CN108642479A - 高效高活性的电极涂层的制备方法 - Google Patents

高效高活性的电极涂层的制备方法 Download PDF

Info

Publication number
CN108642479A
CN108642479A CN201810529298.3A CN201810529298A CN108642479A CN 108642479 A CN108642479 A CN 108642479A CN 201810529298 A CN201810529298 A CN 201810529298A CN 108642479 A CN108642479 A CN 108642479A
Authority
CN
China
Prior art keywords
coating
preparation
high activity
titanium
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810529298.3A
Other languages
English (en)
Inventor
程亚莲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangyin Anno Electrode Co Ltd
Original Assignee
Jiangyin Anno Electrode Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangyin Anno Electrode Co Ltd filed Critical Jiangyin Anno Electrode Co Ltd
Priority to CN201810529298.3A priority Critical patent/CN108642479A/zh
Publication of CN108642479A publication Critical patent/CN108642479A/zh
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1291—Process of deposition of the inorganic material by heating of the substrate
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10—Electrodes, e.g. composition, counter electrode
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C25D7/0642—Anodes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Ceramic Engineering (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

本发明公开了一种高效高活性的电极涂层的制备方法，包括以下步骤：（1）用四氯化钛、五氯化钽、盐酸和醇液制备钛钽涂液；（2）用氯铱酸、五氯化钽、四氯化锡、盐酸和醇液制备铱钽涂液；（3）以钛板为基体，在钛板上涂覆4‑5次钛钽涂液，并在每次涂覆结束之后进行烧结；（4）在步骤（3）制备的基板上涂覆15‑25次铱钽涂液，并在每次涂覆结束之后进行烧结；（5）冷却至室温后进行检测。通过本发明制备的涂层不但高活性、高效节能，而且涂层均匀孔隙率低，不易开裂，使用寿命长。

