CN108620767B - Preparation method of composite solder for brazing quartz short fiber reinforced silicon dioxide composite material and Invar alloy - Google Patents
Preparation method of composite solder for brazing quartz short fiber reinforced silicon dioxide composite material and Invar alloy Download PDFInfo
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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Abstract
A preparation method of a composite solder for brazing a quartz short fiber reinforced silicon dioxide composite material and Invar alloy relates to a composite solder and a preparation method thereof. Aims to solve the problem of the prior welding SiO2f/SiO2The joint of the composite material and the Invar alloy adopts active solder to braze the microstructure of the joint at the temperature of more than 400 ℃ to generate a large amount of brittle compounds, and the composite solder is prepared from Cu powder, few-layer graphene and TiH2And (4) forming. The method comprises the following steps: one, Cu powder, TiH2Weighing the powder; secondly, growing graphene in situ by using CuTi brazing filler metal; third, VFG/Cu powder and TiH2Mechanical mixing of (2). The shear strength of the joint brazed by the brazing filler metal is improved to 15MPa from the original 5MPa, and the improvement range is 200%. The invention is used in the field of brazing filler metal.
Description
Technical Field
The invention relates to a composite solder and a preparation method thereof.
Background
In recent years, with rapid development in the field of aerospace, people pay more and more attention to advanced materials, and have higher requirements on advanced ceramic matrix composite materials. The quartz has the characteristics of high light transmittance, high hardness and high corrosion resistance, so that the quartz can be widely applied to the fields of electronics, communication, optical instruments and the like. However, the fracture toughness and the bending strength can not meet the requirements of the aerospace severe conditions. SiO 22f/SiO2(SiO2Short fiber reinforced and toughened SiO2Ceramic matrix composite) is gradually explored by people and is obtained by taking silica ceramic as a matrix and two-dimensional woven quartz fibers as a reinforcing phase through a silica sol infiltration sintering method. It is composed ofThe material is insensitive to cracks, has excellent thermal shock performance, and has excellent broadband wave-transmitting performance on centimeter and millimeter waves, so the material gradually becomes one of ideal materials in the manufacturing process of the antenna housing.
In the process of assembling the antenna housing, SiO is required2f/SiO2The shell of the composite material is connected with the metal matrix, so that reliable connection is a prerequisite for wide application. Invar alloy, which has a very low coefficient of thermal expansion at room temperature, is the first choice for the metal ring in the radome. SiO is usually achieved by mechanical bonding, reactive bonding and welding2f/SiO2Reliable attachment of the composite to the Invar alloy. The mechanical connection is simple in principle, and the complexity of the structure of the composite material part needs to be increased, so that the mechanical connection cannot be widely applied. Although the bonding joint can avoid the complexity of structural design, the joint can not meet the temperature-resistant requirement of the radome in the flight. The active vacuum brazing is to form effective metallurgical bonding through the reaction of high-activity elements in the liquid brazing filler metal and a base metal at high temperature, so as to obtain a reliable and compact joint.
Realization of SiO2f/SiO2The difficulty in connecting the composite material and the Invar is that the chemical bond types, the constituent elements, the thermal expansion coefficients and the like of the composite material and the Invar are greatly different. SiO 22f/SiO2In the preparation process of the composite material, due to the formation of a three-dimensional network structure with silicon-oxygen bonds as units and the formation of a surface with high surface energy after multiple times of dipping and compounding, the surface of a ceramic material is difficult to wet, so that the reaction of an active element and a ceramic interface is required to be realized and a stable interface layer is obtained. SiO 22f/SiO2The joint of the composite material and the Invar alloy will develop large residual stress during cooling due to the large difference between the coefficient of thermal expansion and the elastic modulus. The coefficient of thermal expansion of the Invar alloy is low at room temperature; the coefficient of thermal expansion rises sharply with increasing temperature. However, brazing SiO with active elements2f/SiO2When the composite material is made of Invar alloy, a large amount of brittle compounds and SiO exist in the microstructure of the obtained brazing joint2f/SiO2Composite material and Invar alloy elastic modulusAnd the thermal expansion coefficients are different greatly, and residual thermal stress is induced in the cooling process, so that the strength of the soldered joint is seriously deteriorated.
