CN107570830B - A method for assisted brazing of CuO nanostructure-enhanced foamed copper intermediate layer - Google Patents
A method for assisted brazing of CuO nanostructure-enhanced foamed copper intermediate layer Download PDFInfo
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- 238000005219 brazing Methods 0.000 title claims abstract description 112
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 77
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Abstract
一种CuO纳米结构增强的泡沫铜中间层辅助钎焊的方法，本发明涉及钎焊陶瓷或陶瓷基复合材料与金属的方法，它要解决现有的陶瓷或陶瓷基复合材料与金属钎焊连接中，残余应力较大的问题。钎焊方法：一、泡沫金属浸渍在NaOH和K2S2O8的混合溶液中，通过化学氧化法制备CuO纳米结构增强的泡沫铜中间层；二、打磨待焊金属、AgCuTi箔片、AgCu箔片和陶瓷或陶瓷基复合材料；三、将待焊金属、AgCuTi钎料箔片、CuO纳米结构增强的泡沫铜中间层、AgCu钎料箔片及陶瓷或陶瓷基复合材料依次叠放；四、待焊件真空钎焊。本发明通过CuO纳米结构与Ti原位反应，生成增强相，细化并增强钎缝基体组织，提高接头的力学性能。
A method for auxiliary brazing of a CuO nanostructure-enhanced foamed copper intermediate layer. The invention relates to a method for brazing ceramics or ceramic-based composite materials and metals, which solves the problem of brazing connection between existing ceramics or ceramic-based composite materials and metals. , the problem of large residual stress. Brazing method: 1. The foam metal is immersed in the mixed solution of NaOH and K 2 S 2 O 8 , and the CuO nanostructure-enhanced copper foam intermediate layer is prepared by chemical oxidation method; 2. The metal to be welded, AgCuTi foil, AgCu Foil and ceramic or ceramic matrix composite material; 3. Stack the metal to be welded, the AgCuTi solder foil, the CuO nanostructure-enhanced foamed copper interlayer, the AgCu solder foil and the ceramic or ceramic matrix composite material in turn; 4 , Vacuum brazing of parts to be welded. In the invention, the CuO nanostructure reacts with Ti in-situ to generate a reinforcing phase, refine and strengthen the matrix structure of the brazing seam, and improve the mechanical properties of the joint.
Description
Technical Field
The present invention relates to a method of brazing ceramic or ceramic matrix composites to metals.
Background
The ceramic or ceramic matrix composite material has the characteristics of high melting point, high hardness, good high-temperature stability, low linear expansion coefficient and the like, and has wide application prospects in the fields of aerospace, electronics industry, nuclear energy industry and the like. However, the ceramic or ceramic matrix composite material has poor processability due to its high brittleness and poor toughness, so that a ceramic/metal composite member needs to be manufactured by a connection method in the practical application process.
To date, the most common process for achieving a ceramic or ceramic matrix composite to metal connection is brazing. However, since there is a great difference between the physical and chemical properties of the ceramic or ceramic matrix composite and the metal, the connection between them is mainly faced with two problems of difficult wettability and large residual stress of the joint. The wettability of the brazing filler metal on the ceramic or ceramic matrix composite material in the brazing process can be improved by adding an active element into the conventional brazing filler metal, but joint residual stress generated by the difference of the coefficient of thermal expansion and the elastic modulus of the two materials and the problems of low strength, poor high-temperature performance and the like of the ceramic/metal joint caused by the joint residual stress often limit the wide application of the brazing filler metal in the practical process.
