CN113463178B - A kind of electrolytic polishing liquid and electrolytic polishing method of tungsten-based wire or sheet - Google Patents
A kind of electrolytic polishing liquid and electrolytic polishing method of tungsten-based wire or sheet Download PDFInfo
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- 238000005498 polishing Methods 0.000 title claims abstract description 132
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 106
- 239000010937 tungsten Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000007788 liquid Substances 0.000 title description 18
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 33
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 33
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 33
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- IRUDSQHLKGNCGF-UHFFFAOYSA-N 2-methylhex-1-ene Chemical compound CCCCC(C)=C IRUDSQHLKGNCGF-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract 6
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 3
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 3
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 3
- KVFVBPYVNUCWJX-UHFFFAOYSA-M ethyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(C)C KVFVBPYVNUCWJX-UHFFFAOYSA-M 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000004381 surface treatment Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000007517 polishing process Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 45
- 239000000463 material Substances 0.000 description 37
- 239000002585 base Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229960000935 dehydrated alcohol Drugs 0.000 description 8
- 238000012876 topography Methods 0.000 description 8
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 210000004400 mucous membrane Anatomy 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
- C25F3/26—Polishing of heavy metals of refractory metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
Abstract
Description
技术领域technical field
本发明涉及难熔金属表面处理技术领域，具体涉及一种安全、环保、可控、高效的钨基丝材或片材的电解抛光液及其电解抛光方法。The invention relates to the technical field of refractory metal surface treatment, in particular to a safe, environment-friendly, controllable and efficient electrolytic polishing liquid for tungsten-based wire or sheet and an electrolytic polishing method thereof.
背景技术Background technique
钨基丝材或片材具有高熔点、高强度、高硬度等特点，被广泛应用于航天发动机、核反应堆等高技术领域。钨基丝材或片材在开发制备过程中，往往需要进行挤压、拉拔、轧制等多道次加工，但由于此类材料塑性差、硬度高，机械加工难度较大，而且难以得到表面较为平整、低粗糙度的工件表面。因此，亟需一种简单、高效的工件表面处理方法。Tungsten-based wire or sheet has the characteristics of high melting point, high strength and high hardness, and is widely used in high-tech fields such as aerospace engines and nuclear reactors. In the development and preparation process of tungsten-based wire or sheet, it is often necessary to carry out multi-pass processing such as extrusion, drawing, rolling, etc., but due to the poor plasticity and high hardness of such materials, machining is difficult and difficult to obtain The workpiece surface with relatively flat surface and low roughness. Therefore, a simple and efficient workpiece surface treatment method is urgently needed.
电解抛光是一种特殊的阳极电化学加工方式，在该过程中被抛光件作阳极，不溶性金属作阴极，通过电化学阳极溶解，从而达到去除工件表面划痕、毛刺等效果，使工件表面平整光亮。目前比较公认的电解抛光原理为黏膜理论，即工件上脱离的金属离子与抛光液中的磷酸形成一层磷酸盐膜吸附在工件表面，该黏膜在凸起处较薄，凹处较厚，因凸起处电流密度高而溶解快，随黏膜流动，凹凸不断变化，粗糙表面逐渐被整平的过程。随着金属材料尤其是高硬度材料应用的日益增多，电解抛光逐渐成为了一种广泛应用的表面处理工艺，且该工艺成本低、效率高、效果好、操作方便，可以很好的应用于钨基丝材或片材的材料表面处理。Electropolishing is a special anodic electrochemical processing method. In this process, the polished piece is used as the anode, and the insoluble metal is used as the cathode. The electrochemical anode is dissolved to achieve the effect of removing scratches and burrs on the surface of the workpiece and making the surface of the workpiece smooth. bright. At present, the generally accepted principle of electrolytic polishing is the mucous membrane theory, that is, the metal ions detached from the workpiece and the phosphoric acid in the polishing solution form a layer of phosphate film and adsorb on the surface of the workpiece. The current density of the protrusion is high and the dissolution is fast. With the flow of the mucous membrane, the unevenness is constantly changing, and the rough surface is gradually leveled. With the increasing application of metal materials, especially high-hardness materials, electrolytic polishing has gradually become a widely used surface treatment process, and the process is low in cost, high in efficiency, good in effect and convenient in operation, and can be well applied to tungsten Surface treatment of materials based on wire or sheet.
