CN108000058B - A method for manufacturing a high-clean flow-limiting sealing gasket - Google Patents
A method for manufacturing a high-clean flow-limiting sealing gasket Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000007789 sealing Methods 0.000 title abstract description 44
- 238000005498 polishing Methods 0.000 claims abstract description 46
- 238000012545 processing Methods 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 3
- 238000002161 passivation Methods 0.000 claims description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 235000012431 wafers Nutrition 0.000 claims description 35
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- 239000010964 304L stainless steel Substances 0.000 claims description 19
- 239000010935 stainless steel Substances 0.000 claims description 19
- 229910001220 stainless steel Inorganic materials 0.000 claims description 19
- 239000010963 304 stainless steel Substances 0.000 claims description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052802 copper Inorganic materials 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 239000007772 electrode material Substances 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 229940117975 chromium trioxide Drugs 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 6
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 6
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 238000003698 laser cutting Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 229910001369 Brass Inorganic materials 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010951 brass Substances 0.000 claims description 3
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 3
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 239000002274 desiccant Substances 0.000 claims 1
- 238000003754 machining Methods 0.000 claims 1
- 238000011161 development Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000009434 installation Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 27
- 235000011007 phosphoric acid Nutrition 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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Abstract
Description
技术领域technical field
本发明涉及气路系统领域，特别是一种用于高洁净气路接头密封的同时能实现限制气体流量的高洁净限流密封垫片的制造方法。The invention relates to the field of gas circuit systems, in particular to a method for manufacturing a high-clean flow-limiting sealing gasket used for sealing high-clean gas circuit joints and capable of limiting gas flow.
背景技术Background technique
气路系统在工农业生产、科技研发各个环节中都非常常见。进入20世纪90年以后，随着世界高新技术的快速发展，计算机工业对大规模集成电路的需求，对液晶显示器的需求大量增加；随着新型能源的发展，还大力开拓多晶硅太阳能电池和薄膜太阳能电池的生产；此外，新型电光源、光电半导体器件、光纤通讯器件也获得迅猛发展，在上述高新产品的生产过程中，都需要大量高纯气体，以制造出性能可靠的各种器件。在使用高纯气体的过程中，满足相应要求的高纯气体管路系统是必不可少的。这些气体管路系统的功能主要实现气体的通断、流量控制、加热、冷却、止回、过滤、限流等功能。而要实现这些功能就需要在气体管路系统中加入各种零部件以实现相关功能，比如：气体的通断就需要隔膜阀，流量控制就需要质量流量控制器，止回就需要止回阀，限流就需要限流器等。这些零部件之间的连接接头位置需要保证可靠的密封效果，以防止气体泄漏，因为上述应用中可能涉及到大量有毒有害，易燃易爆的气体，一旦泄漏，不仅会造成经济损失，而且会导致人员伤亡的事故发生。Gas system is very common in all aspects of industrial and agricultural production, scientific and technological research and development. After entering the 1990s, with the rapid development of high-tech in the world, the computer industry's demand for large-scale integrated circuits and liquid crystal displays has increased significantly; with the development of new energy sources, it has also vigorously developed polysilicon solar cells and thin-film solar cells. The production of batteries; in addition, new electric light sources, optoelectronic semiconductor devices, and optical fiber communication devices have also achieved rapid development. In the production process of the above-mentioned high-tech products, a large amount of high-purity gases are required to manufacture various devices with reliable performance. In the process of using high-purity gas, a high-purity gas pipeline system that meets the corresponding requirements is essential. The functions of these gas pipeline systems mainly realize gas on-off, flow control, heating, cooling, non-return, filtration, flow limiting and other functions. To achieve these functions, various components need to be added to the gas pipeline system to achieve related functions. For example, a diaphragm valve is required for gas on-off, a mass flow controller is required for flow control, and a check valve is required for non-return. , current limiting requires a current limiter, etc. The connection joints between these parts need to ensure a reliable sealing effect to prevent gas leakage, because the above-mentioned applications may involve a large amount of toxic, harmful, flammable and explosive gases. Once leaked, it will not only cause economic losses, but also cause Accidents that resulted in casualties occurred.
目前，对于这些应用使用最为广泛的接头就是端面密封型接头，接头之间夹着密封垫片，通过内、外螺纹互锁来压迫金属垫片，使垫片产生一定的变形，从而达到密封的效果。然而，目前市场上还没有孔直径为0.1mm以下的微孔限流器，无法产生微小流量的气体，而且在某些情况下，对空间尺寸大小要求比较严格也会导致现有的限流器无法使用。因此，有必要开发同时兼具密封和微孔限流的高洁净垫片，通过该高洁净垫片可以简化气路系统的组装过程、产生微小流量的气体、实现更为紧凑的效果，降低相关气路的生产成本。At present, the most widely used joints for these applications are end-face seal joints, with sealing gaskets sandwiched between the joints, and the metal gaskets are pressed through the interlocking of the internal and external threads, causing the gaskets to deform to a certain extent, so as to achieve sealing. Effect. However, there is currently no microporous flow restrictor with a hole diameter of less than 0.1mm on the market, which cannot generate a small flow rate of gas, and in some cases, stricter requirements on the size of the space will also cause the existing flow restrictor to Not available. Therefore, it is necessary to develop a high-clean gasket with both sealing and micropore flow restriction. The high-clean gasket can simplify the assembly process of the gas circuit system, generate a small flow of gas, achieve a more compact effect, and reduce related The production cost of the gas path.