Among the methods of relieving residual stress in ceramic or ceramic matrix composites and metal joints, the composite braze method and the addition of a soft interlayer are the most common methods. The invention patent (patent No. CN 102699558A) proposes that TiB whiskers with low expansion coefficient are formed in a brazing seam by using an in-situ reaction by adopting a composite brazing filler metal method, so that the linear expansion coefficient of the brazing seam is reduced, the residual stress of a joint is relieved, and the mechanical property of the joint is improved. The invention patent (patent No. CN 102699558A) proposes to use a soft copper foil as an intermediate layer, and to relieve the larger residual stress in a soldered joint by means of the good plastic deformation capability of the copper foil. The invention patent (patent number CN 106270889 a) reports a method for improving the brazing performance of TC4 alloy and ceramic by adding a foam copper interlayer, wherein the foam copper has a three-dimensional structure composed of a metal framework and holes, and has a wider plastic strain platform on a stress-strain curve compared with a copper foil, so that the foam copper has better deformability and energy absorption characteristics, but the method has no significant effect on optimizing the overall microstructure of a joint, and therefore, a novel interlayer needs to be developed to solve the above problems.
Disclosure of Invention
The invention provides a novel method for brazing a foam copper interlayer with an enhanced CuO nano structure in an auxiliary manner, aiming at solving the problems of larger residual stress and lower connection reliability in the existing brazing connection of ceramic or ceramic matrix composite materials and metals.
The method for auxiliary brazing of the CuO nanostructure-reinforced foam copper intermediate layer is realized according to the following steps:
firstly, ultrasonically cleaning foamed copper metal with dilute hydrochloric acid solution, absolute ethyl alcohol and deionized water for 5-10 min in sequence, then naturally drying to obtain pretreated foamed copper metal, and soaking the pretreated foamed metal in NaOH with the concentration of 1-3 mol/L and K with the concentration of 0.05-0.2 mol/L2S2O8Standing for 0.5-3 h in the mixed solution, taking out and washing with deionized water to obtain a CuO nanostructure-enhanced foam copper metal intermediate layer;
secondly, sequentially polishing the metal to be welded, the AgCuTi and the AgCu brazing filler metal foil by using 200#, 600#, and 1000# abrasive paper, polishing the ceramic or ceramic matrix composite material to be welded by using a diamond grinding wheel, and ultrasonically pretreating the ceramic or ceramic matrix composite material to be welded, the metal to be welded, the AgCuTi brazing filler metal foil and the AgCu brazing filler metal foil by using absolute ethyl alcohol for 5-10 min to obtain the metal to be welded, the ceramic or ceramic matrix composite material, the AgCuTi brazing filler metal foil and the AgCu brazing filler metal foil with surface impurities removed;
sequentially stacking the metal to be welded with the surface impurities removed, the AgCuTi brazing filler metal foil, the CuO nanostructure-enhanced copper foam interlayer, the AgCu brazing filler metal foil and the ceramic or ceramic matrix composite with the surface impurities removed, and fixing with a graphite block to obtain a part to be welded;
fourthly, placing the to-be-welded piece obtained in the third step into a vacuum brazing furnace, wherein the vacuum degree is 2-8 multiplied by 10-3And Pa, performing brazing connection under the conditions that the brazing temperature is 800-950 ℃ and the heat preservation time is 1-30 min, and then cooling the weldment to room temperature at the cooling speed of 2-10 ℃/min to finish the CuO nanostructure-reinforced foamy copper middle layer auxiliary brazing.
The invention provides a novel auxiliary brazing method for a foam copper interlayer reinforced by a CuO nano structure, which is characterized in that a chemical oxidation method is utilized to oxidize a foam copper metal framework to generate a CuO nano structure which is uniformly distributed, the oxidized foam copper is taken as an interlayer to be introduced into a brazing joint, and the CuO nano structure reacts with active element Ti in situ to generate Cu in the brazing process3Ti3The O particle reinforced phase is uniformly and dispersedly distributed in the brazing seam, reduces the linear expansion coefficient of the brazing seam, refines and strengthens the matrix structure of the brazing seam, thereby obviously improving the mechanical property of the obtained joint.
The method for auxiliary brazing of the CuO nanostructure-reinforced foamy copper middle layer mainly comprises the following beneficial effects:
1. the method is simple and effective to operate, and the CuO nano structure which is uniformly distributed is prepared on the foamed copper metal framework by adopting a chemical oxidation method, so that the novel foamed copper intermediate layer with the reinforced CuO nano structure is obtained.
