CN115476012B - Application of high Cu atomic ratio Cu-Ti brazing filler metal in brazing of ceramic and metal - Google Patents
Application of high Cu atomic ratio Cu-Ti brazing filler metal in brazing of ceramic and metal Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 74
- 238000005219 brazing Methods 0.000 title claims abstract description 71
- 239000002184 metal Substances 0.000 title claims abstract description 46
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 46
- 229910017945 Cu—Ti Inorganic materials 0.000 title claims abstract description 21
- 239000000945 filler Substances 0.000 title claims abstract description 18
- 239000011888 foil Substances 0.000 claims abstract description 39
- 229910000679 solder Inorganic materials 0.000 claims abstract description 37
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000012459 cleaning agent Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 7
- 150000002739 metals Chemical class 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 125000003158 alcohol group Chemical group 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims 4
- 244000137852 Petrea volubilis Species 0.000 claims 2
- 238000007517 polishing process Methods 0.000 claims 1
- 230000005496 eutectics Effects 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000010008 shearing Methods 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
Classifications
-
- 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
- B23K1/20—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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/18—Dissimilar materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Ceramic Products (AREA)
Abstract
一种高Cu原子比Cu‑Ti钎料在陶瓷与金属钎焊中的应用，涉及高Cu原子比Cu‑Ti钎料的应用技术领域。本发明的目的是为了解决采用现有的共晶成分Cu‑23Ti(wt.％)钎料进行Ti3SiC2陶瓷与Nb的钎焊连接时，接头内产生的脆性CuTi化合物导致接头抗剪切强度低的问题。方法：按照Ti3SiC2陶瓷/Ti箔/Cu箔/Nb的顺序装配，得到待焊装配件；将待焊装配件放入真空钎焊炉内，在5×10‑2Pa的真空度及950～1010℃的钎焊温度下保温5～60min，钎焊结束后冷却至室温。本发明可获得一种高Cu原子比Cu‑Ti钎料在陶瓷与金属钎焊中的应用。
The invention discloses an application of Cu-Ti solder with high atomic ratio of Cu in ceramic and metal brazing, and relates to the technical field of application of Cu-Ti solder with high atomic ratio of Cu. The purpose of the present invention is to solve the problem that when the existing eutectic composition Cu-23Ti (wt.%) brazing filler metal is used to carry out the brazing connection of Ti 3 SiC 2 ceramics and Nb, the brittle CuTi compound produced in the joint causes the joint to resist shearing The problem of low intensity. Method: Assemble according to the order of Ti 3 SiC 2 ceramic/Ti foil/Cu foil/Nb to obtain the assembly to be welded; put the assembly to be welded into a vacuum brazing furnace, at a vacuum degree of 5×10 ‑2 Pa and Keep it warm for 5-60 minutes at a brazing temperature of 950-1010°C, and cool to room temperature after brazing. The present invention can obtain the application of Cu-Ti solder with high Cu atomic ratio in ceramic and metal brazing.
Description
技术领域technical field
本发明涉及高Cu原子比Cu-Ti钎料的应用技术领域，具体涉及一种高Cu原子比Cu-Ti钎料在陶瓷与金属钎焊中的应用。The invention relates to the application technical field of high Cu atomic ratio Cu-Ti solder, in particular to the application of high Cu atomic ratio Cu-Ti solder in ceramic and metal brazing.
背景技术Background technique
Ti3SiC2陶瓷具有良好的室温与高温强度、抗氧化性和耐腐蚀性，又具备较好的可加工性等优点，有望成为新型高温结构材料，用作窑具材料、涡轮叶片部件及航空发动机高温零部件等。Nb作为一种高温材料和结构材料，广泛应用于航空航天等领域，将Ti3SiC2陶瓷与金属Nb进行可靠连接，可以充分发挥二者优势，拓宽材料的应用领域。其中，共晶成分Cu-23Ti(wt.％)钎料能够实现Ti3SiC2陶瓷与Nb的直接钎焊连接，但在接头中会生成大量脆性的CuTi化合物，导致钎焊接头抗剪强度降低。Ti 3 SiC 2 ceramics have good room temperature and high temperature strength, oxidation resistance and corrosion resistance, and good machinability, etc., and are expected to become new high-temperature structural materials, used as kiln furniture materials, turbine blade parts and Engine high temperature parts, etc. As a high-temperature material and structural material, Nb is widely used in aerospace and other fields. The reliable connection of Ti 3 SiC 2 ceramics and metal Nb can give full play to the advantages of both and broaden the application fields of materials. Among them, the eutectic composition Cu-23Ti (wt.%) solder can realize the direct brazing connection of Ti 3 SiC 2 ceramics and Nb, but a large amount of brittle CuTi compounds will be generated in the joint, resulting in a decrease in the shear strength of the brazed joint .