Description

高效高活性的电极涂层的制备方法
技术领域
本发明涉及电极领域，尤其是涉及一种高效高活性的电极涂层的制备方法，主要用于电解铜箔中。
背景技术
以金属钛或者其他阀型金属为基材，涂覆贵金属溶液为涂层的电极，在多种电化学领域诸如电解、电镀、有机电合成等行业大量被应用是众所周知的。而随着电化学工业的发展，在电子工业的电解铜箔领域，阳极电流密度明显加大。在这种环境下，加上工作温度又高，涂有常规贵金属溶液的电极表面所形成的涂层不规则，容易开裂，寿命也会明显下降。
发明内容
本发明为了解决目前电极表面涂层不规则、易开裂、寿命短的问题，为此提供了一种高效高活性的电极涂层的制备方法，包括以下步骤：
（1）用四氯化钛、五氯化钽、盐酸和醇液制备钛钽涂液；
（2）用氯铱酸、五氯化钽、四氯化锡、盐酸和醇液制备铱钽涂液；
（3）以钛板为基体，在钛板上涂覆4-5次钛钽涂液，并在每次涂覆结束之后进行烧结；（4）在步骤（3）制备的基板上涂覆15-25次铱钽涂液，并在每次涂覆结束之后进行烧结； （5）冷却至室温后进行检测。
本发明高效高活性的电极涂层的制备方法，步骤（1）中四氯化钛、五氯化钽、盐酸、醇液的重量分数分别为2%-3%、18%-22%、5%-10%、5%-10%，其余为去离子水，上述各组分在室温下搅拌制备成钛钽涂液。
本发明高效高活性的电极涂层的制备方法，钛钽涂液在涂覆时，每次每1m2涂12-15ml，每次涂覆结束之后在510-530℃烧结并冷却至室温。
本发明高效高活性的电极涂层的制备方法，步骤（2）中氯铱酸、五氯化钽、四氯化锡、盐酸的重量分数分别为12%-15%、35%-45%、0.5%-2%、10%-15%、5%-10%，其余为去离子水，上述各组分在60-70℃搅拌均匀，再保温1h，冷却至室温后加入醇液搅拌制成铱钽涂液。
本发明高效高活性的电极涂层的制备方法，铱钽涂液在涂覆时，每次每1m2涂15-20ml，每次涂覆结束之后在510-530℃烧结并冷却至室温。
本发明高效高活性的电极涂层的制备方法，醇液包括丙醇、正丁醇、乙二醇中的一种或多种。
本发明高效高活性的电极涂层的制备方法，盐酸浓度为10%。
本发明的有益效果是：
通过本发明制备的涂层不但高活性、高效节能，而且涂层均匀孔隙率低，不易开裂，使用寿命长。
具体实施方式
现在对本发明作进一步详细的说明。
一种高效高活性的电极涂层的制备方法，包括以下步骤：
（1）用四氯化钛、五氯化钽、盐酸和醇液制备钛钽涂液；
（2）用氯铱酸、五氯化钽、四氯化锡、盐酸和醇液制备铱钽涂液；
（3）以5-6mm厚的钛板为基体，在钛板上涂覆4-5次钛钽涂液，并在每次涂覆结束之后进行烧结；
（4）在步骤（3）制备的基板上涂覆15-25次铱钽涂液，并在每次涂覆结束之后进行烧结；（5）冷却至室温后进行检测。
步骤（1）中四氯化钛、五氯化钽、盐酸、醇液的重量分数分别为2%-3%、18%-22%、5%-10%、5%-10%，其余为去离子水，上述各组分在室温下搅拌制备成钛钽涂液。
步骤（2）中氯铱酸、五氯化钽、四氯化锡、盐酸的重量分数分别为12%-15%、35%-45%、0.5%-2%、10%-15%、5%-10%，其余为去离子水，上述各组分在60-70℃搅拌均匀，在保温1h，冷却至室温后加入醇液搅拌制成铱钽涂液。
上述醇液包括丙醇、正丁醇、乙二醇中的一种或多种，盐酸浓度为10%。
钛钽涂液在涂覆时，每次每1m2涂12-15ml，每次涂覆结束之后在510-530℃烧结并冷却至室温，在最后一次冷却之后涂覆铱钽涂液，每次每1m2涂15-20ml，每次涂覆结束之后在510-530℃烧结并冷却至室温，上述两种涂液的具体涂覆次数根据使用电流密度和寿命要求来设置。
该电极涂层在制备好之后，经检测不但高活性、高效节能，而且涂层均匀孔隙率低，不易开裂，使用寿命长。尤其是在钛钽涂液涂覆5次，铱钽涂液涂覆20次，形成6-8μm厚涂层时，效果最佳。
上述依据本发明为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。

Claims (7)

1.一种高效高活性的电极涂层的制备方法，其特征在于，包括以下步骤：
（1）用四氯化钛、五氯化钽、盐酸和醇液制备钛钽涂液；
（2）用氯铱酸、五氯化钽、四氯化锡、盐酸和醇液制备铱钽涂液；
（3）以钛板为基体，在钛板上涂覆4-5次钛钽涂液，并在每次涂覆结束之后进行烧结；（4）在步骤（3）制备的基板上涂覆15-18次铱钽涂液，并在每次涂覆结束之后进行烧结； （5）冷却后进行检测。
2.根据权利要求1所述的高效高活性的电极涂层的制备方法，其特征在于，步骤（1）中四氯化钛、五氯化钽、盐酸、醇液的重量分数分别为2%-3%、18%-22%、5%-10%、5%-10%，其余为去离子水，上述各组分在室温下搅拌制备成钛钽涂液。
3.根据权利要求2所述的高效高活性的电极涂层的制备方法，其特征在于，钛钽涂液在涂覆时，每次每1m2涂12-15ml，每次涂覆结束之后在510-530℃烧结并冷却至室温。
4.根据权利要求1所述的高效高活性的电极涂层的制备方法，其特征在于，步骤（2）中氯铱酸、五氯化钽、四氯化锡、盐酸的重量分数分别为12%-15%、35%-45%、0.5%-2%、10%-15%、5%-10%，其余为去离子水，上述各组分在60-70℃搅拌均匀，再保温1h，冷却至室温后加入醇液搅拌制成铱钽涂液。
5.根据权利要求4所述的高效高活性的电极涂层的制备方法，其特征在于，铱钽涂液在涂覆时，每次每1m2涂15-20ml，每次涂覆结束之后在510-530℃烧结并冷却至室温。
6.根据权利要求1所述的高效高活性的电极涂层的制备方法，其特征在于，醇液包括丙醇、正丁醇、乙二醇中的一种或多种。
7.根据权利要求1所述的高效高活性的电极涂层的制备方法，其特征在于，盐酸浓度为10%。
CN201810529298.3A 2018-05-29 2018-05-29 高效高活性的电极涂层的制备方法 Pending CN108642479A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810529298.3A CN108642479A (zh) 2018-05-29 2018-05-29 高效高活性的电极涂层的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810529298.3A CN108642479A (zh) 2018-05-29 2018-05-29 高效高活性的电极涂层的制备方法