如中国专利CN200410103517公开了一种高精度钨片的电解抛光方法，所述抛光液由NaOH、KClO3和K2CO3按照1:8:3的比例进行配制，其中KClO3属于易爆试剂，且运输和保存要求较高；中国专利CN104060320A公开了一种钨螺旋线电解抛光的拋光液，所述拋光液由磷酸钠、氢氧化钠、丙三醇和水配制而成，采用该电解抛光液进行电解抛光需要每隔一定时间对工件表面的不溶性电解产物进行清洗，这就导致抛光效率低；中国专利CN105887179公开了一种钨合金或钼合金的电解抛光液和电解抛光方法，所述抛光液由氢氧化钠、碳酸钠和钼酸钠按照35:8:1的重量比例进行配制，电解抛光过程中会产生大量不溶性气体，降低了抛光速率，且电解抛光过程中还需加热。因此，开发一种安全、环保、可控、效率高的电解抛光方法是十分有必要的。For example, Chinese patent CN200410103517 discloses an electrolytic polishing method for high-precision tungsten sheets. The polishing solution is prepared by NaOH, KClO 3 and K 2 CO 3 in a ratio of 1:8:3, wherein KClO 3 is an explosive reagent. And the transportation and storage requirements are relatively high; Chinese patent CN104060320A discloses a polishing solution for tungsten helix electrolytic polishing, the polishing solution is prepared from sodium phosphate, sodium hydroxide, glycerol and water, and the electrolytic polishing solution is used for Electropolishing needs to clean the insoluble electrolytic products on the workpiece surface at regular intervals, which leads to low polishing efficiency; Chinese patent CN105887179 discloses a kind of electrolytic polishing liquid and electropolishing method of tungsten alloy or molybdenum alloy, and the polishing liquid is composed of Sodium hydroxide, sodium carbonate and sodium molybdate are prepared in a weight ratio of 35:8:1. A large amount of insoluble gas will be generated during the electropolishing process, which reduces the polishing rate, and heating is required during the electropolishing process. Therefore, it is necessary to develop a safe, environmentally friendly, controllable and efficient electrolytic polishing method.
发明内容Contents of the invention
本发明所要解决的技术问题在于针对上述现有技术中的不足，提供一种钨基丝材或片材的电解抛光液，该抛光液为季铵碱、无水乙醇、2-甲基-1-己烯和硫酸钠的水溶液，采用该电解抛光液进行电解抛光过程中无不溶性气体产生，无需加热，因此采用该电解抛光液进行电解抛光安全、环保、可控、高效。The technical problem to be solved by the present invention is to provide an electrolytic polishing solution for tungsten-based wire or sheet, which is composed of quaternary ammonium base, absolute ethanol, 2-methyl-1 - An aqueous solution of hexene and sodium sulfate, no insoluble gas is generated during the electropolishing process using the electrolytic polishing solution, and no heating is required, so the electrolytic polishing using the electrolytic polishing solution is safe, environmentally friendly, controllable, and efficient.
本发明的技术解决方案如下：Technical solution of the present invention is as follows:
一种钨基丝材或片材的电解抛光液，包括以下组分：季铵碱、无水乙醇、2-甲基-1-己烯、硫酸钠和水，电解抛光液中季铵碱的浓度为20～40g/L，无水乙醇的浓度为10～50g/L，2-甲基-1-己烯的浓度为1～5g/L，硫酸钠的浓度为50～100g/L。An electrolytic polishing solution for tungsten-based wire or sheet materials, comprising the following components: quaternary ammonium base, absolute ethanol, 2-methyl-1-hexene, sodium sulfate and water, the quaternary ammonium base in the electrolytic polishing solution The concentration is 20-40g/L, the concentration of absolute ethanol is 10-50g/L, the concentration of 2-methyl-1-hexene is 1-5g/L, and the concentration of sodium sulfate is 50-100g/L.
本发明的一种具体实施方式中，季铵碱的浓度为25～35g/L，无水乙醇的浓度为30～40g/L，2-甲基-1-己烯的浓度为2～4g/L，硫酸钠的浓度为70～80g/L。In a specific embodiment of the present invention, the concentration of the quaternary ammonium base is 25 to 35 g/L, the concentration of absolute ethanol is 30 to 40 g/L, and the concentration of 2-methyl-1-hexene is 2 to 4 g/L. L, the concentration of sodium sulfate is 70-80g/L.
本发明的一种具体实施方式中，季铵碱的浓度为35g/L，无水乙醇的浓度为35g/L，2-甲基-1-己烯的浓度为3g/L，硫酸钠的浓度为80g/L。In a specific embodiment of the present invention, the concentration of quaternary ammonium base is 35g/L, the concentration of dehydrated alcohol is 35g/L, the concentration of 2-methyl-1-hexene is 3g/L, the concentration of sodium sulfate 80g/L.
本发明的一种具体实施方式中，季铵碱的浓度为35g/L，无水乙醇的浓度为40g/L，2-甲基-1-己烯的浓度为3g/L，硫酸钠的浓度为80g/L。In a specific embodiment of the present invention, the concentration of quaternary ammonium base is 35g/L, the concentration of dehydrated alcohol is 40g/L, the concentration of 2-methyl-1-hexene is 3g/L, the concentration of sodium sulfate 80g/L.
