CN107298535A - A kind of composite connecting method of titanium alloy-K4 glass foreign materials - Google Patents
A kind of composite connecting method of titanium alloy-K4 glass foreign materials Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000010936 titanium Substances 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 title claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 7
- 239000002131 composite material Substances 0.000 title claims description 11
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 36
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000005530 etching Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 abstract description 11
- 238000003466 welding Methods 0.000 abstract description 10
- 238000007731 hot pressing Methods 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000005488 sandblasting Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 230000005684 electric field Effects 0.000 abstract description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910000833 kovar Inorganic materials 0.000 description 3
- 239000010410 layer Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
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- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
- Joining Of Glass To Other Materials (AREA)
Abstract
本发明公开了一种钛合金‑K4玻璃异种材料的复合连接方法，通过真空热压的方法将喷砂处理和酸蚀处理之后的钛合金与K4玻璃实现机械互锁结合，然后运用场致扩散连接技术，施加电场促进钛合金与玻璃接头附近离子迁移和界面元素扩散，实现金属与K4玻璃的冶金结合。本发明降低了连接所需温度，减少了焊接时间，同时降低了场致扩散对钛合金的表面要求，最终达到减少内应力的产生，提高了焊接的效率和焊接强度。
The invention discloses a compound connection method of titanium alloy-K4 glass dissimilar materials. The titanium alloy after sand blasting and acid etching treatment and K4 glass are mechanically interlocked and combined by vacuum hot pressing, and then field-induced diffusion is used to Connection technology, applying an electric field to promote ion migration and interface element diffusion near the titanium alloy and glass joints, to achieve metallurgical bonding between metal and K4 glass. The invention reduces the temperature required for the connection, reduces the welding time, and at the same time reduces the field-induced diffusion's requirement on the surface of the titanium alloy, finally reduces the generation of internal stress, and improves the welding efficiency and welding strength.
Description
技术领域 technical field
本发明属于金属加工领域，具体涉及一种钛合金-K4玻璃异种材料的复合连接方法。 The invention belongs to the field of metal processing, and in particular relates to a compound connection method of titanium alloy-K4 glass dissimilar materials.
背景技术 Background technique
由于玻璃属于非晶体材料，主要为硅氧四面体网状结构，具有非常稳定的电子配对和很强的化学稳定性，与金属存在本质上的不同，要想获得良好的连接接头具有较大的难度。同时，K4玻璃属于硼硅玻璃的一种，具有优良的光学稳定性，抗热震性和离子导电性能，因此被广泛应用在光学仪器、传感器和电子封装领域。 Since glass is an amorphous material, mainly a silicon-oxygen tetrahedral network structure, it has very stable electron pairing and strong chemical stability, and is essentially different from metals. To obtain a good connection joint has a large difficulty. At the same time, K4 glass is a kind of borosilicate glass, which has excellent optical stability, thermal shock resistance and ion conductivity, so it is widely used in the fields of optical instruments, sensors and electronic packaging.
目前，国内外对于玻璃和金属的连接研究主要集中在玻璃和铝、铜、可伐合金的连接上，Tsann-ShyiChern对可伐合金在不同温度和时间下预氧化，发现 700℃，5～15 min 时，可形成厚度为4～7μm的致密氧化膜（主要FeO），氧化膜具有良好的粘附性，可以实现可伐合金与玻璃的牢固连接。Gen Sasakil研究证实了Al /玻璃键合界面的纳米晶 γ-Al2O3起到钉扎作用，从而实现Al/玻璃的有效连接。 At present, research on the connection of glass and metal at home and abroad is mainly focused on the connection of glass and aluminum, copper, and Kovar alloys. Tsann-ShyiChern pre-oxidized Kovar alloys at different temperatures and times and found that 700 ° C, 5 to 15 min, a dense oxide film (mainly FeO) with a thickness of 4-7 μm can be formed. The oxide film has good adhesion and can realize a firm connection between Kovar alloy and glass. The Gen Sasakil study confirmed that the nanocrystalline γ-Al 2 O 3 at the Al/glass bonding interface plays a pinning role, thereby achieving an effective connection of Al/glass.