Disclosure of Invention
The invention aims to solve the problem of the existing welding SiO2f/SiO2The problem that joints of the composite material and Invar alloy adopt active solder to braze the microstructures of the joints at the temperature of over 400 ℃ to generate a large amount of brittle compounds is solved, and the method is used for brazing the quartz short fiber reinforced silicon dioxide composite material (SiO)2f/SiO2Composite material) and Invar alloy and a preparation method thereof.
The composite brazing filler metal for brazing the quartz short fiber reinforced silicon dioxide composite material and the Invar alloy consists of Cu powder, few-layer graphene and TiH2And (4) forming.
The purity of the Cu is 99.0-99.9%, the grain diameter of Cu powder is 300 meshes, and the TiH powder is2Has a purity of more than 99 percent and is TiH2The particle size of the graphene is 48-52 mu m, the number of layers of the few-layer graphene (VFG) is 8-12, and the diameter of the graphene is 10-90 nm.
The preparation method of the composite solder for brazing the quartz short fiber reinforced silicon dioxide composite material and the Invar alloy comprises the following steps of:
one, Cu powder, TiH2Weighing of the powder: weighing 50-80% of Cu powder and 20-50% of TiH according to atomic percentage2Powder, ultrasonic cleaning by using acetone;
secondly, growing graphene in situ by using CuTi solder: uniformly paving the Cu powder cleaned in the step one on the surface of a silicon wafer, and putting the silicon wafer loaded with the Cu powder on a heating table of PECVD equipment; vacuumizing to below 1Pa, and introducing H2(ii) a Heating to the growth temperature of 550-650 ℃ at the speed of 10-30 ℃/min, and stopping introducing H2Instead, CH is introduced4And Ar gas, adjusting Ar and CH4The flow ratio of (A) is continuously increased to 750-850 ℃, the radio frequency is started, the plasma sputtering is stopped after 40-90 minutes, the radio frequency, the heating and the gas are sequentially closed, the Ar gas is always introduced in the cooling process, the flow of the Ar is 20-50 sccm, the pressure is maintained at 400-600 Pa, and the temperature is cooled to room temperatureObtaining Cu powder (VFG/Cu powder) doped with few-layer graphene;
third, VFG/Cu powder and TiH2Mechanical mixing of (2): mixing the few-layer graphene-doped Cu powder obtained in the second step with TiH2And mixing the powder, and then ball-milling for 1.5-5 h to obtain the composite solder.
Furthermore, the flow ratio of Ar to CH4 in the second step is (70-95): 5-30).
According to the invention, graphene vertically grown on the surface of Cu powder reacts with Ti element in the brazing filler metal, and the activity of C atoms at the edge of the graphene is higher and is preferentially combined with the Ti, so that the interface structure of a joint is improved, the formation of excessive brittle intermetallic compounds in the joint is inhibited, and the SiO is effectively improved2f/SiO2The microstructure of the composite material and the Invar alloy joint is greatly improved, and the SiO content is greatly improved2f/SiO2Mechanical properties of the composite material and the Invar alloy joint.
In addition, the invention adds TiH2The Ti content is replenished, the atomic ratio of Ti to Cu is fixed to be 23:77, and the composite solder doped with few layers of graphene is prepared.
The invention has the beneficial effects that:
the solder of the invention is SiO for braze welding connection2f/SiO2The composite material and the Invar alloy have proper melting point and good wettability, and can meet the use requirement of a brazed joint at 400 ℃. Compared with the prior art, the brazing seam structure has more Cu-Ti compounds after the brazing seam is connected by adopting the single CuTi brazing filler metal, and the intermetallic compounds of Cu-Ti, Ti-Fe and Ti-Ni in the brazing seam after the brazing seam is connected by using the VFG/CuTi composite brazing filler metal are inhibited, so that a large-area Cu-based solid solution area appears, and the better plastic deformation capability is shown. Through detection, the shearing strength of the joint brazed by the brazing filler metal is improved from 5MPa to 15MPa, and the improvement range is 200%.
