CN105821453A - Method for electro-deposition of bright chrome plating layer through low-eutectic-melting solvent - Google Patents
Method for electro-deposition of bright chrome plating layer through low-eutectic-melting solvent Download PDFInfo
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- 239000002904 solvent Substances 0.000 title claims abstract description 42
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000007747 plating Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 17
- 238000002844 melting Methods 0.000 title abstract 6
- 239000003792 electrolyte Substances 0.000 claims abstract description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract 6
- 230000005496 eutectics Effects 0.000 claims description 35
- 150000001408 amides Chemical class 0.000 claims description 11
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 11
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 10
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 3
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 claims description 3
- 235000019743 Choline chloride Nutrition 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical group [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 3
- 229960003178 choline chloride Drugs 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 235000013877 carbamide Nutrition 0.000 claims 1
- 238000011010 flushing procedure Methods 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 150000003672 ureas Chemical group 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 238000005299 abrasion Methods 0.000 abstract 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 19
- 238000000576 coating method Methods 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 229910052804 chromium Inorganic materials 0.000 description 8
- 239000011651 chromium Substances 0.000 description 8
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 6
- SHFJWMWCIHQNCP-UHFFFAOYSA-M hydron;tetrabutylazanium;sulfate Chemical compound OS([O-])(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC SHFJWMWCIHQNCP-UHFFFAOYSA-M 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002659 electrodeposit Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000010201 Exanthema Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 201000005884 exanthem Diseases 0.000 description 1
- 239000001257 hydrogen Chemical group 0.000 description 1
- 229910052739 hydrogen Chemical group 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 238000009856 non-ferrous metallurgy Methods 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 231100000075 skin burn Toxicity 0.000 description 1
- 231100000046 skin rash Toxicity 0.000 description 1
- 231100000019 skin ulcer Toxicity 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
Description
技术领域 technical field
本发明涉及一种低共熔溶剂电沉积亮铬镀层的方法，涉及表面工程和表面处理技术。 The invention relates to a method for electrodepositing a bright chrome coating with a deep eutectic solvent, and relates to surface engineering and surface treatment technologies.
背景技术 Background technique
铬镀层具有光亮性好、硬度高、抗变色能力强、耐磨性好等诸多优点，在大气条件下，能长久的保持原来的光泽，在酸、碱中具有较高的化学稳定性，在装饰性和功能性方面都令人满意。目前使用最普遍的工业工艺为六价铬镀铬，该法是在600°C的高温环境中镀铬，镀铬层会急剧氧化；镀铬的阴极电流效率极低，而在电镀过程中有氢气的析出，导致大量的酸雾，对环境和工人的健康造成危害。而且六价铬会造成黏膜及皮肤灼烧、溃疡，镀液中溢出的铬雾使镀铬工人易患皮肤斑疹，造成长期的危害。随着人们环保意识的增强，六价铬镀铬工艺改革势在必行。 Chromium plating has many advantages such as good brightness, high hardness, strong discoloration resistance, and good wear resistance. Under atmospheric conditions, it can maintain the original luster for a long time, and has high chemical stability in acid and alkali. Both decorative and functional aspects are satisfactory. The most common industrial process currently used is hexavalent chromium plating, which is chromium plating in a high-temperature environment of 600°C, and the chromium plating layer will be rapidly oxidized; the cathode current efficiency of chromium plating is extremely low, and hydrogen gas is released during the electroplating process. A large amount of acid mist is caused, which is harmful to the environment and the health of workers. Moreover, hexavalent chromium can cause mucous membranes and skin burns and ulcers, and the chromium mist overflowing from the plating solution makes chrome-plating workers susceptible to skin rashes, causing long-term harm. With the enhancement of people's awareness of environmental protection, the reform of hexavalent chromium plating process is imperative.