本发明的一种具体实施方式中，季铵碱的浓度为25g/L，无水乙醇的浓度为35g/L，2-甲基-1-己烯的浓度为5g/L，硫酸钠的浓度为75g/L。In a specific embodiment of the present invention, the concentration of quaternary ammonium base is 25g/L, the concentration of dehydrated alcohol is 35g/L, the concentration of 2-methyl-1-hexene is 5g/L, the concentration of sodium sulfate It is 75g/L.
本发明的一种具体实施方式中，季铵碱的浓度为20g/L，无水乙醇的浓度为30g/L，2-甲基-1-己烯的浓度为2g/L，硫酸钠的浓度为100g/L。In a specific embodiment of the present invention, the concentration of quaternary ammonium base is 20g/L, the concentration of dehydrated alcohol is 30g/L, the concentration of 2-methyl-1-hexene is 2g/L, the concentration of sodium sulfate 100g/L.
本发明的一种具体实施方式中，季铵碱的浓度为35g/L，无水乙醇的浓度为50g/L，2-甲基-1-己烯的浓度为5g/L，硫酸钠的浓度为50g/L。In a specific embodiment of the present invention, the concentration of quaternary ammonium base is 35g/L, the concentration of dehydrated alcohol is 50g/L, the concentration of 2-methyl-1-hexene is 5g/L, the concentration of sodium sulfate 50g/L.
本发明的一种具体实施方式中，季铵碱选用氢氧化四甲铵、氢氧化四乙铵、氢氧化四丙铵、氢氧化四丁铵和氢氧化三甲基乙基铵中的一种或多种。In a specific embodiment of the present invention, the quaternary ammonium base is selected from one of tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide and trimethylethylammonium hydroxide or more.
本发明还提供一种采用上述电解抛光液对钨基丝材或片材进行电解抛光的方法，包括：将待处理的钨基丝材或片材置于电解抛光液中作为阳极，以镍作为阴极，调节直流稳压电源的电流密度为1.0～4.0A/cm2，优选地，电流密度为2.0～3.0A/cm2，更优选地，电流密度为2.5A/cm2，控制电解抛光液的搅拌速度为5～40r/s，优选地，搅拌速度为10～20r/s，更优选地，搅拌速度为15r/s，对钨基丝材或片材表面进行电解抛光，所述电解抛光的抛光时间不低于30s，优选地，抛光时间为100～350s。The present invention also provides a method for electropolishing tungsten-based wires or sheets using the above-mentioned electrolytic polishing solution, including: placing the tungsten-based wires or sheets to be treated in the electrolytic polishing solution as an anode, and using nickel as an anode. For the cathode, adjust the current density of the DC stabilized power supply to 1.0-4.0A/cm 2 , preferably, the current density is 2.0-3.0A/cm 2 , more preferably, the current density is 2.5A/cm 2 , and control the electrolytic polishing solution The stirring speed is 5 to 40r/s, preferably, the stirring speed is 10 to 20r/s, more preferably, the stirring speed is 15r/s, and the surface of the tungsten-based wire or sheet is electrolytically polished, and the electrolytic polishing The polishing time is not less than 30s, preferably, the polishing time is 100-350s.
本发明至少具有以下有益效果之一：The present invention has at least one of the following beneficial effects:
本发明的电解抛光液为含有季铵碱、无水乙醇、2-甲基-1-己烯和硫酸钠的水溶液，主要成分为季铵碱的碱性抛光液可以溶解阳极电解抛光产物，并搭配适量的无水乙醇、2-甲基-1-己烯和硫酸钠，电解抛光过程中适当的无水乙醇、2-甲基-1-己烯和硫酸钠可以提高工件表面抛光质量和效率，防止出现纹路、针孔等缺陷。因为，本发明通过对电解抛光液的原料和含量进行选择和合理搭配，通过无水乙醇、2-甲基-1-己烯、硫酸钠和季铵碱协同作用，使得处理后的钨基线材表面光亮平整，呈现低粗糙度，无加工产生的划痕和凹槽，抛光效果好；并且2-甲基-1-己烯对产生的气体有加成反应，从而本发明的电解抛光液在电解抛光过程中无不溶性气体产生，无需加热升温，离子流动速度快，抛光速度快。同时，本发明的电解抛光液中有效成分稳定，易于储存。The electrolytic polishing solution of the present invention is an aqueous solution containing quaternary ammonium base, dehydrated alcohol, 2-methyl-1-hexene and sodium sulfate, and the main component is the alkaline polishing solution of quaternary ammonium base, which can dissolve the anode electrolytic polishing product, and With appropriate amount of absolute ethanol, 2-methyl-1-hexene and sodium sulfate, appropriate absolute ethanol, 2-methyl-1-hexene and sodium sulfate during electropolishing can improve the quality and efficiency of workpiece surface polishing , to prevent defects such as lines and pinholes. Because, the present invention selects and rationally matches the raw materials and contents of the electrolytic polishing liquid, and through the synergistic effect of absolute ethanol, 2-methyl-1-hexene, sodium sulfate and quaternary ammonium base, the treated tungsten-based wire The surface is bright and smooth, showing low roughness, no scratches and grooves produced by processing, and the polishing effect is good; and 2-methyl-1-hexene has an addition reaction to the generated gas, so that the electrolytic polishing solution of the present invention is No insoluble gas is produced during the electropolishing process, no heating is required, the ion flow speed is fast, and the polishing speed is fast. At the same time, the active ingredients in the electrolytic polishing liquid of the present invention are stable and easy to store.