The brazing filler metal of the invention brazes SiO under the conditions of 930 ℃ and 10min of heat preservation2f/SiO2The shear strength of the joint obtained by the composite material and the Invar alloy at room temperature can reach 13-17 MPa, and the retention rate of the joint is improved from 50% to 70% at 500 ℃ compared with the AgCuTi brazing filler metal joint, so that the joint has more excellent high-temperature performance.
Drawings
FIG. 1 is SiO prepared in example 12f/SiO2Electron microscope photographs of the composite;
FIG. 2 is an electron micrograph of a single CuTi solder.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the composite solder for brazing the quartz short fiber reinforced silicon dioxide composite material and the Invar alloy is prepared from Cu powder, few-layer graphene and TiH2And (4) forming.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the purity of the Cu powder is 99.0-99.9%, and the grain size of the Cu powder is 300 meshes. The rest is the same as the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the TiH2Has a purity of more than 99 percent and is TiH2The particle size of (A) is 48 to 52 μm. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the number of layers of the few-layer graphene (VFG) is 8-12, and the diameter of the graphene is 10-90 nm. The rest is the same as the first embodiment.
The fifth concrete implementation mode: the preparation method of the composite solder for brazing the quartz short fiber reinforced silica composite material and the Invar alloy comprises the following steps of:
one, Cu powder, TiH2Weighing of the powder: weighing 50-80% of Cu powder and 20-50% of TiH according to atomic percentage2Powder, ultrasonic cleaning by using acetone;
secondly, growing graphene in situ by using CuTi solder: uniformly paving the Cu powder cleaned in the step one on the surface of a silicon wafer, and putting the silicon wafer loaded with the Cu powder on a heating table of PECVD equipment; vacuumizing to below 1Pa, and introducing H2(ii) a Heating the substrate to a growth temperature of 550 to 650 ℃ at a rate of 10 to 30 ℃/minThen stopping introducing H2Instead, CH is introduced4And Ar gas, adjusting Ar and CH4The flow ratio is continuously increased to 750-850 ℃, the radio frequency is started, the plasma sputtering is stopped after 40-90 minutes, the radio frequency, the heating and the gas are sequentially closed, the Ar gas is continuously introduced in the cooling process, the flow of the Ar is 20-50 sccm, the pressure is maintained at 400-600 Pa, and the Cu powder doped with few-layer graphene is obtained after the cooling to the room temperature;
third, VFG/Cu powder and TiH2Mechanical mixing of (2): mixing the few-layer graphene-doped Cu powder obtained in the second step with TiH2And mixing the powder, and then ball-milling for 1.5-5 h to obtain the composite solder.
In the embodiment, a Plasma Enhanced Chemical Vapor Deposition (PECVD) method is adopted to vertically grow few-layer graphene (VFG) on the surface of Cu powder, and TiH is added in the process of preparing the composite solder2The method realizes the supply of Ti content and prepares the composite solder doped with few layers of graphene.
The composite solder of the embodiment is used for soldering SiO under the condition of keeping the temperature at 910 ℃ for 10min2f/SiO2The shear strength of the joint obtained by the composite material and the Invar alloy at room temperature can reach 6-10 MPa.
The composite solder of the embodiment is used for soldering SiO under the conditions of 950 ℃ and 10min of heat preservation2f/SiO2The shear strength of the joint obtained by the composite material and the Invar alloy at room temperature can reach 11-14 MPa.
The composite solder of the embodiment is used for soldering SiO under the conditions of 930 ℃ and 10min of heat preservation2f/SiO2The shear strength of the joint obtained by the composite material and the Invar alloy at room temperature can reach 13-17 MPa.
The sixth specific implementation mode: the fifth embodiment is different from the fifth embodiment in that: in the first step, 77 percent of Cu powder and 23 percent of TiH powder are weighed according to the atomic percentage2And (3) powder. The rest is the same as the fifth embodiment.
The seventh embodiment: the fifth embodiment is different from the fifth embodiment in that: in the second step, the RF power is 140-160W. The rest is the same as the fifth embodiment.