发明内容Contents of the invention
本发明的目的在于提供一种用于高洁净气路接头密封同时能实现限制气体流量的高洁净限流密封垫片的制造方法，通过该方法可以制备出低泄漏率，低表面粗糙度，密封可靠，可以产生微小流量的高洁净限流密封垫片。The purpose of the present invention is to provide a method for manufacturing a high-clean flow-limiting sealing gasket that is used for sealing high-clean gas path joints and can limit gas flow at the same time. By this method, low leakage rate, low surface roughness, and sealing gasket can be prepared. Reliable, high-clean flow-restricting gasket that can generate small flow rates.
本发明的技术方案是：Technical scheme of the present invention is:
一种高洁净限流密封垫片的制造方法，具体操作步骤如下：A method for manufacturing a high-clean flow-limiting sealing gasket, the specific operation steps are as follows:
(1)采用板厚为1～2mm金属板，通过冲压或者激光切割的方式，加工生成外径为12～20mm的圆片；(1) Using a metal plate with a plate thickness of 1-2 mm, process it into a disc with an outer diameter of 12-20 mm by stamping or laser cutting;
(2)采用深微孔电火花加工机床对圆片中心进行直径为0.05～0.1mm微孔的成形加工；(2) Using a deep micro-hole EDM machine tool to form a micro-hole with a diameter of 0.05 to 0.1 mm in the center of the wafer;
(3)待完成微孔加工成型之后，对其进行退火软化处理；(3) After the micropore processing and forming are completed, it is annealed and softened;
(4)对经过热处理之后带有微孔的圆片进行电解抛光；(4) Carry out electrolytic polishing to the disc with micropore after heat treatment;
(5)对经过电解抛光后的圆片进行钝化处理；(5) carry out passivation treatment to the wafer after electrolytic polishing;
(6)对钝化处理后的圆片采用去离子水超声清洗，以去除钝化液，并在百级无尘洁净室中进行烘干，并对每片进行单独真空塑料封装。(6) The passivated wafers are ultrasonically cleaned with deionized water to remove the passivation solution, and dried in a class 100 dust-free clean room, and each piece is individually vacuum-packed in plastic.
所述的高洁净限流密封垫片的制造方法，金属板的材质为304/304L不锈钢板，或者316/316L不锈钢板，或者T2/T1紫铜板，或者1050/1060/1070纯铝板。In the manufacturing method of the high-clean current-limiting sealing gasket, the material of the metal plate is 304/304L stainless steel plate, or 316/316L stainless steel plate, or T2/T1 copper plate, or 1050/1060/1070 pure aluminum plate.
所述的高洁净限流密封垫片的制造方法，步骤(2)中，进行微孔加工时，对于材质为304/304L不锈钢、316/316L不锈钢，以及T1/T2紫铜的圆片，所使用的工作液为绝缘强度为15～20MΩ·cm的去离子水；而对于材质为1050/1060/1070纯铝的圆片，所使用的工作液为煤油；对于材质为304/304L不锈钢和316/316L不锈钢的圆片，所使用的电极材料为钨丝，直径为0.03～0.08mm；对于材质为T1/T2紫铜的圆片，所使用的电极材料为钼丝，直径为0.03～0.08mm；对于材质为1050/1060/1070纯铝的圆片，所使用的电极材料为黄铜丝，直径为0.03～0.08mm。In the manufacturing method of the described high-clean flow-limiting sealing gasket, in step (2), when micropore processing is performed, for discs made of 304/304L stainless steel, 316/316L stainless steel, and T1/T2 red copper, the used The working fluid is deionized water with a dielectric strength of 15-20MΩ·cm; for the discs made of 1050/1060/1070 pure aluminum, the working fluid used is kerosene; for the materials made of 304/304L stainless steel and 316/ For 316L stainless steel discs, the electrode material used is tungsten wire with a diameter of 0.03-0.08mm; for discs made of T1/T2 copper, the electrode material used is molybdenum wire with a diameter of 0.03-0.08mm; The material is a disc of 1050/1060/1070 pure aluminum, and the electrode material used is brass wire with a diameter of 0.03-0.08mm.
所述的高洁净限流密封垫片的制造方法，步骤(2)中，微孔加工所采用的峰值电流为0.2～0.3A，电流脉宽为2～4μs，脉冲时间为90～110μs，加工电容为3000～3500pF，电极与工件之间的距离控制在40～55μm，加工电极振动振幅为4～6×10-6m，振动频率为900～1100Hz，转速为8000～12000rpm。In the manufacturing method of the high-clean current-limiting sealing gasket, in step (2), the peak current used for micropore processing is 0.2-0.3A, the current pulse width is 2-4μs, and the pulse time is 90-110μs. The capacitance is 3000-3500pF, the distance between the electrode and the workpiece is controlled at 40-55μm, the vibration amplitude of the processing electrode is 4-6×10 -6 m, the vibration frequency is 900-1100Hz, and the rotation speed is 8000-12000rpm.