Publications (1)

Publication Number Publication Date
CN108642479A true CN108642479A (zh) 2018-10-12

Family

ID=63758398

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810529298.3A Pending CN108642479A (zh) 2018-05-29 2018-05-29 高效高活性的电极涂层的制备方法

Country Status (1)

Country Link
CN (1) CN108642479A (zh)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109440158A (zh) * 2018-12-28 2019-03-08 南京时恒电子科技有限公司 一种Cu-Ti-Co复合电极及其制备方法
CN109706513A (zh) * 2019-03-12 2019-05-03 江阴安诺电极有限公司 涂层阳极板的制备方法
CN109763149A (zh) * 2019-03-12 2019-05-17 江阴安诺电极有限公司 铱钽涂层阳极板
CN109868464A (zh) * 2019-03-11 2019-06-11 江阴安诺电极有限公司 具有贵金属涂层的阳极板
CN110983387A (zh) * 2019-12-26 2020-04-10 西安泰金工业电化学技术有限公司 一种提高电解铜箔用阳极板寿命的方法
CN111926310A (zh) * 2020-08-04 2020-11-13 淮南师范学院 高效高活性的电极涂层的制备方法
CN111926311A (zh) * 2020-08-06 2020-11-13 淮南师范学院 复合电极及其制备方法

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4481097A (en) * 1983-01-31 1984-11-06 Permelec Electrode Ltd Durable electrode for electrolysis
KR20070107411A (ko) * 2006-05-03 2007-11-07 주식회사 코일렉트로드 규칙적인 세공구조를 가진 메트릭스형 촉매층을 갖는전기분해용 전극 및 이의 제조방법
CN101479409A (zh) * 2006-06-30 2009-07-08 大曹株式会社 金属线材电镀用不溶性阳极和采用它的金属线材电镀方法
CN101565834A (zh) * 2009-05-26 2009-10-28 北京科技大学 一种钛电极基体表面预处理的方法
CN102174704A (zh) * 2011-02-20 2011-09-07 中国船舶重工集团公司第七二五研究所 一种含钽中间层金属氧化物电极的制备方法
CN102449200A (zh) * 2009-07-28 2012-05-09 德诺拉工业有限公司 用于工业电解工艺中析氧的电极
CN106521404A (zh) * 2016-11-02 2017-03-22 苏州云瑞环境科技有限公司 一种一次氧化制造钛阳极工艺
CN107699912A (zh) * 2017-09-01 2018-02-16 广东省稀有金属研究所 一种涂层电极的涂层溶液及其涂层电极的制备方法
CN107779847A (zh) * 2017-09-25 2018-03-09 上海同臣环保有限公司 一种涂层钛阳极及其喷涂热解制备方法

