WO2018068184A1 - 一种 TiNC 膜的退镀液及退镀工艺 - Google Patents

一种 TiNC 膜的退镀液及退镀工艺 Download PDF

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Publication number
WO2018068184A1
WO2018068184A1 PCT/CN2016/101697 CN2016101697W WO2018068184A1 WO 2018068184 A1 WO2018068184 A1 WO 2018068184A1 CN 2016101697 W CN2016101697 W CN 2016101697W WO 2018068184 A1 WO2018068184 A1 WO 2018068184A1
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deplating
solution
deplating solution
workpiece
tinc
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PCT/CN2016/101697
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English (en)
French (fr)
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向雄志
胡远立
程淼
黄琪
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深圳大学
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Priority to PCT/CN2016/101697 priority Critical patent/WO2018068184A1/zh
Publication of WO2018068184A1 publication Critical patent/WO2018068184A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
    • C23G1/26—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions using inhibitors

Definitions

  • the invention belongs to the technical field of coating treatment, and in particular relates to a deplating solution and a deplating process of a TiNC film.
  • Unqualified coatings are produced during the coating process and need to be recycled. This requires the plating of the substrate surface to be completely removed, and the deplating solution is generally suitable for the removal of the coating on the surface of the substrate.
  • the deplating solution contains a substance having poor oxidizing property such as nitric acid, cyanide or nitro compound sulfuric acid, and having serious pollution.
  • nitric acid cyanide or nitro compound sulfuric acid
  • Part of the copper will react with nitric acid, to produce polluting gases NO X, not only the greater harm to the human body, and there is a certain danger to equipment and plant.
  • the technical problem to be solved by the present invention is to provide a deplating solution and a deplating process for a TiNC film, which are intended to perform deplating on a TiNC film, and the deplating is thorough, efficient, and environmentally friendly.
  • the present invention is achieved by a deplating solution of a TiNC film, the solvent of the deplating solution is deionized water or distilled water, and the components of the solute of the deplating solution and the content thereof include:
  • Antiseptic complexing agent 3-35g/L 3-35g/L
  • ammonium chloride is analytically pure ammonium chloride.
  • the surfactant includes at least one of sodium alkyl polyoxyethylene ether sulfate, sodium dodecylbenzenesulfonate, and sodium alkylsulfonate.
  • the anticorrosive complexing agent comprises disodium edetate and sodium citrate.
  • the corrosion inhibitor comprises at least one of hexamethylenetetramine and lemon triammonium.
  • the substrate of the TiNC film is a titanium alloy or a stainless steel substrate.
  • each component of the solute of the deplating solution and its content include:
  • the invention also provides a deplating process of the deplating solution of the TiNC film, comprising:
  • Cleaning step cleaning the workpiece with the TiNC film on the surface
  • Deplating step the workpiece processed by the cleaning step is placed in the deplating solution to perform deplating treatment; the speed of the deplating treatment is 0.4 um/min;
  • the workpiece treated by the deplating solution is washed twice with distilled water or deionized water, and the washing time is 20-50 seconds each time; drying treatment.
  • the cleaning step includes
  • Water washing step the workpiece coated with the TiNC film on the surface is rinsed in room temperature water for 25-45 seconds;
  • Organic solvent ultrasonic cleaning step The workpiece treated by the water washing step is ultrasonically washed in an absolute ethanol or acetone solution for 10-15 minutes.
  • drying treatment is vacuum drying at 70-90 ° C for 20-30 minutes.
  • the present invention has the beneficial effects that the deplating solution of the TiNC film provided by the embodiment of the invention has no toxic and side effects.
  • the workpiece is subjected to deplating, not only the TiNC film on the surface of the workpiece can be completely removed, but also the substrate of the workpiece is not damaged.
  • sodium chloride and cesium chloride are chemically reacted with the TiNC film to remove them.