2. CuO nano structure reacts with active element Ti in situ to generate Cu3Ti3The O particle reinforcing phase is uniformly dispersed and distributed in the brazing seam, and the brazing seam matrix structure is refined and enhanced, so that the mechanical property of the joint is improved, for example, the TC4 alloy and ZrO are connected by brazing in the invention2The shearing strength of the ceramic can reach more than 90 MPa.
3. In situ generated Cu3Ti3The expansion coefficient of the O-grain reinforced phase line is low, the linear expansion coefficient of a brazing seam can be adjusted, and simultaneously, the plasticity of the selected foam copper metal is good, so that the residual stress of the obtained joint is reduced.
Drawings
FIG. 1 shows ZrO obtained in example I2Microstructure backscatter plot of solder joint of ceramic with TC4 alloy.
Detailed Description
The first embodiment is as follows: the method for auxiliary brazing of the CuO nanostructure-reinforced foam copper intermediate layer is implemented according to the following steps:
firstly, ultrasonically cleaning foamed copper metal with dilute hydrochloric acid solution, absolute ethyl alcohol and deionized water for 5-10 min in sequence, then naturally drying to obtain pretreated foamed copper metal, and soaking the pretreated foamed metal in NaOH with the concentration of 1-3 mol/L and K with the concentration of 0.05-0.2 mol/L2S2O8Standing for 0.5-3 h in the mixed solution, taking out and washing with deionized water to obtain a CuO nanostructure-enhanced foam copper metal intermediate layer;
secondly, sequentially polishing the metal to be welded, the AgCuTi and the AgCu brazing filler metal foil by using 200#, 600#, and 1000# abrasive paper, polishing the ceramic or ceramic matrix composite material to be welded by using a diamond grinding wheel, and ultrasonically pretreating the ceramic or ceramic matrix composite material to be welded, the metal to be welded, the AgCuTi brazing filler metal foil and the AgCu brazing filler metal foil by using absolute ethyl alcohol for 5-10 min to obtain the metal to be welded, the ceramic or ceramic matrix composite material, the AgCuTi brazing filler metal foil and the AgCu brazing filler metal foil with surface impurities removed;
sequentially stacking the metal to be welded with the surface impurities removed, the AgCuTi brazing filler metal foil, the CuO nanostructure-enhanced copper foam interlayer, the AgCu brazing filler metal foil and the ceramic or ceramic matrix composite with the surface impurities removed, and fixing with a graphite block to obtain a part to be welded;
fourthly, placing the to-be-welded piece obtained in the third step into a vacuum brazing furnace, wherein the vacuum degree is 2-8 multiplied by 10-3And Pa, performing brazing connection under the conditions that the brazing temperature is 800-950 ℃ and the heat preservation time is 1-30 min, and then cooling the weldment to room temperature at the cooling speed of 2-10 ℃/min to finish the CuO nanostructure-reinforced foamy copper middle layer auxiliary brazing.
In the embodiment, a chemical oxidation method is adopted to prepare the CuO nanostructure-reinforced foam copper intermediate layer, the CuO nanostructure-reinforced foam copper intermediate layer is introduced into brazing of ceramics or ceramic matrix composite materials and metals, the CuO nanostructure growing on the surface of the foam copper intermediate layer reacts in the brazing process, and the CuO nanostructure reacts with active element Ti in situ to generate Cu in the brazing process3Ti3A reinforcing phase of O particles, and a reinforcing phase of O particles,the brazing filler metal is uniformly and dispersedly distributed in brazing seams, so that the brazing seam structure is refined, the linear expansion coefficient of the brazing seams is reduced, and the mechanical property of brazed joints is obviously improved. Compared with the composite brazing method, the method successfully avoids the defects caused by the agglomeration of the reinforcing phase and ensures the uniform distribution of the reinforcing phase in the brazing seam. Compared with a pure foam copper intermediate layer, the method can generate the Cu with fine dispersion distribution in situ in the brazing seam3Ti3The O-grain phase refines the brazing seam structure and reduces the linear expansion coefficient of the brazing seam, and has a relatively obvious optimization effect on the overall microstructure of the joint.