本发明的电解抛光方法操作简单，抛光效率高，电解抛光液的电解抛光速度由搅拌速度控制，无需加热，因此可控性、环保性好。因此本发明电解抛光液的组成成分和电解抛光的工艺参数设计合理，采用该电解抛光液和方法电解抛光后的钨基丝材或片材表面光泽度高，抛光效果好、效率高。The electrolytic polishing method of the present invention has simple operation and high polishing efficiency, and the electrolytic polishing speed of the electrolytic polishing liquid is controlled by the stirring speed without heating, so the controllability and environmental protection are good. Therefore, the components of the electrolytic polishing liquid and the technological parameters of the electrolytic polishing are designed reasonably, and the surface gloss of the tungsten-based wire or sheet after electrolytic polishing by using the electrolytic polishing liquid and the method is high, and the polishing effect is good and the efficiency is high.
附图说明Description of drawings
图1为本发明钨基线材电解抛光前的扫描电子显微镜照片(放大倍数150倍)；Fig. 1 is the scanning electron micrograph (150 times of magnification) of tungsten-based wire rod electrolytic polishing of the present invention;
图2为本发明实施例1钨基线材电解抛光后的扫描电子显微镜照片(放大倍数200倍)；Fig. 2 is the scanning electron microscope photo (magnification 200 times) of the tungsten-based wire rod electrolytic polishing of
图3为本发明实施例1钨基线材电解抛光后的扫描电子显微镜照片(放大倍数500倍)；Fig. 3 is the scanning electron microscope photograph (magnification 500 times) of the tungsten-based wire rod electrolytic polishing of
图4为本发明实施例1钨基线材电解抛光后的原子力形貌图(Ra＝0.06μm)；4 is an atomic force topography diagram (Ra=0.06 μm) of the tungsten-based wire material in Example 1 of the present invention after electrolytic polishing;
图5为本发明实施例2钨基线材电解抛光后的扫描电子显微镜照片(放大倍数500倍)；Fig. 5 is the scanning electron microscope photo (500 times of magnification) after the electropolishing of tungsten-based wire material of
图6为本发明实施例2钨基线材电解抛光后的原子力形貌图(Ra＝0.08μm)；Fig. 6 is an atomic force topography diagram (Ra=0.08 μm) of the tungsten-based wire material in Example 2 of the present invention after electropolishing;
图7为本发明实施例3钨基线材电解抛光后的扫描电子显微镜照片(放大倍数500倍)；Fig. 7 is the scanning electron microscope photo (magnification 500 times) of the tungsten-based wire rod electrolytic polishing of
图8为本发明实施例4钨基线材电解抛光后的扫描电子显微镜照片(放大倍数500倍)；Fig. 8 is the scanning electron microscope photograph (magnification 500 times) of the tungsten-based wire rod electrolytic polishing of
图9为对比例1钨基线材电解抛光后的扫描电子显微镜照片(放大倍数200倍)；Fig. 9 is the scanning electron microscope photo (200 times of magnification) after electrolytic polishing of comparative example 1 tungsten-based wire rod;
图10为对比例1钨基线材电解抛光后的原子力形貌图(Ra＝5.2μm)；Figure 10 is the atomic force topography (Ra=5.2 μm) of the tungsten-based wire material of Comparative Example 1 after electrolytic polishing;
图11为对比例2钨基线材电解抛光后的扫描电子显微镜照片(放大倍数200倍)；Fig. 11 is the scanning electron microscope photo (200 times of magnification) after electrolytic polishing of comparative example 2 tungsten-based wire rod;
图12为对比例2钨基线材电解抛光后的原子力形貌图(Ra＝2.5μm)。Fig. 12 is the atomic force topography (Ra = 2.5 μm) of the tungsten-based wire material of Comparative Example 2 after electrolytic polishing.
具体实施方式detailed description
下面用具体实施例对本发明做进一步详细说明，但本发明不仅局限于以下具体实施例。The present invention will be described in further detail below with specific examples, but the present invention is not limited to the following specific examples.
