, if the active solder is powdered, the active solder is fully mixed with a binder (such as a mixed solution of octyl acetate and cellulose nitrate) during assembly, and the mixture is uniformly coated on a workpiece to be welded.
In the technical scheme of the invention, the carbon-carbon composite material is cut and molded, put into acetone for ultrasonic cleaning for 5-30min and then dried for standby, the metal to be welded is cut and molded, the SiC sand paper is used for polishing the metal to 1000#, the metal is put into acetone for ultrasonic cleaning for 5-30min and then dried for standby.
Compared with the prior art, the product obtained by the reaction of the SiCNWs introduced in the invention and the active elements in the brazing filler metal is very fine and cannot become a weak phase in a joint. The product can change the joint forming process, provide nucleation particles for the precipitation of the brittle compounds in the joint forming process, refine the brittle compounds and break the original continuous brittle phase. This facilitates the release of residual stresses in the joint, thereby improving joint strength. Compared with chemical vapor deposition, electrophoretic deposition has the advantages of short period and low cost, and carbon fibers can not be damaged. The C/C composite material and metal brazing connection method based on electrophoretic deposition SiCNWs refines the brittle compounds by changing the nucleation and growth mode of the brittle compounds in the interface structure in the brazing joint forming process. Thereby reducing residual stress in the joint and improving the strength of the joint.
Drawings
FIG. 1 is a schematic diagram of the electrophoretic deposition employed in the present invention.
FIG. 2 is a SEM photograph of the interface between the C/C composite material and the Nb metal braze joint obtained in example 1 of the present invention.
FIG. 3 is a scanning electron microscope photograph of the interface of the soldered joint of the C/C composite material and Nb metal obtained after 30s of electrophoretic deposition in example 2 of the present invention.
FIG. 4 is a schematic view of a shear strength testing apparatus for a brazed joint according to the present invention.
Detailed Description
The technical solution of the present invention will be described in detail with reference to specific examples. It is to be noted that the following implementation steps are intended to better understand the process of the invention, without any limiting effect. The carbon-carbon composite material is purchased from New Material Ltd of Hunan Boyun, and is used as a carbon fiber reinforced composite material, and consists of carbon fiber and pyrolytic carbon; 100 μm thick Ag-21Cu-4.5Ti (21 wt% Cu, 4.5 wt% Ti, remainder Ag, total 100 wt%) foil, as braze solder, available from Beijing institute of nonferrous metals; SiC nanowires, available from xu state agile innovative materials science and technology ltd; disodium methylene dinaphthalenesulfonate (NNO) was purchased from maya reagent.
The first embodiment is as follows:
this example is a control, a method for braze joining of a C/C composite to Nb metal without electrophoretic deposition, using an AgCuTi braze with a nominal composition of Ag-21Cu-4.5Ti wt.%. The method comprises the following steps:
(1) processing the C/C composite material to be welded into small blocks of 5mm multiplied by 5mm by an inner circle cutting machine, putting the small blocks into acetone, ultrasonically cleaning for 5-30min, and drying for later use.
(2) Cutting Nb metal to be welded into small blocks of 10mm × 15mm × 3mm by wire, polishing to 1000# with SiC sand paper, ultrasonic cleaning in acetone for 5-30min, and drying.
(3) Assembling the C/C composite material, AgCuTi solder and Nb metal into a brazing part, putting the brazing part into a high-temperature vacuum brazing furnace, and waiting until the pressure in the furnace is lower than 1 x 10-3When the temperature is MPa, the temperature is heated to 750 ℃ at the speed of 10 ℃/min, then the temperature is preserved for 10min, and then the temperature is continuously raised at the temperature rise speed of 10 ℃/min to 880 ℃. Keeping the temperature at 880 ℃ for 10min, cooling to 400 ℃ at the speed of 5 ℃/min, and finally cooling to the room temperature of 20-25 ℃ along with the furnace. Thereby realizing the braze welding connection of the C/C composite material and the Nb metal. This implementationExample a scanning picture of the resulting brazed joint of C/C composite material and Nb metal is shown in fig. 2, from which it can be seen that in the joint interface structure without the electrophoretic deposition process, the brittle TiCu compound is continuous, which is the weak phase in the joint.