The method is simple and effective to operate, and the novel CuO nanostructure-reinforced foamy copper intermediate layer is obtained by a chemical oxidation method and is applied to brazing of ceramics or ceramic matrix composite materials and metals.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the thickness of the copper foam in the first step is 0.5-2 mm, and the porosity is 80% -95%. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the difference between the first and second embodiments is that the first step is to dip the pretreated foam metal in NaOH with a concentration of 1-2 mol/L and K with a concentration of 0.1-0.2 mol/L2S2O8Standing the mixed solution for 2-3 hours. Other steps and parameters are the same as those in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and the first to third embodiments is that the concentration of the dilute hydrochloric acid solution in the first step is 0.5-2 mol/L. Other steps and parameters are the same as those in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between the present embodiment and one of the first to the fourth embodiments is that the metal to be welded in the second step is a TC4 titanium alloy, 304 stainless steel, Nb alloy or TiAl alloy. Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between the present embodiment and one of the first to fifth embodiments is that the thickness of the AgCuTi solder foil and the AgCu solder foil in the second step is 50 to 150 μm. Other steps and parameters are the same as those in one of the first to fifth embodiments.
The seventh embodiment: this embodiment is different from the first to sixth embodiments in that the ceramic in the second step is ZrO2Ceramic, Al2O3Ceramics, SiC ceramics, Si3N4Ceramics, SiO2f/SiO2Ceramics, C/C composites or C/SiC composites. Other steps and parameters are the same as those in one of the first to sixth embodiments.
The specific implementation mode is eight: the difference between the second step and the first step and the seventh step is that the ceramic or ceramic matrix composite to be welded in the second step is ground by using diamond grinding wheels of No. 600 and No. 1000 in sequence. Other steps and parameters are the same as those in one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment is different from the first to eighth embodiments in that the vacuum degree of the fourth step is 3 to 6 × 10-3And Pa, raising the temperature at 15 ℃/min to the brazing temperature of 850-900 ℃, and carrying out brazing connection under the condition that the heat preservation time is 10-20 min. Other steps and parameters are the same as those in one to eight of the embodiments.
The detailed implementation mode is ten: the present embodiment differs from the ninth embodiment in that step four is performed in a vacuum degree of 4X 10-3And Pa, raising the temperature at 15 ℃/min to 870 ℃ for brazing, and carrying out brazing connection under the condition of 10min of heat preservation time. Other steps and parameters are the same as those in the ninth embodiment.
The first embodiment is as follows: the method for brazing the CuO nanostructure-reinforced foam copper interlayer in an auxiliary manner is implemented according to the following steps:
firstly, ultrasonically cleaning foamed copper metal for 10min by using a dilute hydrochloric acid solution with the concentration of 1mol/L, absolute ethyl alcohol and deionized water in sequence, then naturally airing to obtain pretreated foamed copper metal, and soaking the pretreated foamed metal in NaOH with the concentration of 2mol/L and K with the concentration of 0.1mol/L2S2O8Standing and oxidizing for 2h, taking out and washing with deionized water to obtain the CuO nano-structure reinforced CuOA foam copper metal intermediate layer; wherein the dimension of the copper foam is 5mm multiplied by 1.2mm (length multiplied by width multiplied by thickness), and the porosity is 90 percent;
secondly, sequentially polishing TC4 to be welded, AgCuTi and AgCu brazing filler metal foils by using 200#, 600#, and 1000# sandpaper, and then, ZrO to be welded2Sequentially grinding the ceramics by using 600# and 1000# diamond grinding wheels, and then ultrasonically pretreating for 10min by using absolute ethyl alcohol to obtain TC4 alloy and ZrO to be welded with surface impurities removed2Ceramic, AgCuTi and AgCu solder foils; the TC4 alloy has the size of 18mm multiplied by 10mm multiplied by 3mm, and the ZrO has the thickness of2The size of the ceramic is 5mm multiplied by 5mm, and the size of the AgCuTi and AgCu brazing filler metal is 5mm multiplied by 100 mu m;
thirdly, removing TC4 alloy to be welded with surface impurities, AgCuTi solder foil, CuO nanostructure-enhanced foam copper intermediate layer, AgCu solder foil and ZrO with surface impurities removed2Sequentially stacking the ceramics, and fixing the ceramics by using graphite blocks to obtain a piece to be welded;
fourthly, placing the to-be-welded piece obtained in the third step into a vacuum brazing furnace, wherein the vacuum degree is 4 multiplied by 10-3Pa, the brazing temperature is 870 ℃, the heat preservation time is 10min, the brazing connection is carried out, then the temperature reduction speed is 5 ℃/min, the weldment is cooled to the room temperature, and ZrO is obtained2the/TC 4 braze joint is completed with CuO nano structure reinforced foam copper interlayer auxiliary braze.