低共熔溶剂通常是由一定化学计量比的季铵盐和氢键给体（如酰胺、羧酸和多元醇等化合物）组合而成的低共熔混合物。低共熔溶剂具有电化学窗口宽、溶解性和导电性好、蒸汽压低以及良好的物理化学稳定性等优点，是一种新型的绿色溶剂。在电沉积金属方面，由于低共熔溶剂能够选择性的溶解金属氧化物，同时具有良好的导电性和较负的还原电势，在室温下即可电沉积得到大多数能在水溶液中得到的金属，且无副反应，因而得到的金属质量好，电流效率高。同时，由于低共熔溶剂的制备过程简单、原料价格低廉，使之成为电沉积铅粉研究的崭新电解液，在有色金属冶金技术领域具有广阔的应用前景。 Deep eutectic solvents are usually eutectic mixtures composed of certain stoichiometric ratios of quaternary ammonium salts and hydrogen bond donors (such as compounds such as amides, carboxylic acids, and polyols). Deep eutectic solvent has the advantages of wide electrochemical window, good solubility and conductivity, low vapor pressure and good physical and chemical stability, and is a new type of green solvent. In terms of electrodepositing metals, since the deep eutectic solvent can selectively dissolve metal oxides, and has good conductivity and relatively negative reduction potential, most metals that can be obtained in aqueous solutions can be obtained by electrodeposition at room temperature. , and there is no side reaction, so the obtained metal has good quality and high current efficiency. At the same time, due to the simple preparation process of the deep eutectic solvent and the low price of raw materials, it becomes a new electrolyte for the study of electrodeposited lead powder, and has broad application prospects in the field of non-ferrous metallurgy technology.
发明内容 Contents of the invention
本发明要解决的是现有镀铬技术中存在的六价铬镀铬工艺中存在的镀液挥发对人体有害，六价铬对环境不友好等技术问题，提供一种采用绿色环保的低共熔溶剂中电沉积亮铬镀层的方法，本发明通过以下技术方案实现。 The invention aims to solve technical problems such as the volatilization of the plating solution in the hexavalent chromium plating process existing in the existing chromium plating technology is harmful to the human body, and the hexavalent chromium is not friendly to the environment, and provides a green and environment-friendly deep eutectic solvent The method for electro-depositing bright chrome coatings in the present invention is realized through the following technical solutions.
一种低共熔溶剂电沉积亮铬镀层的方法，其具体步骤如下： A method for electrodepositing a bright chrome coating from a deep eutectic solvent, the specific steps of which are as follows:
（1）在惰气环境下，首先将季铵盐与酰胺按照摩尔比为（2~5）：（1~3）混合均匀后形成低共熔溶剂，然后向温度为20~80℃的低共熔溶剂中加入氧化铬，制备得到低共熔溶剂电解液； (1) In an inert gas environment, first mix the quaternary ammonium salt and amide according to the molar ratio of (2~5): (1~3) to form a deep eutectic solvent, and then transfer to a low temperature of 20~80°C adding chromium oxide to the eutectic solvent to prepare a deep eutectic solvent electrolyte;
（2）以石墨为阳极，预处理后的基体为阴极，在控制电解液温度为40~80℃、槽电压为2.0~2.6V、阳极与阴极距离为0.5~2cm的条件下，在步骤（1）制备得到的低共熔溶剂电解液中电沉积0.5~3h，将电积后的阴极基体经丙酮、蒸馏水冲洗，干燥后即能在阴极基体上得到一层亮铬。 (2) With graphite as the anode and the pretreated substrate as the cathode, under the conditions of controlling the electrolyte temperature at 40-80°C, the cell voltage at 2.0-2.6V, and the distance between the anode and the cathode at 0.5-2cm, in step ( 1) Electrodeposit in the prepared deep eutectic solvent electrolyte for 0.5~3h, wash the electrodeposited cathode substrate with acetone and distilled water, and obtain a layer of bright chrome on the cathode substrate after drying.
所述季铵盐为氯化胆碱、氯化苄基三乙基铵或硫酸氢四丁基铵。 The quaternary ammonium salt is choline chloride, benzyltriethylammonium chloride or tetrabutylammonium hydrogen sulfate.