由于钛合金氧化膜的润湿性较差，传统封接方法难以实现钛合金与玻璃的有效连接，Piotr Mrozek（Anodic bonding of glasses with interlayers for fully transparent device applications）研究了通过浮法玻璃表面真空蒸镀纳米级Ti膜，以Ti膜为中间层，采用阳极焊的方法实现玻璃与玻璃的封接，但是并没有解决较厚较大的钛合金块体与玻璃阳极键合时由于较大内应力而导致连接强度不高的问题，同时由于在连接过程中Ti膜表面发生氧化，生成氧化膜，所以连接后的工件强度受氧化膜层与Ti膜基体的连接强度的严重制约，强度有限。 Due to the poor wettability of titanium alloy oxide film, it is difficult to achieve effective connection between titanium alloy and glass by traditional sealing methods, Piotr Mrozek (Anodic bonding of glasses with interlayers for fully transparent device applications) studied the vacuum evaporation of nano-scale Ti film on the surface of float glass, using the Ti film as the intermediate layer, and using the method of anodic welding to realize the sealing of glass and glass, but it did not solve the problem of thicker and larger titanium alloy blocks. When bonding with the glass anode, the connection strength is not high due to the large internal stress. At the same time, due to the oxidation of the surface of the Ti film during the connection process, an oxide film is formed, so the strength of the workpiece after connection is affected by the oxidation film layer and the Ti film substrate. The connection strength is severely restricted, and the strength is limited.
发明内容 Contents of the invention
本发明的目的在于提供一种钛合金-K4玻璃异种材料的复合连接方法。 The purpose of the present invention is to provide a composite connection method of titanium alloy-K4 glass dissimilar materials.
实现本发明的目的的技术解决方案是： The technical solution that realizes the object of the present invention is:
一种钛合金-K4玻璃异种材料的复合连接方法，通过真空热压的方法将喷砂处理和酸蚀处理之后的钛合金与K4玻璃实现机械互锁结合，然后运用场致扩散连接技术，施加电场促进钛合金与玻璃接头附近离子迁移和界面元素扩散，实现金属与K4玻璃的冶金结合，降低连接所需温度，减少焊接时间，从而达到减少内应力的产生，提高焊接的效率和焊接强度，其具体步骤为： A composite connection method of titanium alloy-K4 glass dissimilar materials, through the method of vacuum hot pressing, the titanium alloy after sand blasting and acid etching treatment and K4 glass are mechanically interlocked and combined, and then the field-induced diffusion connection technology is used to apply The electric field promotes ion migration and interface element diffusion near the titanium alloy and glass joint, realizes the metallurgical combination of metal and K4 glass, reduces the temperature required for connection, and reduces welding time, thereby reducing the generation of internal stress and improving welding efficiency and welding strength. The specific steps are:
先对钛合金进行去污去氧化膜处理，再对其表面进行喷砂和酸蚀处理，然后将K4玻璃叠放在钛合金表面，在真空热压炉中，抽真空至2×10-3-3×10-3Pa，升温至750℃~850℃，保温0.5~1h，同时施加压力0.5~1MPa，保压20~30min，保压结束之后缓慢降温至400~500℃，然后在工件两端施加500~800V电压，直至电流完全消失即可，最终实现钛合金与K4玻璃的复合连接。 The titanium alloy is decontaminated and deoxidized first, and then the surface is sandblasted and acid-etched, and then the K4 glass is stacked on the titanium alloy surface, and the vacuum is evacuated to 2×10 -3 in a vacuum hot-press furnace -3×10 -3 Pa, raise the temperature to 750°C~850°C, keep it warm for 0.5~1h, apply a pressure of 0.5~1MPa at the same time, keep the pressure for 20~30min, after the end of the hold pressure, slowly cool down to 400~500°C, Apply a voltage of 500~800V to the terminal until the current disappears completely, and finally realize the composite connection of titanium alloy and K4 glass.