  • the surfactant, the anticorrosive complexing agent and the corrosion inhibitor act to protect the substrate of the workpiece, and further control the speed of the chemical reaction of the TiNC film by controlling sodium chloride and barium chloride, thereby controlling the deplating The speed of processing.
  • the processing degree and treatment of the TiNC film are performed when the deplating solution is subjected to deplating treatment on the TiNC film-plated workpiece by rationally adjusting the components of the solute of the deplating solution and the content thereof.
  • the speed is suitable, so as to obtain the corresponding technical effect.
  • the embodiment of the present invention provides a deplating solution for a TiNC film
  • the solvent of the deplating solution is deionized water or distilled water
  • the components of the solute of the deplating solution and the content thereof include:
  • Antiseptic complexing agent 3-35g/L 3-35g/L
  • the deplating solution of the TiNC film provided by the embodiment of the invention has no toxic and side effects.
  • the workpiece is subjected to deplating, not only the TiNC film on the surface of the workpiece can be completely removed, but also the substrate of the workpiece is not damaged.
  • sodium chloride and cesium chloride are chemically reacted with the TiNC film to remove them.
  • the surfactant, the anticorrosive complexing agent and the corrosion inhibitor act to protect the substrate of the workpiece, and further control the speed of the chemical reaction of the TiNC film by controlling sodium chloride and barium chloride, thereby controlling the deplating The speed of processing.
  • the processing degree and treatment of the TiNC film are performed when the deplating solution is subjected to deplating treatment on the TiNC film-plated workpiece by rationally adjusting the components of the solute of the deplating solution and the content thereof.
  • the speed is suitable, so as to obtain the corresponding technical effect.
  • the ammonium chloride is analytically pure ammonium chloride.
  • the surfactant includes at least one of sodium alkyl polyoxyethylene ether sulfate, sodium dodecylbenzenesulfonate, and sodium alkylsulfonate.
  • the antiseptic complexing agent comprises disodium edetate and sodium citrate.
  • the corrosion inhibitor includes at least one of hexamethylenetetramine and lemon triammonium.
  • the substrate of the TiNC film is a titanium alloy or a stainless steel substrate.
  • the base material is effectively protected by the corrosion inhibitor containing the rare earth element in the deplating solution, and the titanium alloy or the stainless steel substrate is not corroded at all.
  • the components of the solute of the stripping solution and their contents include:
  • the embodiment of the invention further provides a deplating process of the deplating solution of the TiNC film, comprising:
  • Cleaning step cleaning the workpiece with the TiNC film on the surface
  • Deplating step the workpiece processed by the cleaning step is placed in the deplating solution to perform deplating treatment; the speed of the deplating treatment is 0.4 um/min;
  • the workpiece treated by the deplating solution is washed twice with distilled water or deionized water, and the washing time is 20-50 seconds each time; drying treatment.
  • the deplating process of the deplating solution of the TiNC film provided by the embodiment of the invention is simple and easy to operate, high efficiency, and free from pollution.
  • the deplating solution of the TiNC film provided by the embodiment of the present invention is subjected to deplating treatment on the surface of the workpiece coated with the TiNC film, the TiNC film on the surface of the workpiece can be completely removed without causing damage to the substrate of the workpiece.
  • the cleaning step includes:
  • Water washing step the workpiece coated with the TiNC film on the surface is rinsed in room temperature water for 25-45 seconds;
  • Organic solvent ultrasonic cleaning step The workpiece treated by the water washing step is ultrasonically washed in an absolute ethanol or acetone solution for 10-15 minutes.
  • the ultrasonic frequency in the ultrasonic cleaning is 20 to 40 kHz.
  • the drying treatment is vacuum drying at 70 to 90 ° C for 20 to 30 minutes.
  • the deplating process of the deplating solution of the TiNC film provided by the embodiment of the present invention, by controlling various parameters in the deplating process, the deplating process has achieved the corresponding effect, and the TiNC film on the surface of the workpiece can be completely removed, and Damage to the substrate of the workpiece.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