所述酰胺为尿素、硫脲、乙酰胺或苯甲酰胺。 The amide is urea, thiourea, acetamide or benzamide.
所述氧化铬的加入量为10~80mM。 The added amount of the chromium oxide is 10-80mM.
所述基体为铜片、不锈钢或锌片。 The substrate is copper sheet, stainless steel or zinc sheet.
本发明的有益效果是：采用该方法可制备得到的亮铬镀层光亮致密平整，与基体结合能力强，耐磨性及耐腐蚀性优异，避免了六价铬及镀液的危害，环境友好。 The beneficial effects of the invention are: the bright chromium coating prepared by the method is bright, dense and smooth, has strong bonding ability with the substrate, excellent wear resistance and corrosion resistance, avoids the harm of hexavalent chromium and plating solution, and is environmentally friendly.
附图说明 Description of drawings
图1是实施例1铜基体上电沉积产物的XRD图； Fig. 1 is the XRD figure of electrodeposition product on the copper substrate of embodiment 1;
图2是实施例1铜基体上电沉积产物的SEM图。 FIG. 2 is an SEM image of the electrodeposited product on the copper substrate of Example 1. FIG.
具体实施方式 detailed description
下面结合具体实施方式，对本发明作进一步说明。 The present invention will be further described below in combination with specific embodiments.
实施例1 Example 1
该低共熔溶剂电沉积亮铬镀层的方法，其具体步骤如下： The method of this deep eutectic solvent electrodeposition bright chrome coating, its concrete steps are as follows:
（1）在惰气环境下，首先将季铵盐与酰胺按照摩尔比为2：3混合均匀后形成低共熔溶剂，然后向温度为20℃的低共熔溶剂中加入氧化铬，制备得到低共熔溶剂电解液，其中季铵盐为氯化胆碱，酰胺为尿素，氧化铬的加入量为10mM； (1) In an inert gas environment, first mix the quaternary ammonium salt and amide evenly at a molar ratio of 2:3 to form a deep eutectic solvent, then add chromium oxide to the deep eutectic solvent at a temperature of 20°C to prepare Deep eutectic solvent electrolyte, wherein the quaternary ammonium salt is choline chloride, the amide is urea, and the addition of chromium oxide is 10mM;
（2）以石墨为阳极，预处理后的基体为阴极，在控制电解液温度为40℃、槽电压为2.0V、阳极与阴极距离为0.5cm的条件下，在步骤（1）制备得到的低共熔溶剂电解液中电沉积0.5h，将电积后的阴极基体经丙酮、蒸馏水冲洗，干燥后即能在阴极基体上得到亮铬镀层，其中基体为铜片，电沉积产物的XRD图和SEM图分别如图1和2所示。 (2) With graphite as the anode and the pretreated substrate as the cathode, under the conditions of controlling the electrolyte temperature to 40°C, the cell voltage to 2.0V, and the distance between the anode and the cathode to be 0.5cm, the prepared in step (1) Electrodeposition in the deep eutectic solvent electrolyte for 0.5h, rinse the electrodeposited cathode substrate with acetone and distilled water, and dry it to obtain a bright chromium coating on the cathode substrate, in which the substrate is copper sheet, the XRD pattern of the electrodeposited product and SEM images are shown in Figures 1 and 2, respectively.