Example two:
this example is a method for braze joining of a C/C composite with Nb metal based on electrophoretic deposition of SiCNWs, using an AgCuTi braze with nominal composition Ag-21Cu-4.5Ti wt.%. The method comprises the following steps:
(1) processing the C/C composite material to be welded into small blocks of 5mm multiplied by 5mm by an inner circle cutting machine, putting the small blocks into acetone, ultrasonically cleaning for 5-30min, and drying for later use.
(2) Cutting Nb metal to be welded into small blocks of 10mm × 15mm × 3mm by wire, polishing to 1000# with SiC sand paper, ultrasonic cleaning in acetone for 5-30min, and drying.
(3) According to the concentration SiCNWs0.5g/L, dispersant NNO0.75g/L and AlNO30.05g/L of SiCNWs is prepared into isopropanol suspension, and ultrasonic dispersion is carried out for 1 h.
(4) And (2) taking the C/C composite material obtained in the step (1) as a negative electrode, taking a Cu plate as a positive electrode, and immersing the C/C composite material into the electrophoretic solution prepared in the step (3) with the distance of 10mm, and carrying out electrophoretic deposition by introducing direct current with the voltage of 40V for 30s, wherein the time for electrophoretic deposition is shown in the attached drawing 1.
(5) Assembling the parts to be welded treated in the step (4), AgCuTi brazing filler metal and Nb metal into a brazing part, putting the brazing part into a high-temperature vacuum brazing furnace, and placing the brazing part into the high-temperature vacuum brazing furnace until the pressure in the furnace is lower than 1 x 10-3When the temperature is MPa, the temperature is heated to 750 ℃ at the speed of 10 ℃/min, then the temperature is preserved for 10min, and then the temperature is continuously raised at the temperature rise speed of 10 ℃/min to 880 ℃. Keeping the temperature at 880 ℃ for 10min, cooling to 400 ℃ at the speed of 5 ℃/min, and finally cooling to room temperature along with the furnace. Thereby realizing the braze welding connection of the C/C composite material and the Nb metal.
In the embodiment, a scanning picture of the soldered joint of the C/C composite material and the Nb metal obtained after 30 seconds of electrophoretic deposition is shown in fig. 3, and it can be seen from the figure that the brittle TiCu compound is obviously refined after the electrophoretic deposition process.
Example three: the difference between this embodiment and the second embodiment is: the electrophoretic deposition time in step (4) was 5 s. The other steps are the same as those in the embodiment.
Example four: the difference between this embodiment and the second or third embodiment is: the electrophoretic deposition time in step (4) was 10 s. The other steps are the same as those of the second embodiment or the third embodiment.
Example five: the present embodiment is different from the second to fourth embodiments in that: the electrophoretic deposition time in step (4) was 20 s. The rest is the same as the second to fourth embodiments.
Example six: the difference between the present embodiment and the second to fifth embodiments is: the electrophoretic deposition time in step (4) was 60 s. The rest is the same as the second to fifth embodiments.
After welding, the performance of the C/C composite and Nb brazed joints was evaluated by the shear strength of the joints. The shear test is completed by a universal testing machine (Instron 1186), the moving speed of a pressure head is set to be 0.2mm/min, the brazed sample is placed in a special fixture, stress is applied to the metal Nb by the pressure head, and the shear effect is achieved, and the specific test process is shown in figure 4. The average shear strength of the samples is the average value of 3-5 samples.
The shear strength of the joint is calculated by the formula
In the formula: tau-shear strength (MPa)
F-maximum breaking load (N) obtained by experiment
S-effective area (mm) of joint brazing seam2)
The shear strength of the brazed joint in each example was calculated as shown in table 1. The data in the table show that the process of electrophoretic deposition of SiCNWs can obviously improve the strength of the soldered joint. When the electrophoretic deposition time was 20s, the shear strength was the highest, 37.0MPa, which was twice the shear strength of the original joint in example one.