The specific implementation mode is eight: the true bookThe difference between the embodiment mode and the fifth embodiment mode is that: ar and CH in step two4The flow rate ratio of (70-95) to (5-30). The rest is the same as the fifth embodiment.
The specific implementation method nine: the fifth embodiment is different from the fifth embodiment in that: ar and CH in step two4At a flow ratio of 80: 20. The rest is the same as the fifth embodiment.
The detailed implementation mode is ten: the fifth embodiment is different from the fifth embodiment in that: the composite brazing filler metal prepared in the third step is powdery. The rest is the same as the fifth embodiment.
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1:
this example is for brazing SiO2f/SiO2The preparation method of the composite solder of the composite material and the Invar alloy comprises the following steps:
firstly, selecting Cu powder with the purity of 99.9 percent and TiH2The purity of the powder was 99%. The grain diameter of Cu powder is 300 meshes, TiH2Is about 50 μm in size. 77 percent of Cu powder and 23 percent of TiH are weighed according to the atomic percentage2Pulverizing;
and secondly, putting the weighed powder and the silicon wafer into acetone, and carrying out ultrasonic cleaning for 10min (the ultrasonic frequency is 20 KHz). After the powder and the silicon wafer are naturally air-dried, uniformly paving the Cu powder on the surface of the silicon wafer;
thirdly, placing the silicon wafer loaded with the Cu powder in the second step on a heating table of PECVD equipment, vacuumizing to below 1Pa, and introducing H2The flow rate is 30sccm, and the pressure is maintained at 450 Pa; heating to 600 deg.C at 15 deg.C/min, and stopping introducing H2Instead, CH is introduced4And Ar gas, adjusting Ar and CH4Flow ratio of (1), adjusting CH4The flow rate is 10sccm, the flow rate of Ar is 90sccm, and the pressure is maintained at 900 Pa; continuously heating to 700 ℃, starting radio frequency with the radio frequency power of 200W, sputtering the plasma for 60 minutes and stoppingStopping, sequentially closing the radio frequency, heating, gas and the like, introducing Ar gas in the cooling process, keeping the flow rate of Ar at 30sccm and the pressure at 500Pa, and obtaining few-layer graphene-doped Cu powder (VFG/Cu powder) after cooling to room temperature;
fourthly, obtaining VFG/Cu powder and TiH in the third step2Ball milling the mixed powder for 2h to obtain composite solder;
cleaning oil stains and oxides on the to-be-welded surface of the Invar alloy by using a mechanical cleaning method, then putting the Invar alloy into acetone, and carrying out ultrasonic cleaning for 10min (the ultrasonic frequency is 20 KHz);
sixthly, tabletting the composite solder powder obtained in the step four and processing the composite solder powder into a sheet with the area equal to the surface area to be welded;
seventhly, naturally drying the cleaned material in the air, and then preparing SiO from top to bottom2f/SiO2Assembling the composite material, the composite solder pressing sheet and the Invar alloy, and applying a pressure of 2MPa on the surface for fixing.
Eighthly, placing the assembled workpiece into a vacuum heating furnace, and when the vacuum degree is 1 multiplied by 10-3When Pa is needed, the SiO is heated to 930 ℃ at the speed of 10 ℃/min, the temperature is kept for 10min, then the temperature is reduced to 400 ℃ at the speed of 10 ℃/min, and then the SiO is cooled to room temperature along with the furnace, thus completing the process of SiO2f/SiO2Brazing of composite materials to Invar alloy.
SiO prepared in this example2f/SiO2An electron micrograph of the composite material is shown in FIG. 1. The electron micrograph of the CuTi-only brazing filler metal used as a control is shown in FIG. 2. The brazing seam structure after the single CuTi brazing filler metal is connected has more Cu-Ti compounds, and the intermetallic compounds of Cu-Ti, Ti-Fe and Ti-Ni in the brazing seams after the VFG/CuTi composite brazing filler metal is connected are inhibited, so that a large-area Cu-based solid solution area appears, and the better plastic deformation capability is shown.