实施例2 Example 2
该低共熔溶剂电沉积亮铬镀层的方法，其具体步骤如下： The method of this deep eutectic solvent electrodeposition bright chrome coating, its concrete steps are as follows:
（1）在惰气环境下，首先将季铵盐与酰胺按照摩尔比为5：1混合均匀后形成低共熔溶剂，然后向温度为50℃的低共熔溶剂中加入氧化铬，制备得到低共熔溶剂电解液，其中季铵盐为氯化苄基三乙基铵，酰胺为硫脲，氧化铬的加入量为45mM； (1) In an inert gas environment, first mix the quaternary ammonium salt and amide evenly at a molar ratio of 5:1 to form a deep eutectic solvent, then add chromium oxide to the deep eutectic solvent at a temperature of 50°C to prepare Deep eutectic solvent electrolyte, wherein the quaternary ammonium salt is benzyltriethylammonium chloride, the amide is thiourea, and the addition of chromium oxide is 45mM;
（2）以石墨为阳极，预处理后的基体为阴极，在控制电解液温度为60℃、槽电压为2.3V、阳极与阴极距离为1cm的条件下，在步骤（1）制备得到的低共熔溶剂电解液中电沉积2h，将电积后的阴极基体经丙酮、蒸馏水冲洗，干燥后即能在阴极基体上得到亮铬镀层，其中基体为不锈钢。 (2) With graphite as the anode and the pretreated substrate as the cathode, under the conditions of controlling the electrolyte temperature at 60°C, the cell voltage at 2.3V, and the distance between the anode and the cathode at 1cm, the low Electrodeposit in the eutectic solvent electrolyte for 2 hours, rinse the electrodeposited cathode substrate with acetone and distilled water, and obtain a bright chrome coating on the cathode substrate after drying, wherein the substrate is stainless steel.
实施例3 Example 3
该低共熔溶剂电沉积亮铬镀层的方法，其具体步骤如下： The method of this deep eutectic solvent electrodeposition bright chrome coating, its concrete steps are as follows:
（1）在惰气环境下，首先将季铵盐与酰胺按照摩尔比为3：2混合均匀后形成低共熔溶剂，然后向温度为80℃的低共熔溶剂中加入氧化铬，制备得到低共熔溶剂电解液，其中季铵盐为硫酸氢四丁基铵，酰胺为乙酰胺，氧化铬的加入量为80mM； (1) In an inert gas environment, firstly mix the quaternary ammonium salt and amide evenly at a molar ratio of 3:2 to form a deep eutectic solvent, then add chromium oxide to the deep eutectic solvent at a temperature of 80°C to prepare Deep eutectic solvent electrolyte, wherein the quaternary ammonium salt is tetrabutylammonium hydrogen sulfate, the amide is acetamide, and the addition of chromium oxide is 80mM;
（2）以石墨为阳极，预处理后的基体为阴极，在控制电解液温度为80℃、槽电压为2.6V、阳极与阴极距离为2cm的条件下，在步骤（1）制备得到的低共熔溶剂电解液中电沉积3h，将电积后的阴极基体经丙酮、蒸馏水冲洗，干燥后即能在阴极基体上得到亮铬镀层，其中基体为锌。 (2) Using graphite as the anode and the pretreated substrate as the cathode, under the conditions of controlling the electrolyte temperature at 80°C, the cell voltage at 2.6V, and the distance between the anode and the cathode at 2cm, the low Electrodeposit in the eutectic solvent electrolyte for 3 hours, rinse the electrodeposited cathode substrate with acetone and distilled water, and obtain a bright chrome coating on the cathode substrate after drying, wherein the substrate is zinc.
Claims (5)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106567110A (en) * | 2016-11-07 | 2017-04-19 | 昆明理工大学 | Method of electro-deposition of chromium-manganese alloy coating through deep-eutectic solvents |
| CN108070887A (en) * | 2016-11-15 | 2018-05-25 | 财团法人工业技术研究院 | Electroplating method and system thereof |
| CN108842172A (en) * | 2018-06-15 | 2018-11-20 | 昆明理工大学 | A kind of method that eutectic solvent electro-deposition prepares stainless steel coating |
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| CN108842172A (en) * | 2018-06-15 | 2018-11-20 | 昆明理工大学 | A kind of method that eutectic solvent electro-deposition prepares stainless steel coating |
| CN109338406A (en) * | 2018-12-05 | 2019-02-15 | 昆明理工大学 | Method and device for electrolytic reduction of metal sulfides |
| CN113652735A (en) * | 2021-08-26 | 2021-11-16 | 安徽工业大学 | Zr-based metal glass and preparation method and application thereof |
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