发明内容Contents of the invention
本发明的目的是为了解决采用现有的共晶成分Cu-23Ti(wt.％)钎料进行Ti3SiC2陶瓷与Nb的钎焊连接时，接头内产生的脆性CuTi化合物导致接头抗剪切强度低的问题，而提供一种高Cu原子比Cu-Ti钎料在陶瓷与金属钎焊中的应用。The purpose of the present invention is to solve the problem that when the existing eutectic composition Cu-23Ti (wt.%) brazing filler metal is used to carry out the brazing connection of Ti 3 SiC 2 ceramics and Nb, the brittle CuTi compound produced in the joint causes the joint to resist shearing In order to solve the problem of low strength, an application of Cu-Ti solder with high Cu atomic ratio in ceramic and metal brazing is provided.
一种高Cu原子比Cu-Ti钎料在陶瓷与金属钎焊中的应用，所述的高Cu原子比Cu-Ti钎料为Cu-10Ti钎料，所述的Cu-10Ti钎料用于陶瓷与金属的接触反应钎焊。A kind of application of high Cu atomic ratio Cu-Ti solder in ceramics and metal brazing, described high Cu atomic ratio Cu-Ti solder is Cu-10Ti solder, described Cu-10Ti solder is used for Contact reaction brazing of ceramics to metals.
所述的陶瓷为Ti3SiC2陶瓷，所述的金属为Nb。The ceramic is Ti 3 SiC 2 ceramic, and the metal is Nb.
所述的Cu-10Ti钎料用于Ti3SiC2陶瓷与金属Nb的接触反应钎焊按照以下步骤进行：Described Cu-10Ti filler metal is used for the contact reaction brazing of Ti 3 SiC 2 ceramics and metal Nb and carries out according to the following steps:
一、Ti3SiC2陶瓷与Nb的焊前处理：将Ti3SiC2陶瓷和Nb切割成预定尺寸，并将Ti3SiC2陶瓷和Nb的待焊面进行打磨和清洗；所述的Ti3SiC2陶瓷中固溶有质量分数为0.5～2.0％的Al元素；1. Pre-welding treatment of Ti 3 SiC 2 ceramics and Nb: cutting Ti 3 SiC 2 ceramics and Nb into predetermined sizes, and grinding and cleaning the surfaces to be welded of Ti 3 SiC 2 ceramics and Nb; the Ti 3 Al elements with a mass fraction of 0.5-2.0% are solid-dissolved in SiC 2 ceramics;
二、Cu-10Ti钎料的制备：将Cu箔、Ti箔切成与Ti3SiC2陶瓷相同的面积，并按照Cu-10Ti钎料中Ti的质量分数为10％的标准将Cu箔和Ti箔进行厚度打磨，然后将Cu箔和Ti箔处理至表面平整，再进行清洗；2. Preparation of Cu-10Ti solder: Cut Cu foil and Ti foil into the same area as Ti 3 SiC 2 ceramics, and cut Cu foil and Ti The thickness of the foil is polished, and then the Cu foil and Ti foil are processed until the surface is flat, and then cleaned;
三、待焊试件的装配、真空接触反应钎焊：按照Ti3SiC2陶瓷/Ti箔/Cu箔/Nb的顺序装配，得到待焊装配件；将待焊装配件放入真空钎焊炉内，在5×10-2Pa的真空度及950～1010℃的钎焊温度下保温5～60min，钎焊结束后冷却至室温，完成Ti3SiC2陶瓷、Cu-10Ti钎料与金属Nb的接触反应钎焊。3. Assembly of the test piece to be welded, vacuum contact reaction brazing: assemble in the order of Ti 3 SiC 2 ceramic/Ti foil/Cu foil/Nb to obtain the assembly to be welded; put the assembly to be welded into the vacuum brazing furnace Inside, keep warm for 5 to 60 minutes at a vacuum of 5×10 -2 Pa and a brazing temperature of 950 to 1010°C, cool to room temperature after brazing, and complete Ti 3 SiC 2 ceramics, Cu-10Ti solder and metal Nb contact reaction brazing.