进一步的，所述的钛合金与K4玻璃均为块体。 Further, both the titanium alloy and the K4 glass are blocks.
进一步的，钛合金为TC4块体，采用250~300μm的Al2O3粉末对钛合金表面进行喷砂处理；采用浓度为5.5-6.0mol/L浓盐酸、8.5-9.0mol/L浓硫酸的混合酸腐蚀液，于60±10℃下酸蚀处理45-70min。 Further, the titanium alloy is a TC4 block, and the surface of the titanium alloy is sandblasted with 250-300 μm Al 2 O 3 powder; Mix acid etching solution, etch at 60±10°C for 45-70min.
进一步的，抽真空至2×10-3~3×10-3Pa后，升温至780℃，同时施加压力0.5MPa。 Further, after evacuating to 2×10 -3 ~3×10 -3 Pa, the temperature was raised to 780° C. while applying a pressure of 0.5 MPa.
进一步的，保压结束之后缓慢降温至450℃，在工件两端施加600V电压。 Further, after the pressure holding is completed, the temperature is slowly lowered to 450°C, and a voltage of 600V is applied across the workpiece.
本发明与现有技术相比，其显著优点是：（1）采用真空热压，一方面可以实现K4玻璃和钛合金的紧密接触，有助于场致扩散连接过程中的离子迁移与元素扩散，另一方面，对钛合金表面进行喷砂和酸蚀处理之后，通过真空热压，实现K4玻璃和钛合金的机械互锁结合，有利于提高最后焊件的连接强度。（2）通过场致扩散连接技术工作温度低，焊接时间短的特点，极大的降低工件残余应力的影响，同时提高焊接效率，实现K4玻璃与钛合金的冶金结合，提高K4玻璃与钛合金的连接强度。（3）本发明可以实现真空热压和场致扩散的连续作业，真正做到真空热压方法和场致扩散连接技术复合使用，从而极大的减少内应力，提高连接强度，提升焊接效率。 Compared with the prior art, the present invention has the following remarkable advantages: (1) By adopting vacuum hot pressing, on the one hand, the close contact between K4 glass and titanium alloy can be realized, which is helpful for ion migration and element diffusion in the process of field-induced diffusion connection On the other hand, after sandblasting and acid etching the titanium alloy surface, the mechanical interlocking combination of K4 glass and titanium alloy is realized by vacuum hot pressing, which is beneficial to improve the connection strength of the final weldment. (2) Through the field diffusion connection technology, the working temperature is low and the welding time is short, which greatly reduces the influence of the residual stress of the workpiece, and at the same time improves the welding efficiency, realizes the metallurgical combination of K4 glass and titanium alloy, and improves the quality of K4 glass and titanium alloy. connection strength. (3) The present invention can realize the continuous operation of vacuum hot pressing and field diffusion, and truly realize the combined use of vacuum hot pressing method and field diffusion connection technology, thereby greatly reducing internal stress, improving connection strength, and improving welding efficiency.
附图说明 Description of drawings
图1为本发明钛合金-K4玻璃异种材料的复合连接工艺流程图。 Fig. 1 is a flow chart of the composite connection process of titanium alloy-K4 glass dissimilar materials of the present invention.
具体实施方式 detailed description
下面结合附图及实施方式对本发明作进一步详细的说明。 The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments.
如图1，首先分别对K4玻璃和钛合金进行表面清洗，再对钛合金单独进行喷砂和酸蚀处理，然后将K4玻璃叠放在钛合金上，放入真空炉中进行热压处理，最后进行场致扩散连接，从而实现K4与钛合金的有效连接。 As shown in Figure 1, firstly, the surfaces of K4 glass and titanium alloy are cleaned separately, and then the titanium alloy is sandblasted and acid-etched separately, and then the K4 glass is stacked on the titanium alloy, and put into a vacuum furnace for hot-pressing treatment. Finally, the field diffusion connection is performed to realize the effective connection between K4 and the titanium alloy.