适用于镀膜处理技术领域，提供了一种TiNC膜的退镀液，所述退镀液的溶剂为去离子水或蒸馏水，所述退镀液的溶质的各组分及其含量包括：氯化铵1-6g/L，氯化铈0.01-0.5g/L，表面活性剂5-30g/L，防腐络合剂3-35g/L，缓蚀剂1-30g/L。还提供了一种TiNC膜的退镀液的退镀工艺。提供的TiNC膜的退镀液，无毒副作用。在对工件进行退镀处理时，不仅可将工件表面的TiNC膜彻底去除，又不会对工件的基底造成损害。

Description

一种 TiNC 膜的退镀液及退镀工艺 技术领域
本发明属于镀膜处理技术领域，尤其涉及一种 TiNC 膜的退镀液及退镀工艺。
背景技术
镀膜过程中会产生不合格的镀层，需要回收利用，这需要将基体表面的镀层彻底退除，而退镀液通常适用于基体表面镀层的退除。传统的退镀工艺中退镀液含有用硝酸、氰化物、硝基化合物硫酸等氧化性强安全性差，污染性严重的物质。此外，在退镀过程中极易对基体本身造成腐蚀，并且产生有毒或者有害气体污染环境。而一部分的铜会与硝酸反应，产生污染性的NOX气体，不仅对人体有较大危害，且对设备及厂房均有一定的危害。
技术问题
本发明所要解决的技术问题在于提供一种TiNC膜的退镀液及退镀工艺，旨在针对TiNC膜进行退镀，且退镀彻底、高效、对环境无污染。
技术解决方案
本发明是这样实现的，一种TiNC膜的退镀液，所述退镀液的溶剂为去离子水或蒸馏水，所述退镀液的溶质的各组分及其含量包括：
氯化铵 1-6g/L，
氯化铈 0.01-0.5g/L，
表面活性剂 5-30g/L，
防腐络合剂 3-35g/L，
缓蚀剂 1-30g/L。
进一步地，所述氯化铵为分析纯氯化铵。
进一步地，所述表面活性剂包括烷基聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠及烷基磺酸钠中的至少一种。
进一步地，所述防腐络合剂包括乙二胺四乙酸二钠及柠檬酸钠。
进一步地，所述缓蚀剂包括六次甲基四胺、柠檬三铵中的至少一种。
进一步地，所述TiNC膜的基底为钛合金或不锈钢基底。
进一步地，所述退镀液的溶质的各组分及其含量包括：
分析纯氯化铵 3g/L，
氯化铈 0.3g/L，
十二烷基苯磺酸钠 15g/L，
乙二胺四乙酸二钠 16g/L，
柠檬酸钠 2g/L，
六次甲基四胺 15g/L。
本发明还提供了一种TiNC膜的退镀液的退镀工艺，包括：
清洗步骤：将表面镀有TiNC膜的工件进行清洗；
退镀步骤：将经所述清洗步骤处理后的工件放入退镀液中进行退镀处理；所述退镀处理的速度为0.4um/min；
二次清洗：将经所述退镀液处理后的工件用蒸馏水或去离子水冲洗两次，每次水洗时间为20-50秒；干燥处理。
进一步地，所述清洗步骤包括
水洗步骤：将表面镀有TiNC膜的工件放置室温水中漂洗25-45秒；
有机溶剂超声清洗步骤：将经所述水洗步骤处理过的工件放入无水乙醇或者丙酮溶液中超声清洗10-15分钟。
进一步地，所述干燥处理为在70-90℃下真空干燥20-30分钟。
本发明与现有技术相比，有益效果在于：本发明实施例提供的TiNC膜的退镀液，无毒副作用。在对工件进行退镀处理时，不仅可将工件表面的TiNC膜彻底去除，又不会对工件的基底造成损害。在进行退镀处理时，氯化钠和氯化铈会与所述TiNC膜进行化学反应，从而将其去除。所述表面活性剂、防腐络合剂及缓蚀剂起到保护工件的基底的作用，此外还可以控制氯化钠和氯化铈对所述TiNC膜进行化学方应的速度，从而控制退镀处理的速度。
 有益效果
本发明实施例通过合理调配退镀液的溶质的各组分及其含量，使所述退镀液对所述镀TiNC膜的工件进行退镀处理时，对所述TiNC膜的处理程度及处理速度均较适宜，从而获得相应的技术效果。
 本发明的实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明实施例提供了一种TiNC膜的退镀液，所述退镀液的溶剂为去离子水或蒸馏水，所述退镀液的溶质的各组分及其含量包括：
氯化铵 1-6g/L，
氯化铈 0.01-0.5g/L，
表面活性剂 5-30g/L，
防腐络合剂 3-35g/L，
缓蚀剂 1-30g/L。
本发明实施例提供的TiNC膜的退镀液，无毒副作用。在对工件进行退镀处理时，不仅可将工件表面的TiNC膜彻底去除，又不会对工件的基底造成损害。在进行退镀处理时，氯化钠和氯化铈会与所述TiNC膜进行化学方应，从而将其去除。所述表面活性剂、防腐络合剂及缓蚀剂起到保护工件的基底的作用，此外还可以控制氯化钠和氯化铈对所述TiNC膜进行化学方应的速度，从而控制退镀处理的速度。
本发明实施例通过合理调配退镀液的溶质的各组分及其含量，使所述退镀液对所述镀TiNC膜的工件进行退镀处理时，对所述TiNC膜的处理程度及处理速度均较适宜，从而获得相应的技术效果。