本发明的有益效果：Beneficial effects of the present invention:
(1)本发明使用含Ti量较少的高Cu原子比的Cu-Ti钎料，由于Ti含量较低，焊缝中大量存在的是塑性较好的Cu4Ti，有效减少了焊缝中CuTi脆性化合物的生成，因此力学性能优异，钎焊Ti3SiC2陶瓷和金属后接头的抗剪强度达到130MPa以上。(1) The present invention uses Cu-Ti brazing filler metal with high Cu atomic ratio containing less Ti. Due to the low Ti content, a large amount of Cu 4 Ti with better plasticity exists in the weld, which effectively reduces the amount of copper in the weld. CuTi brittle compounds are formed, so the mechanical properties are excellent, and the shear strength of the joint after brazing Ti 3 SiC 2 ceramics and metals reaches more than 130MPa.
(2)本发明使用厚度较小的Cu、Ti箔片组成复合钎料，通过接触反应钎焊方法使得处于非共晶成分的高Cu原子比钎料可以在相对较低的温度下发生融化、液相扩展，从而实现在相对较低的温度下实现焊接。(2) The present invention uses less Cu and Ti foils with a thickness to form a composite solder, and the high Cu atomic ratio solder in the non-eutectic composition can be melted at a relatively low temperature by the contact reaction brazing method. The liquid phase expands, enabling soldering at relatively low temperatures.
本发明可获得一种高Cu原子比Cu-Ti钎料在陶瓷与金属钎焊中的应用。The invention can obtain the application of Cu-Ti solder with high Cu atomic ratio in ceramic and metal brazing.
附图说明Description of drawings
图1为实施例1中采用高Cu原子比的Cu-Ti钎料将Ti3SiC2陶瓷与Nb接触反应钎焊后钎焊接头的微观组织背散射图片；Fig. 1 is the microstructure backscattering picture of the brazed joint after Ti 3 SiC 2 ceramics and Nb contact reaction brazing by adopting the Cu-Ti filler metal of high Cu atomic ratio in embodiment 1;
图2为对比例1中采用传统Cu-Ti共晶钎料将Ti3SiC2陶瓷与Nb接触反应钎焊后钎焊接头的微观组织背散射图片。Fig. 2 is a backscattering picture of the microstructure of the brazed joint after contact reaction brazing of Ti 3 SiC 2 ceramics and Nb by using traditional Cu-Ti eutectic solder in Comparative Example 1.
具体实施方式Detailed ways
具体实施方式一：本实施方式一种高Cu原子比Cu-Ti钎料在陶瓷与金属钎焊中的应用，所述的高Cu原子比Cu-Ti钎料为Cu-10Ti钎料，所述的Cu-10Ti钎料用于陶瓷与金属的接触反应钎焊。Specific Embodiment 1: In this embodiment, a high Cu atomic ratio Cu-Ti solder is used in ceramic and metal brazing. The high Cu atomic ratio Cu-Ti solder is Cu-10Ti solder. The Cu-10Ti solder is used for contact reaction brazing of ceramics and metals.
具体实施方式二：本实施方式与具体实施方式一不同点是：所述的陶瓷为Ti3SiC2陶瓷。Embodiment 2: The difference between this embodiment and Embodiment 1 is that the ceramic is Ti 3 SiC 2 ceramic.
其他步骤与具体实施方式一相同。Other steps are the same as in the first embodiment.