实施例1Example 1
本实施例提供一种钨基丝材或片材的电解抛光液及其电解抛光方法，钨基丝材或片材的电解抛光液由季铵碱氢氧化四甲铵、无水乙醇、2-甲基-1-己烯、硫酸钠和水混合配制而成，配制形成的电解抛光液中，季铵碱的浓度为35g/L，无水乙醇的浓度为40g/L，2-甲基-1-己烯的浓度为3g/L，硫酸钠的浓度为80g/L。This embodiment provides an electrolytic polishing solution for a tungsten-based wire or sheet and an electrolytic polishing method thereof. The electrolytic polishing solution for a tungsten-based wire or sheet is composed of quaternary ammonium alkali tetramethylammonium hydroxide, absolute ethanol, 2-formazol It is prepared by mixing base-1-hexene, sodium sulfate and water. In the prepared electrolytic polishing solution, the concentration of quaternary ammonium base is 35g/L, the concentration of absolute ethanol is 40g/L, and the concentration of 2-methyl-1 The concentration of -hexene is 3g/L, and the concentration of sodium sulfate is 80g/L.
采用本实施例的电解抛光液对表面积约30mm2的钨基线材进行电解抛光，具体过程为：将待处理的钨基线材置于电解抛光液中作为阳极，以镍棒作为阴极，阴阳两极相距30mm，控制电解抛光液的搅拌速度为15r/s，调节直流稳压电源的电流密度为2.5A/cm2，对钨基线材表面进行电解抛光，所述电解抛光的抛光时间为100s，电解抛光完成后将钨基线材用去离子水清洗，然后冷风吹干，得到表面光亮的钨基线材。The electrolytic polishing solution of this embodiment is used to electropolish the tungsten-based wire material with a surface area of about 30 mm 2 . The specific process is: the tungsten-based wire material to be treated is placed in the electrolytic polishing solution as the anode, and the nickel rod is used as the cathode. 30mm, the stirring speed of the electrolytic polishing liquid is controlled to be 15r/s, the current density of the DC stabilized power supply is adjusted to be 2.5A/cm 2 , and the surface of the tungsten-based wire is electrolytically polished, the polishing time of the electrolytic polishing is 100s, and the electrolytic polishing After the completion, the tungsten-based wire is cleaned with deionized water, and then dried with cold air to obtain a tungsten-based wire with a bright surface.
将实施例1处理前和处理后的钨基线材在扫描电子显微镜下观察，结果如图1～4，其中，图1为钨基线材电解抛光前的扫描电子显微镜照片(放大倍数150倍)，图2为钨基线材电解抛光后的扫描电子显微镜照片(放大倍数200倍)，图3为钨基线材电解抛光后的扫描电子显微镜照片(放大倍数500倍)；图4为本发明实施例1钨基线材电解抛光后的原子力形貌图，表面粗糙度Ra＝0.06μm。The tungsten-based wire rod before and after the treatment of Example 1 is observed under a scanning electron microscope, and the results are shown in Figures 1 to 4, wherein Fig. 1 is a scanning electron microscope photo (magnification 150 times) before the electrolytic polishing of the tungsten-based wire rod, Fig. 2 is the scanning electron micrograph (200 times of magnification) after electropolishing of tungsten-based wire material, and Fig. 3 is the scanning electron micrograph (500 times of magnification) of electrolytic polishing of tungsten-based wire material; Fig. 4 is
由图1可以看出，处理前的钨基线材表面粗糙、不平整，有明显的加工产生的划痕和凹槽。由图2～4可以看出，经实施例1处理后的钨基线材表面光亮平整、呈现低粗糙度Ra＝0.06μm，无加工产生的划痕和凹槽，因此，采用本实施例的电解抛光液和方法对钨基线材进行抛光，能够改善钨基线材表面平整度，使钨基线材表面光亮平整，呈现低粗糙度，无加工产生的划痕和凹槽。It can be seen from Figure 1 that the surface of the tungsten-based wire material before treatment is rough and uneven, and there are obvious scratches and grooves caused by processing. It can be seen from Figures 2 to 4 that the surface of the tungsten-based wire treated in Example 1 is bright and smooth, with a low roughness Ra=0.06 μm, and no scratches and grooves caused by processing. Therefore, the electrolytic The polishing liquid and method polish the tungsten-based wire material, which can improve the surface flatness of the tungsten-based wire material, make the surface of the tungsten-based wire material bright and flat, present low roughness, and have no scratches and grooves caused by processing.