具体地，所述氯化铵为分析纯氯化铵。所述表面活性剂包括烷基聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠及烷基磺酸钠中的至少一种。所述防腐络合剂包括乙二胺四乙酸二钠及柠檬酸钠。所述缓蚀剂包括六次甲基四胺、柠檬三铵中的至少一种。所述TiNC膜的基底为钛合金或不锈钢基底。
在本发明实施例提供的TiNC膜的退镀液中，由于退镀液中含有稀土元素的缓蚀剂从而有效的保护了基底材料，对钛合金或不锈钢基底完全没有腐蚀。
作为优选，所述退镀液的溶质的各组分及其含量包括：
分析纯氯化铵 3g/L，
氯化铈 0.3g/L，
十二烷基苯磺酸钠 15g/L，
乙二胺四乙酸二钠 16g/L，
柠檬酸钠 2g/L，
六次甲基四胺 15g/L。
本发明实施例还提供了一种TiNC膜的退镀液的退镀工艺，包括：
清洗步骤：将表面镀有TiNC膜的工件进行清洗；
退镀步骤：将经所述清洗步骤处理后的工件放入退镀液中进行退镀处理；所述退镀处理的速度为0.4um/min；
二次清洗：将经所述退镀液处理后的工件用蒸馏水或去离子水冲洗两次，每次水洗时间为20-50秒；干燥处理。
在本发明实施例提供的TiNC膜的退镀液的退镀工艺，简单易操作，高效率，且无污染。采用本发明实施例提供的TiNC膜的退镀液对表面镀有TiNC膜的工件进行退镀处理时，不仅可将工件表面的TiNC膜彻底去除，又不会对工件的基底造成损害。
具体地，所述清洗步骤包括：
水洗步骤：将表面镀有TiNC膜的工件放置室温水中漂洗25-45秒；
有机溶剂超声清洗步骤：将经所述水洗步骤处理过的工件放入无水乙醇或者丙酮溶液中超声清洗10-15分钟。
具体地，所述超声清洗中超声频率为20～40kHz。
具体地，所述干燥处理为在70-90℃下真空干燥20-30分钟。
在本发明实施例提供的TiNC膜的退镀液的退镀工艺，通过控制退镀过程中各参数，使退镀处理取得了相应的效果，不仅可将工件表面的TiNC膜彻底去除，又不会对工件的基底造成损害。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种TiNC膜的退镀液，其特征在于，所述退镀液的溶剂为去离子水或蒸馏水，所述退镀液的溶质的各组分及其含量包括：
    氯化铵 1-6g/L，
    氯化铈 0.01-0.5g/L，
    表面活性剂 5-30g/L，
    防腐络合剂 3-35g/L，
    缓蚀剂 1-30g/L。
  2. 如权利要求1所述的退镀液，其特征在于，所述氯化铵为分析纯氯化铵。
  3. 如权利要求1所述的退镀液，其特征在于，所述表面活性剂包括烷基聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠及烷基磺酸钠中的至少一种。
  4. 如权利要求1所述的退镀液，其特征在于，所述防腐络合剂包括乙二胺四乙酸二钠及柠檬酸钠。
  5. 如权利要求1所述的退镀液，其特征在于，所述缓蚀剂包括六次甲基四胺、柠檬三铵中的至少一种。
  6. 如权利要求1所述的退镀液，其特征在于，所述TiNC膜的基底为钛合金或不锈钢基底。
  7. 如权利要求1所述的退镀液，其特征在于，所述退镀液的溶质的各组分及其含量包括：
    分析纯氯化铵 3g/L，
    氯化铈 0.3g/L，
    十二烷基苯磺酸钠 15g/L，
    乙二胺四乙酸二钠 16g/L，
    柠檬酸钠 2g/L，
    六次甲基四胺 15g/L。
  8. 一种TiNC膜的退镀液的退镀工艺，其特征在于，包括：
    清洗步骤：将表面镀有TiNC膜的工件进行清洗；
    退镀步骤：将经所述清洗步骤处理后的工件放入退镀液中进行退镀处理；所述退镀处理的速度为0.4um/min；
    二次清洗：将经所述退镀液处理后的工件用蒸馏水或去离子水冲洗两次，每次水洗时间为20-50秒；干燥处理。
  9. 如权利要求8所述的退镀工艺，其特征在于，所述清洗步骤包括
    水洗步骤：将表面镀有TiNC膜的工件放置室温水中漂洗25-45秒；
    有机溶剂超声清洗步骤：将经所述水洗步骤处理过的工件放入无水乙醇或者丙酮溶液中超声清洗10-15分钟。
  10. 如权利要求8所述的退镀工艺，其特征在于，所述干燥处理为在70-90℃下真空干燥20-30分钟。
PCT/CN2016/101697 2016-10-10 2016-10-10 一种 TiNC 膜的退镀液及退镀工艺 WO2018068184A1 (zh)

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CN112875294A (zh) * 2021-01-06 2021-06-01 甬矽电子(宁波)股份有限公司 自动退镀系统

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