所述的高洁净限流密封垫片的制造方法，步骤(3)中，进行退火软化处理时，使用的电加热装置为管式高温炉，通入含有8～12vol％氢气的氩氢混合气，对于材质为304/304L不锈钢和316/316L不锈钢的圆片，其热处理温度为1000℃～1100℃，保温时间为8～20分钟，迅速水冷；对于材质为T1/T2紫铜的圆片，其热处理温度为400～500℃，保温时间为10～20分钟，迅速水冷；对于材质为1050/1060/1070纯铝的圆片，其热处理温度为360～420℃，保温时间为30～40分钟，迅速水冷。In the manufacturing method of the high-clean current-limiting sealing gasket, in step (3), when performing annealing and softening treatment, the electric heating device used is a tubular high-temperature furnace, and an argon-hydrogen mixture containing 8-12vol% hydrogen is fed , for the discs made of 304/304L stainless steel and 316/316L stainless steel, the heat treatment temperature is 1000 ℃ ~ 1100 ℃, the holding time is 8 to 20 minutes, and rapid water cooling; for the discs made of T1/T2 copper, the The heat treatment temperature is 400-500°C, the holding time is 10-20 minutes, and the water is cooled rapidly; for the wafer made of 1050/1060/1070 pure aluminum, the heat treatment temperature is 360-420°C, and the holding time is 30-40 minutes. Rapid water cooling.
所述的高洁净限流密封垫片的制造方法，步骤(4)中，电解抛光时，对于材质为304/304L不锈钢的圆片，所使用的电解抛光液的配方为：磷酸140～180g/L，六次甲基四胺10～30g/L，硫酸70～90mL/L，丙三醇40～60mL/L，邻苯甲酰磺酰亚胺5～15g/L，水余量；电解抛光的电压为18～22V，电解抛光的时间为5～7分钟，电解抛光的温度为55～65℃；对于材质为316/316L不锈钢的圆片，所使用的电解抛光液的配方为：高氯酸190～210g/L，冰醋酸余量；电解抛光的电压为25～35V，电解抛光的时间为7～9分钟，电解抛光的温度为75～85℃；对于材质为T1/T2紫铜的圆片，其所使用的电解抛光液的配方为：正磷酸820～830mL/L，去离子水余量；电解抛光的电压为1～3V，时间为35～45分钟，电解抛光的温度为35～45℃；对于材质为1050/1060/1070纯铝的圆片，其所使用的电解抛光液的配方为：高氯酸90～110mL/L，无水乙醇余量；电解抛光的电压为29～31V，电解抛光的时间为25～35秒，电解抛光的温度为35～45℃。In the manufacturing method of the high-clean current-limiting sealing gasket, in step (4), during electropolishing, for the wafer made of 304/304L stainless steel, the formula of the electropolishing liquid used is: phosphoric acid 140-180g/ L, hexamethylenetetramine 10-30g/L, sulfuric acid 70-90mL/L, glycerin 40-60mL/L, o-benzoylsulfonimide 5-15g/L, water balance; electrolytic polishing The voltage of the electrolytic polishing is 18-22V, the time of electrolytic polishing is 5-7 minutes, and the temperature of electrolytic polishing is 55-65°C; for the wafer made of 316/316L stainless steel, the formula of the electrolytic polishing liquid used is: high chlorine Acid 190-210g/L, glacial acetic acid balance; electrolytic polishing voltage is 25-35V, electrolytic polishing time is 7-9 minutes, electrolytic polishing temperature is 75-85°C; for rounds made of T1/T2 copper film, the formula of the electropolishing liquid used is: orthophosphoric acid 820-830mL/L, the balance of deionized water; the voltage of electropolishing is 1-3V, the time is 35-45 minutes, and the temperature of electropolishing is 35- 45°C; For wafers made of 1050/1060/1070 pure aluminum, the formula of the electrolytic polishing solution used is: perchloric acid 90-110mL/L, the balance of absolute ethanol; the voltage of electrolytic polishing is 29- 31V, the electrolytic polishing time is 25-35 seconds, and the electrolytic polishing temperature is 35-45°C.
所述的高洁净限流密封垫片的制造方法，步骤(5)中，钝化处理时，对于材质为304/304L不锈钢的圆片，所使用的钝化液的配方为：硫酸8～12ml/L，硝酸钾15～25g/L，水余量；钝化的时间为18～22分钟，钝化的温度为80～85℃；对于材质为316/316L不锈钢的圆片，所使用的钝化液的配方为：硝酸340～360mL/L，去离子水余量；钝化的时间为25～35分钟，钝化的温度为45～55℃；对于材质为T1/T2紫铜的圆片，所使用的钝化液的配方为：硫酸15～17ml/L，三氧化铬90～110g/L，水余量；钝化的时间为15～25秒，钝化的温度为25～35℃；对于材质为1050/1060/1070纯铝的圆片，所使用的钝化液的配方为：硫酸35～37ml/L，三氧化铬190～210g/L，水余量；钝化的时间为25～35秒，钝化的温度为25～30℃。In the manufacturing method of the high-clean current-limiting sealing gasket, in step (5), during the passivation treatment, for the disc made of 304/304L stainless steel, the formula of the passivation solution used is: 8-12ml of sulfuric acid /L, potassium nitrate 15-25g/L, water balance; the passivation time is 18-22 minutes, and the passivation temperature is 80-85°C; The formula of the chemical solution is: nitric acid 340~360mL/L, deionized water balance; the passivation time is 25~35 minutes, and the passivation temperature is 45~55°C; for the disc made of T1/T2 copper, The formula of the passivation solution used is: sulfuric acid 15-17ml/L, chromium trioxide 90-110g/L, water balance; the passivation time is 15-25 seconds, and the passivation temperature is 25-35°C; For wafers made of 1050/1060/1070 pure aluminum, the formula of the passivation solution used is: sulfuric acid 35-37ml/L, chromium trioxide 190-210g/L, water balance; passivation time is 25 ~35 seconds, the passivation temperature is 25~30°C.