实施例2Example 2
本实施例提供一种钨基丝材或片材的电解抛光液及其电解抛光方法，钨基丝材或片材的电解抛光液由季铵碱氢氧化四乙铵、无水乙醇、2-甲基-1-己烯、硫酸钠和水混合配制而成，配制形成的电解抛光液中，季铵碱的浓度为25g/L，无水乙醇的浓度为30g/L，2-甲基-1-己烯的浓度为5g/L，硫酸钠的浓度为75g/L。This embodiment provides an electrolytic polishing solution for a tungsten-based wire or sheet and an electrolytic polishing method thereof. The electrolytic polishing solution for a tungsten-based wire or sheet is composed of a quaternary ammonium alkali tetraethylammonium hydroxide, absolute ethanol, 2-formazol It is prepared by mixing base-1-hexene, sodium sulfate and water. In the prepared electrolytic polishing solution, the concentration of quaternary ammonium base is 25g/L, the concentration of absolute ethanol is 30g/L, and the concentration of 2-methyl-1 -The concentration of hexene is 5g/L, and the concentration of sodium sulfate is 75g/L.
采用本实施例的电解抛光液对表面积约30mm2的钨基线材进行电解抛光，具体过程为：将待处理的钨基线材置于电解抛光液中作为阳极，以镍棒作为阴极，阴阳两极相距30mm，控制电解抛光液的搅拌速度为10r/s，调节直流稳压电源的电流密度为2.0A/cm2，对钨基线材表面进行电解抛光，所述电解抛光的抛光时间为150s，电解抛光完成后将钨基线材用去离子水清洗，然后冷风吹干，得到表面光亮的钨基线材。The electrolytic polishing solution of this embodiment is used to electropolish the tungsten-based wire material with a surface area of about 30mm2 . The specific process is: the tungsten-based wire material to be treated is placed in the electrolytic polishing solution as the anode, and the nickel rod is used as the cathode. 30mm, the stirring speed of the electrolytic polishing liquid is controlled to be 10r/s, the current density of the DC stabilized power supply is adjusted to be 2.0A/cm 2 , and the surface of the tungsten-based wire is electrolytically polished, the polishing time of the electrolytic polishing is 150s, and the electrolytic polishing After the completion, the tungsten-based wire is cleaned with deionized water, and then dried with cold air to obtain a tungsten-based wire with a bright surface.
图5为实施例2钨基线材电解抛光后扫描电子显微镜照片(放大倍数500倍)，图6为实施例2钨基线材电解抛光后的原子力形貌图，表面粗糙度Ra＝0.08μm，由此可以看出，实施例2处理后的钨基线材表面光亮平整、呈现低粗糙度Ra＝0.08μm，无加工产生的划痕和凹槽，因此，采用本实施例的电解抛光液和方法对钨基线材进行抛光，能够改善钨基线材表面平整度，使钨基线材表面光亮平整，呈现低粗糙度，无加工产生的划痕和凹槽。Fig. 5 is the scanning electron microscope photograph (magnification 500 times) of
实施例3Example 3
本实施例提供一种钨基丝材或片材的电解抛光液及其电解抛光方法，钨基丝材或片材的电解抛光液由季铵碱氢氧化四丙铵、无水乙醇、2-甲基-1-己烯、硫酸钠和水混合配制而成，配制形成的电解抛光液中，季铵碱的浓度为20g/L，无水乙醇的浓度为10g/L，2-甲基-1-己烯的浓度为2g/L，硫酸钠的浓度为100g/L。This embodiment provides an electrolytic polishing solution for a tungsten-based wire or sheet and an electrolytic polishing method thereof. The electrolytic polishing solution for a tungsten-based wire or sheet is composed of a quaternary ammonium alkali tetrapropylammonium hydroxide, absolute ethanol, 2-formazol It is prepared by mixing base-1-hexene, sodium sulfate and water. In the prepared electrolytic polishing solution, the concentration of quaternary ammonium base is 20g/L, the concentration of absolute ethanol is 10g/L, and the concentration of 2-methyl-1 -The concentration of hexene is 2g/L, and the concentration of sodium sulfate is 100g/L.
采用本实施例的电解抛光液对表面积约30mm2的钨基线材进行电解抛光，具体过程为：将待处理的钨基线材置于电解抛光液中作为阳极，以镍棒作为阴极，阴阳两极相距30mm，控制电解抛光液的搅拌速度为5r/s，调节直流稳压电源的电流密度为1.5A/cm2，对钨基线材表面进行电解抛光，所述电解抛光的抛光时间为350s，电解抛光完成后将钨基线材用去离子水清洗，然后冷风吹干，得到表面光亮的钨基线材。The electrolytic polishing solution of this embodiment is used to electropolish the tungsten-based wire material with a surface area of about 30mm2 . The specific process is: the tungsten-based wire material to be treated is placed in the electrolytic polishing solution as the anode, and the nickel rod is used as the cathode. 30mm, the stirring speed of the electrolytic polishing liquid is controlled to be 5r/s, the current density of the DC stabilized power supply is adjusted to be 1.5A/cm 2 , and the surface of the tungsten-based wire is electrolytically polished, the polishing time of the electrolytic polishing is 350s, and the electrolytic polishing After the completion, the tungsten-based wire is cleaned with deionized water, and then dried with cold air to obtain a tungsten-based wire with a bright surface.