具体实施方式三：本实施方式与具体实施方式一或二不同点是：所述的金属为Nb。Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the metal is Nb.
其他步骤与具体实施方式一或二相同。Other steps are the same as those in Embodiment 1 or 2.
具体实施方式四：本实施方式与具体实施方式一至三之一不同点是：所述的Cu-10Ti钎料用于Ti3SiC2陶瓷与金属Nb的接触反应钎焊按照以下步骤进行：Embodiment 4: The difference between this embodiment and Embodiments 1 to 3 is that the Cu-10Ti solder is used for contact reaction brazing of Ti 3 SiC 2 ceramics and metal Nb according to the following steps:
一、Ti3SiC2陶瓷与Nb的焊前处理：将Ti3SiC2陶瓷和Nb切割成预定尺寸，并将Ti3SiC2陶瓷和Nb的待焊面进行打磨和清洗；所述的Ti3SiC2陶瓷中固溶有质量分数为0.5～2.0％的Al元素；1. Pre-welding treatment of Ti 3 SiC 2 ceramics and Nb: cutting Ti 3 SiC 2 ceramics and Nb into predetermined sizes, and grinding and cleaning the surfaces to be welded of Ti 3 SiC 2 ceramics and Nb; the Ti 3 Al elements with a mass fraction of 0.5-2.0% are solid-dissolved in SiC 2 ceramics;
二、Cu-10Ti钎料的制备：将Cu箔、Ti箔切成与Ti3SiC2陶瓷相同的面积，并按照Cu-10Ti钎料中Ti的质量分数为10％的标准将Cu箔和Ti箔进行厚度打磨，然后将Cu箔和Ti箔处理至表面平整，再进行清洗；2. Preparation of Cu-10Ti solder: Cut Cu foil and Ti foil into the same area as Ti 3 SiC 2 ceramics, and cut Cu foil and Ti The thickness of the foil is polished, and then the Cu foil and Ti foil are processed until the surface is flat, and then cleaned;
三、待焊试件的装配、真空接触反应钎焊：按照Ti3SiC2陶瓷/Ti箔/Cu箔/Nb的顺序装配，得到待焊装配件；将待焊装配件放入真空钎焊炉内，在3×10-3Pa～5×10-2Pa的真空度及950～1010℃的钎焊温度下保温5～60min，钎焊结束后冷却至室温，完成Ti3SiC2陶瓷、Cu-10Ti钎料与金属Nb的接触反应钎焊。3. Assembly of the test piece to be welded, vacuum contact reaction brazing: assemble in the order of Ti 3 SiC 2 ceramic/Ti foil/Cu foil/Nb to obtain the assembly to be welded; put the assembly to be welded into the vacuum brazing furnace Inside, keep warm for 5 to 60 minutes at a vacuum degree of 3×10 -3 Pa to 5×10 -2 Pa and a brazing temperature of 950 to 1010°C for 5 to 60 minutes, and cool to room temperature after brazing to complete Ti 3 SiC 2 ceramics, Cu Contact reaction brazing of -10Ti filler metal and metal Nb.
其他步骤与具体实施方式一至三相同。Other steps are the same as those in Embodiments 1 to 3.
具体实施方式五：本实施方式与具体实施方式一至四之一不同点是：步骤一中将Ti3SiC2陶瓷和Nb的待焊面采用240～600目砂纸逐级打磨。Embodiment 5: The difference between this embodiment and Embodiments 1 to 4 is that in step 1, the surfaces to be welded of Ti 3 SiC 2 ceramics and Nb are polished step by step with 240-600 mesh sandpaper.
其他步骤与具体实施方式一至四相同。Other steps are the same as those in Embodiments 1 to 4.
具体实施方式六：本实施方式与具体实施方式一至五之一不同点是：步骤一中的清洗过程为：将打磨后的Ti3SiC2陶瓷与Nb放入清洗剂中，在超声清洗机中超声清洗10～20min；所述的清洗剂为酒精或丙酮。Embodiment 6: The difference between this embodiment and Embodiments 1 to 5 is: the cleaning process in step 1 is: put the polished Ti 3 SiC 2 ceramics and Nb into the cleaning agent, and put them in an ultrasonic cleaning machine Ultrasonic cleaning for 10-20 minutes; the cleaning agent is alcohol or acetone.