本发明具有以下优点及有益效果：The present invention has the following advantages and beneficial effects:
(1)本发明使用金属材料少，流程简单高效；(1) The present invention uses few metal materials, and the process is simple and efficient;
(2)采用本发明制作的高洁净限流密封垫片可以长期稳定保存，方便现场使用；(2) The high-clean flow-limiting sealing gasket made by the present invention can be stored stably for a long time, and is convenient for on-site use;
(3)采用本发明制作的高洁净限流密封垫片可以在接头处获得很低的泄漏率(<6×10-12std cm3/s)；(3) The high-clean flow-limiting sealing gasket made by the present invention can obtain a very low leakage rate (<6×10 -12 std cm 3 /s) at the joint;
(4)采用本发明制作的高洁净限流密封垫片其表面具有良好的抵抗腐蚀的能力，因此可用于腐蚀气体管路的接头密封；(4) The surface of the high-clean flow-limiting sealing gasket made by the present invention has good corrosion resistance, so it can be used for joint sealing of corrosive gas pipelines;
(5)采用本发明制作的高洁净限流密封垫片能够承受>200℃的高温，因此可用于高温气体管路的接头密封；(5) The high-clean flow-limiting sealing gasket made by the present invention can withstand high temperatures >200°C, so it can be used for joint sealing of high-temperature gas pipelines;
(6)采用本发明制作的高洁净限流密封垫片可以获得极低的气体流量，可以用于特殊的流量需求；(6) The high-clean flow-limiting sealing gasket made by the present invention can obtain extremely low gas flow, and can be used for special flow requirements;
(7)采用本发明制作的高洁净限流密封垫片具有非常紧凑的尺寸结构，可获得更为紧凑的气路系统，降低安装和使用成本，可同时实现密封和限流的效果，可大大降低相关气路系统的尺寸大小，降低安装和使用成本。(7) The high-clean flow-limiting sealing gasket made by the present invention has a very compact size structure, which can obtain a more compact air circuit system, reduce installation and use costs, and can realize the effects of sealing and flow-limiting at the same time, which can greatly Reduce the size of the relevant gas system, reduce installation and use costs.
附图说明Description of drawings
图1.本发明的操作流程示意图。Fig. 1. Schematic diagram of the operation flow of the present invention.
图2.本发明高洁净限流密封垫片的结构示意简图。Fig. 2. A schematic diagram of the structure of the high-clean flow-limiting sealing gasket of the present invention.
具体实施方式Detailed ways
如图1所示，在具体实施过程中，本发明高洁净限流密封垫片的制造方法，包括如下步骤：As shown in Figure 1, in the specific implementation process, the manufacturing method of the high-clean flow-limiting sealing gasket of the present invention comprises the following steps:
(1)采用304/304L不锈钢板，或者316/316L不锈钢板，或者T1/T2紫铜板，或者1050/1060/1070纯铝板，板厚为1～2mm，通过冲压或者激光切割的方式，加工生成外径为12～20mm的金属圆片。(1) 304/304L stainless steel plate, or 316/316L stainless steel plate, or T1/T2 copper plate, or 1050/1060/1070 pure aluminum plate, with a thickness of 1-2 mm, is processed by stamping or laser cutting A metal disc with an outer diameter of 12 to 20 mm.
(2)采用深微孔电火花加工机床对圆片中心进行直径为0.05～0.1mm微孔的成形加工，对于材质为304/304L不锈钢和316/316L不锈钢，以及T1/T2紫铜的圆片，其加工时所使用的工作液为绝缘强度为15～20MΩ·cm的去离子水，而对于材质为1050/1060/1070纯铝的圆片，其加工时所使用的工作液为煤油；对于材质为304/304L不锈钢和316/316L不锈钢的圆片，其加工时所使用的电极材料为钨丝，直径为0.03～0.08mm；对于材质为T1/T2紫铜的圆片，其加工时所使用的电极材料为钼丝，直径为0.03～0.08mm；对于材质为1050/1060/1070纯铝的圆片，其加工时所使用的电极材料为黄铜丝，直径为0.03～0.08mm；(2) Use a deep micro-hole EDM machine tool to form a micro-hole with a diameter of 0.05 to 0.1 mm in the center of the wafer. For wafers made of 304/304L stainless steel, 316/316L stainless steel, and T1/T2 copper, The working fluid used in the processing is deionized water with a dielectric strength of 15-20MΩ·cm, and for the wafer made of 1050/1060/1070 pure aluminum, the working fluid used in the processing is kerosene; for the material For 304/304L stainless steel and 316/316L stainless steel discs, the electrode material used for processing is tungsten wire with a diameter of 0.03-0.08mm; for T1/T2 copper discs, the electrode material used for processing The electrode material is molybdenum wire with a diameter of 0.03-0.08mm; for the disc made of 1050/1060/1070 pure aluminum, the electrode material used in the processing is brass wire with a diameter of 0.03-0.08mm;
在微孔成形加工过程中所选用的峰值电流为0.2～0.3A，电流脉宽为2～4μs，脉冲时间为90～110μs，加工电容为3000～3500pF，电极与工件之间的距离控制在40～55μm，加工电极振动振幅为4～6×10-6m，振动频率为900～1100Hz，转速为8000～12000rpm。The peak current selected in the microhole forming process is 0.2-0.3A, the current pulse width is 2-4μs, the pulse time is 90-110μs, the processing capacitance is 3000-3500pF, and the distance between the electrode and the workpiece is controlled at 40 ~55μm, the vibration amplitude of the processing electrode is 4~6×10 -6 m, the vibration frequency is 900~1100Hz, and the rotation speed is 8000~12000rpm.