图7为实施例3钨基线材电解抛光后扫描电子显微镜照片(放大倍数500倍)，由此可以看出，实施例3处理后的钨基线材表面光亮平整、呈现低粗糙度Ra＝0.10μm，无加工产生的划痕和凹槽，因此，采用本实施例的电解抛光液和方法对钨基线材进行抛光，能够改善钨基线材表面平整度，使钨基线材表面光亮平整，呈现低粗糙度，无加工产生的划痕和凹槽。Figure 7 is a scanning electron microscope photograph (magnification 500 times) of the tungsten-based wire material in Example 3 after electrolytic polishing, from which it can be seen that the surface of the tungsten-based wire material after the treatment in Example 3 is bright and smooth, and presents a low roughness Ra=0.10 μm , without scratches and grooves produced by processing, therefore, using the electrolytic polishing solution and method of this embodiment to polish the tungsten-based wire rod can improve the surface flatness of the tungsten-based wire rod, so that the surface of the tungsten-based wire rod is bright and smooth, showing low roughness High degree, no scratches and grooves caused by processing.
实施例4Example 4
本实施例提供一种钨基丝材或片材的电解抛光液及其电解抛光方法，钨基丝材或片材的电解抛光液由季铵碱氢氧化四丁铵、无水乙醇、2-甲基-1-己烯、硫酸钠和水混合配制而成，配制形成的电解抛光液中，季铵碱的浓度为40g/L，无水乙醇的浓度为50g/L，2-甲基-1-己烯的浓度为1g/L，硫酸钠的浓度为50g/L。This embodiment provides an electrolytic polishing solution for a tungsten-based wire or sheet and an electrolytic polishing method thereof. The electrolytic polishing solution for a tungsten-based wire or sheet is composed of quaternary ammonium alkali tetrabutylammonium hydroxide, absolute ethanol, 2-formazol It is prepared by mixing base-1-hexene, sodium sulfate and water. In the prepared electrolytic polishing solution, the concentration of quaternary ammonium base is 40g/L, the concentration of absolute ethanol is 50g/L, and the concentration of 2-methyl-1 The concentration of -hexene is 1 g/L, and the concentration of sodium sulfate is 50 g/L.
采用本实施例的电解抛光液对表面积约30mm2的钨基线材进行电解抛光，具体过程为：将待处理的钨基线材置于电解抛光液中作为阳极，以镍棒作为阴极，阴阳两极相距30mm，控制电解抛光液的搅拌速度为20r/s，调节直流稳压电源的电流密度为4A/cm2，对钨基线材表面进行电解抛光，所述电解抛光的抛光时间为60s，电解抛光完成后将钨基线材用去离子水清洗，然后冷风吹干，得到表面光亮的钨基线材。The electrolytic polishing solution of this embodiment is used to electropolish the tungsten-based wire material with a surface area of about 30mm2 . The specific process is: the tungsten-based wire material to be treated is placed in the electrolytic polishing solution as the anode, and the nickel rod is used as the cathode. 30mm, control the stirring speed of the electrolytic polishing liquid to 20r/s, adjust the current density of the DC stabilized power supply to 4A/cm 2 , perform electrolytic polishing on the surface of the tungsten-based wire, the polishing time of the electrolytic polishing is 60s, and the electrolytic polishing is completed Finally, the tungsten-based wire is cleaned with deionized water, and then dried with cold air to obtain a tungsten-based wire with a bright surface.
图8为实施例4钨基线材电解抛光后扫描电子显微镜照片(放大倍数500倍)，由此可以看出，实施例3处理后的钨基线材表面光亮平整、呈现低粗糙度Ra＝0.09μm，无加工产生的划痕和凹槽，因此，采用本实施例的电解抛光液和方法对钨基线材进行抛光，能够改善钨基线材表面平整度，使钨基线材表面光亮平整，呈现低粗糙度，无加工产生的划痕和凹槽。Figure 8 is a scanning electron microscope photo (magnification: 500 times) of the tungsten-based wire material in Example 4 after electrolytic polishing. It can be seen from this that the surface of the tungsten-based wire material after the treatment in Example 3 is bright and smooth, and presents a low roughness Ra=0.09 μm , without scratches and grooves produced by processing, therefore, using the electrolytic polishing solution and method of this embodiment to polish the tungsten-based wire rod can improve the surface flatness of the tungsten-based wire rod, so that the surface of the tungsten-based wire rod is bright and smooth, showing low roughness High degree, no scratches and grooves caused by processing.