其他步骤与具体实施方式一至五相同。Other steps are the same as those in Embodiments 1 to 5.
具体实施方式七：本实施方式与具体实施方式一至六之一不同点是：步骤二中Cu箔和Ti箔的厚度均为50～500μm。Embodiment 7: The difference between this embodiment and Embodiment 1 to Embodiment 6 is that the thickness of Cu foil and Ti foil in Step 2 is both 50-500 μm.
其他步骤与具体实施方式一至六相同。Other steps are the same as those in Embodiments 1 to 6.
具体实施方式八：本实施方式与具体实施方式一至七之一不同点是：步骤二中打磨过程为：使用240～600目的砂纸逐级打磨Cu箔和Ti箔的两面。Embodiment 8: This embodiment differs from Embodiments 1 to 7 in that: the grinding process in step 2 is: use 240-600 mesh sandpaper to polish both sides of the Cu foil and the Ti foil step by step.
其他步骤与具体实施方式一至七相同。Other steps are the same as those in Embodiments 1 to 7.
具体实施方式九：本实施方式与具体实施方式一至八之一不同点是：步骤二中的清洗过程为：将打磨后的Cu箔和Ti箔放入清洗剂中，在超声清洗机中超声清洗10～20min；所述的清洗剂为酒精或丙酮。Embodiment 9: The difference between this embodiment and Embodiment 1 to Embodiment 8 is: the cleaning process in step 2 is: put the polished Cu foil and Ti foil into the cleaning agent, and ultrasonically clean them in an ultrasonic cleaning machine 10-20 minutes; the cleaning agent is alcohol or acetone.
其他步骤与具体实施方式一至八相同。Other steps are the same as those in Embodiments 1 to 8.
具体实施方式十：本实施方式与具体实施方式一至九之一不同点是：步骤三中钎焊结束后以4～6℃/min的降温速率冷却至室温。Embodiment 10: This embodiment differs from Embodiments 1 to 9 in that: after brazing in step 3, cool down to room temperature at a cooling rate of 4-6° C./min.
其他步骤与具体实施方式一至九相同。Other steps are the same as those in Embodiments 1 to 9.
采用以下实施例验证本发明的有益效果：Adopt the following examples to verify the beneficial effects of the present invention:
实施例1：本实施例中钎料为Cu-10Ti(wt.％)；Cu-10Ti钎料用于Ti3SiC2陶瓷与金属Nb的接触反应钎焊按照以下步骤进行：Embodiment 1: brazing filler metal is Cu-10Ti (wt.%) in the present embodiment; Cu-10Ti brazing filler metal is used for the contact reaction brazing of Ti 3 SiC 2 ceramics and metal Nb and carries out according to the following steps:
一、Ti3SiC2陶瓷与Nb的焊前处理：将Ti3SiC2陶瓷切割成5×5×5mm3，将Nb切割成3×10×15mm3，并将Ti3SiC2陶瓷和Nb的待焊面依次采用240、400和600目砂纸逐级打磨，再将打磨后的Ti3SiC2陶瓷与Nb放入清洗剂中，在超声清洗机中超声清洗15min；所述的清洗剂为酒精或丙酮；所述的Ti3SiC2陶瓷中固溶有质量分数为0.5～2.0％的Al元素；1. Pre-welding treatment of Ti 3 SiC 2 ceramics and Nb: Cut Ti 3 SiC 2 ceramics into 5×5×5mm 3 , cut Nb into 3×10×15mm 3 , and cut Ti 3 SiC 2 ceramics and Nb The surface to be welded is polished step by step with 240, 400 and 600 mesh sandpaper, and then the polished Ti 3 SiC 2 ceramics and Nb are put into a cleaning agent, and ultrasonically cleaned in an ultrasonic cleaning machine for 15 minutes; the cleaning agent is alcohol or acetone; the Ti 3 SiC 2 ceramic has a solid solution of Al element with a mass fraction of 0.5-2.0%;