实施例1 Example 1
首先对直径60mm，厚度为6mm的TC4钛合金进行表面去污去氧化膜处理，然后采用250μm的Al2O3粉末斜对钛合金表面进行长达20min的喷砂处理，然后放置在60℃的腐蚀液（浓度为5.8mol/L浓盐酸与8.96mol/L浓硫酸）中浸泡一小时，再取出超声清洗即可，对同样大小的K4玻璃也进行超声清洗，将K4玻璃叠放在TC4表面，放入真空热压炉中，将真空抽至2×10-3Pa，以10℃/min的速度升温至750℃，保温30min，保证炉内工件温度均匀，然后对工件施加1MPa的压力，半小时之后，卸载压力，将炉内温度以5℃/min的速度缓降至450℃，对上压头所接负极，工作台所接的正极施加电压500V，观测电流显示，直至电流完全消失，即可关闭电源，随炉冷却至室温，观察所得TC4钛合金与K4玻璃实现100%的结合率，同时接头剪切强度可达到23MPa。 Firstly, the TC4 titanium alloy with a diameter of 60 mm and a thickness of 6 mm was decontaminated and deoxidized on the surface, and then the surface of the titanium alloy was sandblasted with 250 μm Al 2 O 3 powder for 20 minutes, and then placed in a 60°C Soak in corrosive solution (concentration: 5.8mol/L concentrated hydrochloric acid and 8.96mol/L concentrated sulfuric acid) for one hour, then take it out for ultrasonic cleaning, and perform ultrasonic cleaning on K4 glass of the same size, and stack K4 glass on the surface of TC4 , put it into a vacuum hot-press furnace, pump the vacuum to 2×10 -3 Pa, raise the temperature to 750°C at a rate of 10°C/min, and keep it warm for 30 minutes to ensure that the temperature of the workpiece in the furnace is uniform, and then apply a pressure of 1MPa to the workpiece. After half an hour, unload the pressure, slowly lower the temperature in the furnace to 450°C at a rate of 5°C/min, apply a voltage of 500V to the negative electrode connected to the upper indenter and the positive electrode connected to the workbench, and observe the current display until the current disappears completely. Then turn off the power supply, cool down to room temperature with the furnace, and observe that the obtained TC4 titanium alloy and K4 glass achieve a 100% bonding rate, and the shear strength of the joint can reach 23MPa.
实施例2 Example 2
同样对直径为60mm，厚度为6mm的圆形TC4钛合金进行表面去污去氧化膜处理，然后采用250μm的Al2O3粉末斜对钛合金表面进行长达20min的喷砂处理，然后放置在60℃的腐蚀液（浓度为5.8mol/L浓盐酸与8.96mol/L浓硫酸）中浸泡一小时，再取出超声清洗即可，对同样大小的K4玻璃也进行超声清洗，将玻璃叠放在TC4表面，放入真空热压炉中，将真空抽至2×10-3Pa，以10℃/min的速度升温至780℃，保温30min，保证炉内工件温度均匀，为保证工件变形量以及防止玻璃碎裂，施加压力减小为0.5MPa，半小时之后，卸载压力，将炉内温度以5℃/min的速度缓降至450℃，对上压头所接负极，工作台所接的正极施加电压500V，观测电流显示，直至电流完全消失，即可关闭电源，随炉冷却至室温。同样进行剪切实验的TC4与K4玻璃的接头强度可达25MPa，同时保证两者结合率100%。 Similarly, the round TC4 titanium alloy with a diameter of 60 mm and a thickness of 6 mm was decontaminated and deoxidized on the surface, and then the surface of the titanium alloy was sandblasted with 250 μm Al 2 O 3 powder for 20 minutes, and then placed on Soak in corrosive solution (concentration: 5.8mol/L concentrated hydrochloric acid and 8.96mol/L concentrated sulfuric acid) at 60°C for one hour, then take it out for ultrasonic cleaning, and perform ultrasonic cleaning on K4 glass of the same size, stack the glass on TC4 surface, put it into a vacuum hot-press furnace, pump the vacuum to 2×10 -3 Pa, raise the temperature to 780°C at a rate of 10°C/min, and keep it warm for 30 minutes to ensure that the temperature of the workpiece in the furnace is uniform. In order to ensure the deformation of the workpiece and To prevent glass from breaking, reduce the applied pressure to 0.5MPa. After half an hour, unload the pressure, and slowly lower the temperature in the furnace to 450°C at a rate of 5°C/min. Connect the negative electrode to the upper pressure head and the positive electrode to the workbench. Apply a voltage of 500V, observe the current display, until the current disappears completely, then turn off the power supply and cool down to room temperature with the furnace. The joint strength of TC4 and K4 glass, which was also subjected to the shear test, can reach 25MPa, and at the same time, the bonding rate of the two is guaranteed to be 100%.