The shear test was performed in an electronic universal tester with a loading speed of 0.5mm/min, and the room temperature shear strength of the joint obtained in this example by the CuO nanostructure-enhanced foamy copper interlayer assisted brazing method was 95.6 MPa. Under the same parameters, the shearing strength of the joint obtained by the AgCu brazing filler metal is only 52.2 MPa.
Example two: the method for brazing the CuO nanostructure-reinforced foam copper interlayer in an auxiliary manner is implemented according to the following steps:
firstly, ultrasonically cleaning foamed copper metal for 10min by using a dilute hydrochloric acid solution with the concentration of 1mol/L, absolute ethyl alcohol and deionized water in sequence, then naturally airing to obtain pretreated foamed copper metal, and soaking the pretreated foamed metal in NaOH with the concentration of 2mol/L and K with the concentration of 0.1mol/L2S2O8Standing and oxidizing for 2 hours, then taking out and washing with deionized water to obtain a CuO nanostructure-enhanced foam copper metal intermediate layer; wherein the dimension of the foamy copper is 5mm multiplied by 1.5mm, and the porosity is 80 percent;
secondly, sequentially polishing TC4 alloy to be welded, AgCuTi and AgCu brazing filler metal foils by using 200#, 600#, and 1000# abrasive paper, and then, ZrO to be welded2Sequentially grinding the ceramics by using 600# and 1000# diamond grinding wheels, and then ultrasonically pretreating for 10min by using absolute ethyl alcohol to obtain TC4 alloy and ZrO to be welded with surface impurities removed2Ceramic, AgCuTi and AgCu solder foils; the TC4 alloy has the size of 18mm multiplied by 10mm multiplied by 3mm, and the ZrO has the thickness of2The size of the ceramic is 5mm multiplied by 5mm, and the size of the AgCuTi and AgCu brazing filler metal is 5mm multiplied by 100 mu m;
thirdly, removing TC4 alloy to be welded with surface impurities, AgCuTi solder foil, CuO nanostructure-enhanced foam copper intermediate layer, AgCu solder foil and ZrO with surface impurities removed2Sequentially stacking the ceramics, and fixing the ceramics by using graphite blocks to obtain a piece to be welded;
fourthly, placing the to-be-welded piece obtained in the third step into a vacuum brazing furnace, wherein the vacuum degree is 4 multiplied by 10-3Pa, the brazing temperature is 870 ℃, the heat preservation time is 10min, the brazing connection is carried out, then the temperature reduction speed is 5 ℃/min, the weldment is cooled to the room temperature, and ZrO is obtained2the/TC 4 braze joint is a method for completing the CuO nano structure reinforced foam copper interlayer auxiliary braze.
The shear test was performed in an electronic universal tester with a loading speed of 0.5mm/min, and the room temperature shear strength of the joint obtained in this example by the CuO nanostructure-enhanced foamy copper interlayer assisted brazing method was 105.6 MPa. Under the same parameters, the shearing strength of the joint obtained by the AgCu brazing filler metal is only 52.2 MPa.