二、Cu-10Ti钎料的制备：使用金刚石线切割机将Cu箔、Ti箔切成面积为5.5×5.5mm2的块状，并按照Cu-10Ti钎料中Ti的质量分数为10％的标准，依次采用240、400和600目的砂纸逐级打磨Cu箔和Ti箔的两面，将Cu箔打磨至约31mg、Ti箔打磨至约7mg，用两个平整的表面夹持钎料箔片，并施加压力将Cu箔和Ti箔压平整，再将Cu箔和Ti箔放入酒精中，在超声清洗机中超声清洗15min；Cu箔与Ti箔的厚度比约为10：1；2. Preparation of Cu-10Ti solder: Use a diamond wire cutting machine to cut Cu foil and Ti foil into blocks with an area of 5.5 × 5.5 mm 2 , and make the mass fraction of Ti in Cu-10Ti solder 10%. Standard, use 240, 400 and 600 mesh sandpaper to polish both sides of Cu foil and Ti foil step by step, polish Cu foil to about 31mg, Ti foil to about 7mg, and use two flat surfaces to clamp the solder foil, And apply pressure to flatten the Cu foil and Ti foil, then put the Cu foil and Ti foil in alcohol, and ultrasonically clean them in an ultrasonic cleaner for 15 minutes; the thickness ratio of Cu foil to Ti foil is about 10:1;
三、待焊试件的装配、真空接触反应钎焊：按照Ti3SiC2陶瓷/Ti箔/Cu箔/Nb的顺序，使用石墨块将Ti3SiC2陶瓷、Ti箔、Cu箔和Nb压紧，得到待焊装配件；将待焊装配件放入真空钎焊炉内，在5×10-2Pa的真空度及990℃的钎焊温度下保温10min，钎焊结束后以5℃/min的降温速率冷却至室温，后取出试件，即完成。3. Assembly of the test piece to be welded, vacuum contact reaction brazing: in the order of Ti 3 SiC 2 ceramic/Ti foil/Cu foil/Nb, use graphite block to press Ti 3 SiC 2 ceramic, Ti foil, Cu foil and Nb Tighten to get the assembly to be welded; put the assembly to be welded into a vacuum brazing furnace, keep it warm for 10 minutes at a vacuum degree of 5×10 -2 Pa and a brazing temperature of 990°C, and heat it at 5°C/ The cooling rate of min is to cool to room temperature, and then take out the test piece, which is completed.
对比例1：本对比例中钎料为Cu-23Ti(wt.％)；Comparative example 1: In this comparative example, the solder is Cu-23Ti (wt.%);
一、Ti3SiC2陶瓷与Nb的焊前处理：将Ti3SiC2陶瓷切割成5×5×5mm3，将Nb切割成3×10×15mm3，并将Ti3SiC2陶瓷和Nb的待焊面依次采用240、400和600目的砂纸逐级打磨，再将打磨后的Ti3SiC2陶瓷与Nb放入清洗剂中，在超声清洗机中超声清洗15min；所述的清洗剂为酒精或丙酮；所述的Ti3SiC2陶瓷中固溶有质量分数为0.5～2.0％的Al元素；1. Pre-welding treatment of Ti 3 SiC 2 ceramics and Nb: Cut Ti 3 SiC 2 ceramics into 5×5×5mm 3 , cut Nb into 3×10×15mm 3 , and cut Ti 3 SiC 2 ceramics and Nb The surface to be welded is polished step by step with 240, 400 and 600 mesh sandpaper, and then the polished Ti 3 SiC 2 ceramics and Nb are put into a cleaning agent, and ultrasonically cleaned in an ultrasonic cleaning machine for 15 minutes; the cleaning agent is alcohol or acetone; the Ti 3 SiC 2 ceramic has a solid solution of Al element with a mass fraction of 0.5-2.0%;