(3)待完成微孔加工成型之后，对带孔金属圆片进行退火软化处理，所使用的电加热装置为管式高温炉，通入含有8～12vol％氢气的氩氢混合气，对于材质为304/304L不锈钢和和316/316L不锈钢的圆片，其热处理温度为1000℃～1100℃，保温时间为8～20分钟，迅速水冷；对于材质为T1/T2紫铜的圆片，其热处理温度为400～500℃，保温时间为10～20分钟，迅速水冷；对于材质为1050/1060/1070纯铝的圆片，其热处理温度为360～420℃，保温时间为30～40分钟，迅速水冷。(3) After the micropore processing and forming are completed, the metal disc with holes is annealed and softened. The electric heating device used is a tube-type high-temperature furnace, and an argon-hydrogen mixture containing 8-12vol% hydrogen is introduced. For the material For 304/304L stainless steel and 316/316L stainless steel discs, the heat treatment temperature is 1000 ℃ ~ 1100 ℃, the holding time is 8 to 20 minutes, and rapid water cooling; for T1/T2 copper discs, the heat treatment temperature 400-500°C, the holding time is 10-20 minutes, rapid water cooling; for 1050/1060/1070 pure aluminum wafers, the heat treatment temperature is 360-420°C, the holding time is 30-40 minutes, rapid water cooling .
(4)对经过热处理之后带有微孔的圆片，进行电解抛光处理，其中对于材质为304/304L不锈钢的圆片，所使用的电解抛光液的配方为磷酸140～180g/L，六次甲基四胺10～30g/L，硫酸(浓度98wt％)70～90mL/L，丙三醇40～60mL/L，邻苯甲酰磺酰亚胺5～15g/L，水余量；电解抛光的电压为18～22V，电解抛光的时间为5～7分钟，电解抛光的温度为55～65℃；对于材质为316/316L不锈钢的圆片，所使用的电解抛光液的配方为高氯酸(浓度20wt％)190～210g/L，冰醋酸790～810g/L；电解抛光的电压为25～35V，电解抛光的时间为7～9分钟，电解抛光的温度为75～85℃；对于材质为T1/T2紫铜的圆片，其所使用的电解抛光液的配方为正磷酸820～830mL/L，去离子水170～180mL/L；电解抛光的电压为1～3V，时间为35～45分钟，电解抛光的温度为35～45℃；对于材质为1050/1060/1070纯铝的圆片，其所使用的电解抛光液的配方为高氯酸(浓度20wt％)90～110mL/L，无水乙醇890～910mL/L；电解抛光的电压为29～31V，电解抛光的时间为25～35秒，电解抛光的温度为35～45℃。(4) Perform electropolishing treatment on the disc with micropores after heat treatment. For the disc made of 304/304L stainless steel, the formula of the electropolishing liquid used is phosphoric acid 140-180g/L, six times Methyltetramine 10-30g/L, sulfuric acid (concentration 98wt%) 70-90mL/L, glycerol 40-60mL/L, o-benzoylsulfonimide 5-15g/L, water balance; electrolysis The polishing voltage is 18-22V, the electrolytic polishing time is 5-7 minutes, and the electrolytic polishing temperature is 55-65°C; for the wafer made of 316/316L stainless steel, the formula of the electrolytic polishing solution used is high chlorine Acid (concentration 20wt%) 190～210g/L, glacial acetic acid 790～810g/L; The voltage of electrolytic polishing is 25～35V, the time of electrolytic polishing is 7～9 minutes, the temperature of electrolytic polishing is 75～85 ℃; The material is T1/T2 copper disc, the formula of the electrolytic polishing solution used is 820-830mL/L orthophosphoric acid, 170-180mL/L deionized water; the voltage of electrolytic polishing is 1-3V, and the time is 35- For 45 minutes, the temperature of electropolishing is 35-45°C; for wafers made of 1050/1060/1070 pure aluminum, the formula of the electropolishing liquid used is perchloric acid (concentration 20wt%) 90-110mL/L , absolute ethanol 890-910mL/L; the voltage of electropolishing is 29-31V, the time of electropolishing is 25-35 seconds, and the temperature of electropolishing is 35-45°C.