After testing, this example of SiO2f/SiO2The shear strength of the joint of the composite material and the Invar alloy at room temperature reaches 15 MPa.
Example 2:
the present embodiment differs from embodiment 1 in that: in step eight, the assembledThe workpiece is placed in a vacuum heating furnace with a vacuum degree of 1 × 10-3When Pa is needed, the SiO is heated to 950 ℃ at the speed of 10 ℃/min, the temperature is kept for 10min, then the temperature is reduced to 400 ℃ at the speed of 10 ℃/min, and then the SiO is cooled to room temperature along with the furnace, thus completing the process of SiO2f/SiO2Brazing of composite materials to Invar alloy. Other parameters and procedures were the same as in example 1.
After testing, this example of SiO2f/SiO2The shear strength of the joint of the composite material and the Invar alloy at room temperature reaches 13 MPa.
Claims (6)
1. A preparation method of a composite solder for brazing a quartz short fiber reinforced silica composite material and Invar alloy is characterized by comprising the following steps of:
one, Cu powder, TiH2Weighing of the powder: weighing 50-80% of Cu powder and 20-50% of TiH according to atomic percentage2Powder, ultrasonic cleaning by using acetone;
secondly, growing graphene in situ by using CuTi solder: uniformly paving the Cu powder cleaned in the step one on the surface of a silicon wafer, and putting the silicon wafer loaded with the Cu powder on a heating table of plasma-assisted chemical vapor deposition equipment; vacuumizing to below 1Pa, and introducing H2(ii) a Heating to the growth temperature of 550-650 ℃ at the speed of 10-30 ℃/min, and stopping introducing H2Instead, CH is introduced4And Ar gas, adjusting Ar and CH4The flow ratio is continuously increased to 750-850 ℃, the radio frequency is started, the plasma sputtering is stopped after 40-90 minutes, the radio frequency, the heating and the gas are sequentially closed, the Ar gas is continuously introduced in the cooling process, the flow of the Ar is 20-50 sccm, the pressure is maintained at 400-600 Pa, and the Cu powder doped with few-layer graphene is obtained after the cooling to the room temperature;
third, VFG/Cu powder and TiH2Mechanical mixing of (2): mixing the few-layer graphene-doped Cu powder obtained in the second step with TiH2Mixing the powder, and then ball-milling for 1.5-5 h to obtain a composite solder;
the VFG is few-layer graphene, the number of layers is 8-12, and the diameter of the graphene is 10-90 nm.
2. The method for preparing the composite filler metal for brazing quartz short fiber reinforced silica composite material and Invar alloy according to claim 1, wherein 77% of Cu powder and 23% of TiH are weighed according to atomic percentage in the step one2And (3) powder.
3. The preparation method of the composite solder for brazing the quartz short fiber reinforced silica composite material and the Invar alloy according to claim 1 or 2, wherein the radio frequency power in the second step is 140-160W.
4. The method for preparing the composite filler metal for brazing quartz short fiber reinforced silica composite material and Invar alloy as claimed in claim 3, wherein Ar and CH in the second step4The flow rate ratio of (70-95) to (5-30).
5. The method for preparing the composite filler metal for brazing quartz short fiber reinforced silica composite material and Invar alloy as claimed in claim 4, wherein Ar and CH in the second step4At a flow ratio of 80: 20.
6. The method for preparing the composite filler metal for brazing the quartz short fiber reinforced silica composite material and the Invar alloy according to claim 5, wherein the composite filler metal prepared in the third step is in a powder state.
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| CN109626968A (en) * | 2019-01-25 | 2019-04-16 | 中国航发北京航空材料研究院 | A kind of preparation method of ceramic matric composite |
| CN112427759B (en) * | 2020-10-27 | 2022-08-26 | 哈尔滨工业大学 | ZrC-SiC ceramic and TC4 titanium alloy brazing method |
| CN113307647B (en) * | 2021-04-16 | 2022-05-31 | 长春工业大学 | Indirect brazing method of aluminum nitride ceramic copper-clad plate |
| 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 |
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