二、Cu、Ti复合钎料箔片的制备：使用金刚石线切割机将Cu箔、Ti箔切成面积为5.5×5.5mm2的块状，依次采用240、400和600目的砂纸逐级打磨Cu箔和Ti箔的两面，将Cu箔打磨至约11mg、Ti箔打磨至约7mg，用两个平整的表面夹持钎料箔片，并施加压力将Cu箔和Ti箔压平整，再将Cu箔和Ti箔放入酒精中，在超声清洗机中超声清洗15min；2. Preparation of Cu and Ti composite solder foils: Cut Cu foil and Ti foil into blocks with an area of 5.5×5.5mm2 using a diamond wire cutting machine, and then use 240, 400 and 600 mesh sandpaper to polish Cu step by step. On both sides of the copper foil and the Ti foil, polish the Cu foil to about 11mg and the Ti foil to about 7mg, clamp the solder foil with two flat surfaces, and apply pressure to flatten the Cu foil and the Ti foil, and then put the Cu Put the foil and Ti foil into alcohol, and ultrasonically clean them in an ultrasonic cleaner for 15 minutes;
三、待焊试件的装配、真空接触反应钎焊：按照Ti3SiC2陶瓷/Ti箔/Cu箔/Nb的顺序，使用石墨块将Ti3SiC2陶瓷、Ti箔、Cu箔和Nb压紧，得到待焊装配件；将待焊装配件放入真空钎焊炉内，在5×10-2Pa的真空度及990℃的钎焊温度下保温10min，钎焊结束后以5℃/min的降温速率冷却至室温，后取出试件，即完成。3. Assembly of the test piece to be welded, vacuum contact reaction brazing: in the order of Ti 3 SiC 2 ceramic/Ti foil/Cu foil/Nb, use graphite block to press Ti 3 SiC 2 ceramic, Ti foil, Cu foil and Nb Tighten to get the assembly to be welded; put the assembly to be welded into a vacuum brazing furnace, keep it warm for 10 minutes at a vacuum degree of 5×10 -2 Pa and a brazing temperature of 990°C, and heat it at 5°C/ The cooling rate of min is to cool to room temperature, and then take out the test piece, which is completed.
图1为实施例1中采用高Cu原子比的Cu-Ti钎料将Ti3SiC2陶瓷与Nb接触反应钎焊后钎焊接头的微观组织背散射图片；图2为对比例1中采用传统Cu-Ti共晶钎料将Ti3SiC2陶瓷与Nb接触反应钎焊后钎焊接头的微观组织背散射图片。Fig. 1 is the microstructure backscattering picture of the brazed joint after Ti 3 SiC 2 ceramics and Nb contact reaction brazing by using Cu-Ti filler metal with high Cu atomic ratio in Example 1; Microstructure backscattering pictures of brazed joints after contact reaction brazing of Ti 3 SiC 2 ceramics and Nb by Cu-Ti eutectic solder.
通过图1和图2的对比可以发现，图1的接头中深灰色CuTi脆性化合物明显减少，基底相主要为塑性较好的Cu4Ti和Cu，可见实施例1中采用高Cu原子比的Cu-Ti钎料后，有效改善了接头性能。From the comparison of Figure 1 and Figure 2, it can be found that the dark gray CuTi brittle compounds in the joint in Figure 1 are significantly reduced, and the base phase is mainly Cu 4 Ti and Cu with better plasticity. It can be seen that Cu with a high atomic ratio of Cu was used in Example 1. After -Ti solder, the performance of the joint is effectively improved.
利用电子万能试验机进行剪切测试，加载速度为0.5mm/min。测试结果显示：实施例1采用Cu-10Ti(wt.％)钎料接触反应钎焊方法所得的连接接头室温剪切强度达到130MPa，而相同参数下，对比例1中使用Cu-23Ti(wt.％)钎料接触反应钎焊方法所得的连接接头室温剪切强度只有70MPa。An electronic universal testing machine was used to conduct a shear test with a loading speed of 0.5mm/min. The test results show that: Example 1 adopts Cu-10Ti (wt.%) solder contact reaction brazing method to obtain the joint room temperature shear strength of 130MPa, while under the same parameters, Cu-23Ti (wt.%) is used in Comparative Example 1 %) The room temperature shear strength of the connection joint obtained by the solder contact reaction brazing method is only 70 MPa.
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