(5)对经过电解抛光后的带孔金属圆片进行钝化处理，对于材质为304/304L不锈钢的圆片，所使用的钝化液的配方为硫酸(浓度98wt％)8～12ml/L，硝酸钾15～25g/L，水余量；钝化时间为18～22分钟，钝化温度为80～85℃；对于材质为316/316L不锈钢的圆片，所使用的钝化液的配方为340～360mL/L的浓硝酸(浓度68wt％)和640～660ml/L的去离子水；钝化时间为25～35分钟，钝化温度为45～55℃；对于材质为T1/T2紫铜的圆片，所使用的钝化液的配方为硫酸(浓度98wt％)15～17ml/L，三氧化铬(纯度99.5wt％)90～110g/L，水余量；钝化的时间为15～25秒，钝化温度为25～35℃；对于材质为1050/1060/1070纯铝的圆片，所使用的钝化液的配方为硫酸(浓度98wt％)35～37ml/L，三氧化铬(纯度99.5wt％)190～210g/L，水余量；钝化的时间为25～35秒，钝化的温度为25～30℃。(5) Carry out passivation treatment to the metal disc with holes after electropolishing, for the disc made of 304/304L stainless steel, the formula of the passivation solution used is sulfuric acid (concentration 98wt%) 8～12ml/L , Potassium nitrate 15-25g/L, water balance; passivation time is 18-22 minutes, passivation temperature is 80-85°C; for wafers made of 316/316L stainless steel, the formula of the passivation solution used 340-360mL/L concentrated nitric acid (concentration 68wt%) and 640-660ml/L deionized water; the passivation time is 25-35 minutes, the passivation temperature is 45-55°C; the material is T1/T2 copper The disc, the formula of the passivation solution used is sulfuric acid (concentration 98wt%) 15～17ml/L, chromium trioxide (purity 99.5wt%) 90～110g/L, water surplus; The time of passivation is 15 ~ 25 seconds, the passivation temperature is 25 ~ 35 ° C; for the material of the 1050/1060/1070 pure aluminum wafer, the formula of the passivation solution used is sulfuric acid (concentration 98wt%) 35 ~ 37ml/L, trioxide Chromium (purity 99.5wt%) 190-210g/L, water balance; passivation time is 25-35 seconds, passivation temperature is 25-30°C.
(6)对钝化处理后的带孔金属圆片采用去离子水超声清洗，以去除钝化液，并在百级无尘洁净室中进行烘干，并对每片进行单独真空塑料封装，以实现很好的保护。(6) Use deionized water to ultrasonically clean the metal disc with holes after passivation treatment to remove the passivation solution, and dry it in a class 100 dust-free clean room, and carry out separate vacuum plastic packaging for each piece, for good protection.
下面，通过实施例对本发明进一步详细阐述。Below, the present invention is described in further detail through examples.
实施例1Example 1
本实施例中，采用板厚为1mm的304L不锈钢板，通过冲压的方式，加工生成外径为12mm的圆片，采用深微孔电火花加工机床对圆片中心进行直径为0.1mm微孔的成形加工，加工时所使用的工作液为绝缘强度为16MΩ·cm的去离子水，所使用的电极材料为钨丝，直径为0.08mm；在微孔成形加工过程中所选用的峰值电流为0.25A，电流脉宽为2μs，脉冲时间为90μs，加工电容为3000pF，电极与工件之间的距离控制在40μm，加工电极的振动振幅为4×10-6m，振动频率为900Hz，转速为8000rpm。待完成微孔加工成型之后，对其进行退火软化处理，所使用的电加热装置为管式高温炉，通入含有10vol％氢气的氩氢混合气，其热处理温度为1000℃，保温时间为10分钟，迅速水冷。然后，对经过热处理之后带有微孔的圆片，进行电解抛光，所使用的电解抛光液的配方为磷酸160g/L，六次甲基四胺20g/L，硫酸(浓度98wt％)80mL/L，丙三醇50mL/L，邻苯甲酰磺酰亚胺10g/L，水余量；电解抛光的电压为20V，电解抛光的时间为6分钟，电解抛光的温度为60℃。然后，对经过电解抛光后的圆片进行钝化处理，所使用的钝化液的配方为硫酸(浓度98wt％)10ml/L，硝酸钾20g/L，水余量；钝化的时间为20分钟，钝化的温度为80℃。对进行钝化后的圆片采用去离子水超声清洗，以去除钝化液，并在百级无尘洁净室中进行烘干，并对每片进行单独真空塑料封装，以实现很好的保护。In this embodiment, a 304L stainless steel plate with a plate thickness of 1 mm is used to process a disc with an outer diameter of 12 mm by stamping, and a deep micro-hole EDM machine tool is used to drill a micro-hole with a diameter of 0.1 mm in the center of the disc. Forming process, the working fluid used in the process is deionized water with a dielectric strength of 16MΩ·cm, the electrode material used is tungsten wire with a diameter of 0.08mm; the peak current selected during the micropore forming process is 0.25 A. The current pulse width is 2μs, the pulse time is 90μs, the processing capacitance is 3000pF, the distance between the electrode and the workpiece is controlled at 40μm, the vibration amplitude of the processing electrode is 4×10 -6 m, the vibration frequency is 900Hz, and the rotation speed is 8000rpm . After the micropore processing and forming are completed, it is annealed and softened. The electric heating device used is a tubular high-temperature furnace, and an argon-hydrogen mixture containing 10vol% hydrogen is fed into it. The heat treatment temperature is 1000 ° C, and the holding time is 10 Minutes, rapid water cooling. Then, carry out electrolytic polishing to the disc with micropore after heat treatment, the formula of the electrolytic polishing liquid used is phosphoric acid 160g/L, hexamethylenetetramine 20g/L, sulfuric acid (concentration 98wt%) 80mL/L L, glycerin 50mL/L, o-benzoylsulfonimide 10g/L, water balance; the electropolishing voltage is 20V, the electropolishing time is 6 minutes, and the electropolishing temperature is 60°C. Then, carry out passivation treatment to the wafer after electrolytic polishing, the formula of the passivation solution used is sulfuric acid (concentration 98wt%) 10ml/L, potassium nitrate 20g/L, water surplus; The time of passivation is 20 Minutes, the passivation temperature is 80°C. The passivated wafers are ultrasonically cleaned with deionized water to remove the passivation solution, and dried in a class 100 dust-free clean room, and each piece is individually vacuum-packed in plastic to achieve good protection .