对比例1Comparative example 1
与实施例1的区别在于：钨基丝材或片材的电解抛光液不包括2-甲基-1-己烯，即钨基丝材或片材的电解抛光液由季铵碱、无水乙醇、硫酸钠和水混合配制而成。The difference with Example 1 is that the electropolishing solution of tungsten-based wire or sheet does not include 2-methyl-1-hexene, that is, the electrolytic polishing solution of tungsten-based wire or sheet consists of quaternary ammonium base, dehydrated alcohol , sodium sulfate and water mixed preparation.
其他与实施例1相同。Others are the same as in Example 1.
图9为对比例1钨基线材电解抛光后扫描电子显微镜照片(放大倍数200倍)，图10为对比例1钨基线材电解抛光后的原子力形貌图，表面粗糙度Ra＝5.2μm，由此可以看出，对比例1处理后的钨基线材表面不平整、粗糙，存在划痕和凹槽。Fig. 9 is a scanning electron microscope photograph (magnification 200 times) of the tungsten-based wire material of Comparative Example 1 after electropolishing, and Fig. 10 is an atomic force topography figure of the tungsten-based wire material of Comparative Example 1 after electrolytic polishing, and the surface roughness Ra=5.2 μm, obtained by It can be seen that the surface of the tungsten-based wire material treated in Comparative Example 1 is uneven, rough, and there are scratches and grooves.
对比例2Comparative example 2
与实施例1的区别在于：钨基丝材或片材的电解抛光液不包括硫酸钠，即钨基丝材或片材的电解抛光液由季铵碱、无水乙醇、2-甲基-1-己烯和水混合配制而成。The difference from Example 1 is that the electropolishing solution of tungsten-based wire or sheet does not include sodium sulfate, that is, the electrolytic polishing solution of tungsten-based wire or sheet consists of quaternary ammonium base, absolute ethanol, 2-methyl-1 - Prepared by mixing hexene and water.
其他与实施例1相同。Others are the same as in Example 1.
图11为对比例2钨基线材电解抛光后扫描电子显微镜照片(放大倍数200倍)，图12为对比例1钨基线材电解抛光后的原子力形貌图，表面粗糙度Ra＝2.5μm，由此可以看出，对比例2处理后的钨基线材表面不平整、粗糙，存在划痕和凹槽。Fig. 11 is a scanning electron microscope photo (magnification 200 times) after electropolishing of the tungsten-based wire material of Comparative Example 2, and Fig. 12 is an atomic force topography figure of the tungsten-based wire material of Comparative Example 1 after electrolytic polishing, and the surface roughness Ra=2.5 μm, obtained by It can be seen that the surface of the tungsten-based wire material treated in Comparative Example 2 is uneven, rough, and there are scratches and grooves.
将实施例1～5与对比例1(电解抛光液中缺少2-甲基-1-己烯)、对比例2(电解抛光液中缺少硫酸钠)比较可以看出，实施例1～5处理后的钨基线材表面光亮和平整，呈现低粗糙度，无加工产生的划痕和凹槽，而对比例1～2处理后的钨基线材表面不平整，高粗糙度，有一定划痕和凹槽，由此说明，电解抛光液中缺少2-甲基-1-己烯、硫酸钠会直接影响到抛光效果，因此，本发明的电解抛光液是通过季铵碱、无水乙醇、2-甲基-1-己烯、硫酸钠等原料共同作用，从而使得处理后的钨基线材表面光亮平整，低粗糙度，无加工产生的划痕和凹槽，抛光效果好。Comparing Examples 1 to 5 with Comparative Example 1 (lack of 2-methyl-1-hexene in the electropolishing liquid) and Comparative Example 2 (lack of sodium sulfate in the electropolishing liquid), it can be seen that the treatment of Examples 1 to 5 The surface of the tungsten-based wire after treatment is bright and smooth, showing low roughness, no scratches and grooves caused by processing, while the surface of the tungsten-based wire after treatment in Comparative Examples 1-2 is uneven, high roughness, and has certain scratches and grooves. Groove, this shows that lack of 2-methyl-1-hexene, sodium sulfate in the electrolytic polishing liquid will directly affect the polishing effect, therefore, the electrolytic polishing liquid of the present invention is passed through quaternary ammonium alkali, dehydrated alcohol, 2 -Methyl-1-hexene, sodium sulfate and other raw materials work together to make the surface of the treated tungsten-based wire material bright and smooth, with low roughness, no scratches and grooves caused by processing, and good polishing effect.
以上仅是本发明的特征实施范例，对本发明保护范围不构成任何限制。凡采用同等交换或者等效替换而形成的技术方案，均落在本发明权利保护范围之内。The above are only characteristic implementation examples of the present invention, and do not constitute any limitation to the protection scope of the present invention. All technical solutions formed by equivalent exchange or equivalent replacement fall within the protection scope of the present invention.
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