Example three: the method for brazing the CuO nanostructure-reinforced foam copper interlayer in an auxiliary manner is implemented according to the following steps:
firstly, ultrasonically cleaning foamed copper metal for 10min by using a dilute hydrochloric acid solution with the concentration of 1mol/L, absolute ethyl alcohol and deionized water in sequence, and then naturally airing to obtain pretreated copper metalThe foam copper is prepared by soaking the pretreated foam metal in NaOH with the concentration of 2mol/L and K with the concentration of 0.1mol/L2S2O8Standing and oxidizing for 2 hours, then taking out and washing with deionized water to obtain a CuO nanostructure-enhanced foam copper metal intermediate layer; wherein the dimension of the copper foam is 5mm multiplied by 0.8mm (length multiplied by width multiplied by thickness), and the porosity is 95 percent;
secondly, sequentially polishing TC4 to be welded, AgCuTi and AgCu brazing filler metal foils by using 200#, 600#, and 1000# sandpaper, and then, ZrO to be welded2Sequentially grinding the ceramics by using 600# and 1000# diamond grinding wheels, and then ultrasonically pretreating for 10min by using absolute ethyl alcohol to obtain TC4 alloy and ZrO to be welded with surface impurities removed2Ceramic, AgCuTi and AgCu solder foils; the TC4 alloy has the size of 18mm multiplied by 10mm multiplied by 3mm, and the ZrO has the thickness of2The size of the ceramic is 5mm multiplied by 5mm, and the size of the AgCuTi and AgCu brazing filler metal is 5mm multiplied by 100 mu m;
thirdly, removing TC4 alloy to be welded with surface impurities, AgCuTi solder foil, CuO nanostructure-enhanced foam copper intermediate layer, AgCu solder foil and ZrO with surface impurities removed2Sequentially stacking the ceramics, and fixing the ceramics by using graphite blocks to obtain a piece to be welded;
fourthly, placing the to-be-welded piece obtained in the third step into a vacuum brazing furnace, wherein the vacuum degree is 4 multiplied by 10-3Pa, the brazing temperature is 870 ℃, the heat preservation time is 10min, the brazing connection is carried out, then the temperature reduction speed is 5 ℃/min, the weldment is cooled to the room temperature, and ZrO is obtained2the/TC 4 braze joint is completed with CuO nano structure reinforced foam copper interlayer auxiliary braze.
The shear test was performed in an electronic universal tester with a loading speed of 0.5mm/min, and the room temperature shear strength of the joint obtained in this example by the CuO nanostructure-enhanced foamy copper interlayer assisted brazing method was 90.4 MPa. Under the same parameters, the shearing strength of the joint obtained by the AgCu brazing filler metal is only 52.2 MPa.
Claims (9)
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| CN201710966919.XA CN107570830B (en) | 2017-10-17 | 2017-10-17 | A method for assisted brazing of CuO nanostructure-enhanced foamed copper intermediate layer |
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| CN109759665B (en) * | 2019-03-22 | 2021-06-01 | 中山大学 | Preparation method of TiB whisker reinforced ceramic/metal joint with three-dimensional net distribution |
| CN112404631B (en) * | 2020-10-27 | 2022-06-07 | 哈尔滨工业大学 | Method for assisted brazing of dissimilar materials with carbon nanotube sponge intermediate layer |
| CN113977025B (en) * | 2020-12-04 | 2023-06-30 | 中国电器科学研究院股份有限公司 | Preparation method of large-gap braze joint |
| CN113231706B (en) * | 2021-06-25 | 2022-05-03 | 哈尔滨工业大学 | A method for assisted brazing of dissimilar materials by three-dimensional negative expansion network composite interlayer material |
| CN113909613A (en) * | 2021-11-05 | 2022-01-11 | 北京航空航天大学 | A kind of brazing method of SiCf/SiC ceramic matrix composite material and nickel-based superalloy |
| CN115216770B (en) * | 2022-06-27 | 2023-08-22 | 佛山华智新材料有限公司 | Preparation method of diamond/copper composite material surface metal coating |
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