TABLE 1
The brazing connection of the carbon-carbon composite material and the metal can be realized by adjusting the parameters of the preparation process according to the content of the invention, and the performance basically consistent with the invention is shown, namely the application of the SiC nanowire in improving the brazing connection performance of the carbon-carbon composite material and the metal, the brittle compound is refined, and the original continuous brittle phase is broken. This facilitates the release of residual stresses in the joint, thereby improving joint strength. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The brazing connection method of the carbon-carbon composite material and metal based on the electrophoretic deposition of the SiC nanowire is characterized by comprising the following steps:
step 1, placing a carbon-carbon composite material serving as a negative electrode into a suspension containing SiC nanowires, and performing electrophoretic deposition by using direct current to deposit the SiC nanowires on the surface of the carbon-carbon composite material, wherein in the suspension containing the SiC nanowires, the concentration of the SiC nanowires is 0.4-0.7 g/L, the concentration of a dispersant, namely disodium methylene dinaphthalenesulfonate is 0.5-0.8 g/L, and the concentration of aluminum nitrate is 0.03-0.08 g/L;
step 2, the carbon-carbon composite material processed in the step 1 is used as a piece to be welded, the piece to be welded is assembled with brazing filler metal and metal according to a sandwich structure to form a brazing piece, the brazing piece is clamped by a graphite plate to ensure tight contact, the brazing piece is placed in a vacuum brazing furnace and vacuumized, and the pressure in the furnace reaches 1 x 10-3When the temperature is lower than MPa, the temperature is increased from room temperature of 20-25 ℃ to a temperature which is 20-150 ℃ higher than the melting point of the brazing filler metal at a temperature rise rate of 5-10 ℃/min, the temperature is kept for brazing, and then the temperature is reduced to 20-25 ℃, so that the brazing connection of the carbon-carbon composite material and the metal is realized.
2. The method for brazing and connecting a carbon-carbon composite material and a metal based on the electrophoretic deposition of SiC nanowires as claimed in claim 1, wherein in the step 1, the copper plate is a positive electrode, and the distance between the positive electrode and the negative electrode is 10-20 mm.
3. The method for brazing and connecting a carbon-carbon composite material and a metal based on the SiC nanowire obtained by the electrophoretic deposition as recited in claim 1, wherein in the step 1, the SiC nanowire has a diameter of 100-500nm and a length of 50-100 μm.
4. The method for brazing and connecting a carbon-carbon composite material and a metal based on the electrophoretic deposition of SiC nanowires as claimed in claim 1, wherein in step 1, the SiC nanowires have a diameter of 200-300 nm and a length of 60-80 μm.
5. The method for braze-bonding a carbon-carbon composite material and a metal based on the electrophoretic deposition of SiC nanowires as claimed in claim 1, wherein in the step 1, the deposition voltage is 30-60V and the deposition time is 5-60 s.
6. The method for braze-bonding a carbon-carbon composite material and a metal based on the electrophoretic deposition of SiC nanowires as claimed in claim 1, wherein in the step 1, the deposition voltage is 40-50V and the deposition time is 10-40 s.
7. The method for brazing and connecting a carbon-carbon composite material and a metal based on the electrophoretic deposition of SiC nanowires as claimed in claim 1, wherein in the step 1, in the suspension containing the SiC nanowires, the concentration of the SiC nanowires is 0.5-0.7 g/L, the concentration of the dispersant disodium methylenedinaphthalenesulfonate is 0.6-0.75 g/L, and the concentration of the aluminum nitrate is 0.03-0.05 g/L.
8. The method for braze welding of the carbon-carbon composite material and the metal based on the electrophoretic deposition of the SiC nanowire as claimed in the claim 1, wherein in the step 2, AgCuTi solder with nominal composition of Ag-21Cu-4.5 Tiwt%, namely 21 wt% Cu, 4.5 wt% Ti and the rest of Ag, the total amount is 100 wt%, the braze welding temperature is 850-900 ℃, and the braze welding temperature and the heat preservation time are 10-15 min; the metal is pure Nb plate with purity of 99.9%.
9. The method for brazing and connecting the carbon-carbon composite material and the metal based on the electrophoretic deposition of the SiC nanowire according to claim 1, wherein in the step 2, the pressure in a furnace reaches 8-9 x 10-4And (4) after MPa, raising the temperature for brazing.
10. Use of a method for the braze joining of carbon-carbon composites based on electrophoretically deposited SiC nanowires to metals according to one of claims 1 to 9, for improving the properties of the braze joining of carbon-carbon composites to metals.
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