实施例2Example 2
采用板厚为1mm的316L不锈钢板，通过激光切割的方式，加工生成外径为20mm的圆片，采用深微孔电火花加工机床对圆片中心进行直径为0.06mm微孔的成形加工，加工时所使用的工作液为绝缘强度为18MΩ·cm的去离子水，加工时所使用的电极材料为钨丝，直径为0.04mm；在微孔成形加工过程中所选用的峰值电流为0.25A，电流脉宽为2μs，脉冲时间为100μs，加工电容为3100pF，电极与工件之间的距离控制在42μm，加工电极的振动振幅为4×10-6m，振动频率为1000Hz，转速为10000rpm。待完成微孔加工成型之后，对其进行退火软化处理，所使用的电加热装置为管式高温炉，通入含有10vol％氢气的氩氢混合气，其热处理温度为1100℃，保温时间为12分钟，迅速水冷。然后，对经过热处理之后带有微孔的圆片，进行电解抛光，所使用的电解抛光液的配方为高氯酸(浓度20wt％)200g/L，冰醋酸800g/L，电解抛光的电压为30V，电解抛光的时间为8分钟，电解抛光的温度为80℃。然后，对经过电解抛光后的圆片进行钝化处理，所使用的钝化液的配方为浓硝酸(浓度68wt％)350mL/L和去离子水650ml/L，钝化时间为30分钟，钝化温度为50℃。对进行钝化后的圆片采用去离子水超声清洗，以去除钝化液，并在百级无尘洁净室中进行烘干，并对每片进行单独真空塑料封装，以实现很好的保护。A 316L stainless steel plate with a plate thickness of 1 mm is used to process a disc with an outer diameter of 20 mm by laser cutting, and a deep micro-hole EDM machine is used to form a micro-hole with a diameter of 0.06 mm in the center of the disc. The working fluid used during the process is deionized water with a dielectric strength of 18MΩ·cm, and the electrode material used during processing is tungsten wire with a diameter of 0.04mm; the peak current selected during the micropore forming process is 0.25A, The current pulse width is 2μs, the pulse time is 100μs, the processing capacitance is 3100pF, the distance between the electrode and the workpiece is controlled at 42μm, the vibration amplitude of the processing electrode is 4×10 -6 m, the vibration frequency is 1000Hz, and the rotation speed is 10000rpm. After the micropore processing and forming are completed, it is annealed and softened. The electric heating device used is a tubular high-temperature furnace, and an argon-hydrogen mixture containing 10vol% hydrogen is fed into it. The heat treatment temperature is 1100 ° C, and the holding time is 12 Minutes, rapid water cooling. Then, carry out electrolytic polishing to the disc with micropore after heat treatment, the formula of the used electrolytic polishing liquid is perchloric acid (concentration 20wt%) 200g/L, glacial acetic acid 800g/L, the voltage of electrolytic polishing is 30V, the time of electrolytic polishing is 8 minutes, and the temperature of electrolytic polishing is 80°C. Then, carry out passivation treatment to the wafer after electrolytic polishing, the formula of the passivation solution used is concentrated nitric acid (concentration 68wt%) 350mL/L and deionized water 650ml/L, passivation time is 30 minutes, passivation The melting temperature is 50°C. The passivated wafers are ultrasonically cleaned with deionized water to remove the passivation solution, and dried in a class 100 dust-free clean room, and each piece is individually vacuum-packed in plastic to achieve good protection .