实施例3 Example 3
对直径为75mm，厚度为8mm的圆形TC4钛合金进行表面清洗，然后采用250μm的Al2O3粉末斜对钛合金表面进行长达20min的喷砂处理，同样放置在60℃的腐蚀液（浓度为5.8mol/L浓盐酸与8.96mol/L浓硫酸）中浸泡一小时，再取出超声清洗即可，对同样大小的K4玻璃也进行超声清洗，将玻璃叠放在TC4表面，放入真空热压炉中，将真空抽至2×10-3Pa，以10℃/min的速度升温至780℃，保温30min，保证炉内工件温度均匀，施加压力依然为0.5MPa，半小时之后，卸载压力，同时将炉内温度以5℃/min的速度缓降至450℃，对上压头所接负极，工作台所接的正极施加电压升至600V，电流完全消失，即可关闭电源，随炉冷却至室温。最终得到100%的结合率以及大约28MPa的剪切强度。 Clean the surface of a round TC4 titanium alloy with a diameter of 75 mm and a thickness of 8 mm, and then use 250 μm Al 2 O 3 powder to obliquely sandblast the surface of the titanium alloy for up to 20 minutes, and also place it in a 60°C corrosion solution ( Soak in 5.8mol/L concentrated hydrochloric acid and 8.96mol/L concentrated sulfuric acid) for one hour, then take it out for ultrasonic cleaning, and perform ultrasonic cleaning on K4 glass of the same size, stack the glass on the surface of TC4, and put it in a vacuum In the hot-press furnace, pump the vacuum to 2×10 -3 Pa, raise the temperature to 780°C at a rate of 10°C/min, and keep it warm for 30 minutes to ensure that the temperature of the workpiece in the furnace is uniform. The applied pressure is still 0.5MPa. After half an hour, unload At the same time, the temperature in the furnace is slowly lowered to 450°C at a rate of 5°C/min, and the voltage applied to the negative electrode connected to the upper indenter and the positive electrode connected to the workbench is increased to 600V. When the current disappears completely, the power can be turned off and the furnace Cool to room temperature. Finally, a 100% bonding rate and a shear strength of about 28 MPa are obtained.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110246769A (en) * | 2019-05-10 | 2019-09-17 | 太原理工大学 | Based on cationic electroconductive metal and glass surface original position metallization eutectic bonding method |
| CN118084359A (en) * | 2024-04-22 | 2024-05-28 | 太原理工大学 | Vacuum diffusion connection method for sodium-calcium-silicon glass and metal |
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| CN101746964A (en) * | 2008-12-19 | 2010-06-23 | 沈阳兴华航空电器有限责任公司 | Titanium alloy and glass sealing process method |
| CN102495438A (en) * | 2011-10-27 | 2012-06-13 | 西北工业大学 | Light reflector mirror blank and preparation method thereof |
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| CN101746964A (en) * | 2008-12-19 | 2010-06-23 | 沈阳兴华航空电器有限责任公司 | Titanium alloy and glass sealing process method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110246769A (en) * | 2019-05-10 | 2019-09-17 | 太原理工大学 | Based on cationic electroconductive metal and glass surface original position metallization eutectic bonding method |
| CN118084359A (en) * | 2024-04-22 | 2024-05-28 | 太原理工大学 | Vacuum diffusion connection method for sodium-calcium-silicon glass and metal |
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| CN107298535B (en) | 2019-08-09 |
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