实施例3Example 3
采用板厚为2mm的T2紫铜板，通过冲压的方式，加工生成外径为12mm的圆片，采用深微孔电火花加工机床对圆片中心进行直径为0.08mm微孔的成形加工，其加工时所使用的工作液为绝缘强度为20MΩ·cm的去离子水，所使用的电极材料为钼丝，直径为0.07mm；在微孔成形加工过程中所选用的峰值电流为0.3A，电流脉宽为4μs，脉冲时间为100μs，加工电容为3500pF，电极与工件之间的距离控制在50μm，加工电极的振动振幅为6×10-6m，振动频率为1100Hz，转速为12000rpm。待完成微孔加工成型之后，对其进行退火软化处理，所使用的电加热装置为管式高温炉，通入含有10vol％氢气的氩氢混合气，热处理温度为400～500℃，保温时间为10分钟，迅速水冷。然后，对经过热处理之后带有微孔的圆片，进行电解抛光，所使用的电解抛光液的配方为正磷酸825mL/L，去离子水175mL/L，电解抛光的电压为2V，时间为40分钟，电解抛光的温度为40℃。然后，对经过电解抛光后的圆片进行钝化处理，所使用的钝化液的配方为硫酸(浓度98wt％)16ml/L，三氧化铬(纯度99.5wt％)100g/L，水余量；钝化的时间为20秒，钝化的温度为30℃。对进行钝化后的圆片采用去离子水超声清洗，以去除钝化液，并在百级无尘洁净室中进行烘干，并对每片进行单独真空塑料封装，以实现很好的保护。A T2 red copper plate with a plate thickness of 2mm is used to process a disc with an outer diameter of 12mm by stamping. A deep micro-hole EDM machine is used to form a micro-hole with a diameter of 0.08mm in the center of the disc. The processing The working fluid used is deionized water with a dielectric strength of 20MΩ·cm, and the electrode material used is molybdenum wire with a diameter of 0.07mm; the peak current selected during the micropore forming process is 0.3A, and the current pulse The width is 4μs, the pulse time is 100μs, the processing capacitance is 3500pF, the distance between the electrode and the workpiece is controlled at 50μm, the vibration amplitude of the processing electrode is 6×10 -6 m, the vibration frequency is 1100Hz, and the rotation speed is 12000rpm. After the micropore processing and forming are completed, it is annealed and softened. The electric heating device used is a tubular high-temperature furnace, which is fed with argon-hydrogen mixture containing 10vol% hydrogen. The heat treatment temperature is 400-500 ° C, and the holding time is 10 minutes, rapid water cooling. Then, electrolytic polishing is carried out on the wafer with micropores after heat treatment. The formula of the electrolytic polishing liquid used is orthophosphoric acid 825mL/L, deionized water 175mL/L, the voltage of electrolytic polishing is 2V, and the time is 40 Minutes, the temperature of electrolytic polishing is 40 ℃. Then, carry out passivation treatment to the wafer after electrolytic polishing, the formula of the passivation solution used is sulfuric acid (concentration 98wt%) 16ml/L, chromium trioxide (purity 99.5wt%) 100g/L, water surplus ; The passivation time is 20 seconds, and the passivation temperature is 30°C. The passivated wafers are ultrasonically cleaned with deionized water to remove the passivation solution, and dried in a class 100 dust-free clean room, and each piece is individually vacuum-packed in plastic to achieve good protection .
如图2所示，采用本发明生产的高洁净限流密封垫片，是一种中间有微孔、表面光洁度高、进行过钝化处理的圆形金属薄片，其所使用的材质为316L不锈钢。限流密封垫片的上下两个表面的粗糙度Ra<0.25μm，经过钝化处理，可以长期保存，并且具有很好的密封效果、很强的耐高温和耐腐蚀能力，可用于特殊气体介质的接头密封。As shown in Figure 2, the high-clean current-limiting sealing gasket produced by the present invention is a round metal sheet with micropores in the middle, high surface finish, and passivation treatment, and the material used is 316L stainless steel . The roughness of the upper and lower surfaces of the current-limiting sealing gasket is Ra<0.25μm. After passivation treatment, it can be stored for a long time, and has a good sealing effect, strong high temperature resistance and corrosion resistance, and can be used in special gas media. joint seal.
限流密封垫片整体呈圆片形，所述圆片的直径为12～20mm，所述圆片的厚度为1～2mm。限流密封垫片的中心孔为锥孔和微孔上下组合的孔结构，锥孔为上大下小的锥形孔，锥孔的下端直径与微孔的直径相同。所述微孔的直径为0.05～0.1mm，所述微孔的高度为0.6～0.8mm。The current-limiting sealing gasket is generally in the shape of a disc, the diameter of the disc is 12-20 mm, and the thickness of the disc is 1-2 mm. The central hole of the current-limiting sealing gasket is a hole structure in which a cone hole and a microhole are combined up and down. The cone hole is a tapered hole with a large top and a small bottom. The diameter of the micropores is 0.05-0.1mm, and the height of the micropores is 0.6-0.8mm.
采用本发明生产的限流密封垫片，其上下两个表面用于端面密封型接头的密封，限流密封垫片中间的微孔用于限流，以实现微小气体流量。本发明可有效推进高洁净限流密封垫片的开发应用，限流密封垫片中心的微孔可获得极低的气体流量，满足某些特殊的流量需求，对于发展某些特殊用途气路系统具有重要意义。The upper and lower surfaces of the current-limiting sealing gasket produced by the invention are used for sealing the end-face sealing type joints, and the micropores in the middle of the current-limiting sealing gasket are used for current limiting to realize tiny gas flow. The invention can effectively promote the development and application of high-clean flow-limiting sealing gaskets. The micropores in the center of the flow-limiting sealing gaskets can obtain extremely low gas flow, which can meet some special flow requirements and is useful for the development of some special-purpose gas circuit systems. is of great significance.
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