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4481097A (en) * 1983-01-31 1984-11-06 Permelec Electrode Ltd Durable electrode for electrolysis
KR20070107411A (ko) * 2006-05-03 2007-11-07 주식회사 코일렉트로드 규칙적인 세공구조를 가진 메트릭스형 촉매층을 갖는전기분해용 전극 및 이의 제조방법
CN101479409A (zh) * 2006-06-30 2009-07-08 大曹株式会社 金属线材电镀用不溶性阳极和采用它的金属线材电镀方法
CN101565834A (zh) * 2009-05-26 2009-10-28 北京科技大学 一种钛电极基体表面预处理的方法
CN102449200A (zh) * 2009-07-28 2012-05-09 德诺拉工业有限公司 用于工业电解工艺中析氧的电极
CN102174704A (zh) * 2011-02-20 2011-09-07 中国船舶重工集团公司第七二五研究所 一种含钽中间层金属氧化物电极的制备方法
CN106521404A (zh) * 2016-11-02 2017-03-22 苏州云瑞环境科技有限公司 一种一次氧化制造钛阳极工艺
CN107699912A (zh) * 2017-09-01 2018-02-16 广东省稀有金属研究所 一种涂层电极的涂层溶液及其涂层电极的制备方法
CN107779847A (zh) * 2017-09-25 2018-03-09 上海同臣环保有限公司 一种涂层钛阳极及其喷涂热解制备方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109440158A (zh) * 2018-12-28 2019-03-08 南京时恒电子科技有限公司 一种Cu-Ti-Co复合电极及其制备方法
CN109868464A (zh) * 2019-03-11 2019-06-11 江阴安诺电极有限公司 具有贵金属涂层的阳极板
CN109706513A (zh) * 2019-03-12 2019-05-03 江阴安诺电极有限公司 涂层阳极板的制备方法
CN109763149A (zh) * 2019-03-12 2019-05-17 江阴安诺电极有限公司 铱钽涂层阳极板
CN110983387A (zh) * 2019-12-26 2020-04-10 西安泰金工业电化学技术有限公司 一种提高电解铜箔用阳极板寿命的方法
CN110983387B (zh) * 2019-12-26 2022-05-03 西安泰金工业电化学技术有限公司 一种提高电解铜箔用阳极板寿命的方法
CN111926310A (zh) * 2020-08-04 2020-11-13 淮南师范学院 高效高活性的电极涂层的制备方法
CN111926311A (zh) * 2020-08-06 2020-11-13 淮南师范学院 复合电极及其制备方法

Similar Documents

Publication Publication Date Title
CN108642479A (zh) 高效高活性的电极涂层的制备方法
EP1507899B1 (en) Electrode for gas evolution and method for its production
AU2016282820B2 (en) Electrode for electrolytic processes
WO1989001991A1 (en) A ceramic/metal composite material
Robin et al. Co-electrodeposition and characterization of Cu–Si3N4 composite coatings
AU2012210549B2 (en) Electrode for oxygen evolution in industrial electrochemical processes
Cheng et al. A systematic study of the role of cathodic polarization and new findings on the soft sparking phenomenon from plasma electrolytic oxidation of an Al-Cu-Li alloy
AU2012210549A1 (en) Electrode for oxygen evolution in industrial electrochemical processes
CN109706513A (zh) 涂层阳极板的制备方法
CN101333673B (zh) 用于微弧氧化制备纳米陶瓷涂层的电解液及处理方法
CN109534460B (zh) 一种钛电极及其制备方法与应用
CN107119296A (zh) 一种阳极活化钛合金电镀铜的方法
CN106119899A (zh) 废水回用不溶性阳极板制备方法
CN108707881A (zh) 高效高活性的铱钽涂液及其形成的铱钽涂层
CN108660488A (zh) 电解铜箔阳极板的制备方法
EP2925910B1 (en) Electrode for oxygen evolution in industrial electrochemical processes
CN111020664B (zh) 一种含石墨烯微弧氧化耐蚀陶瓷层的制备方法
JPWO2016010045A1 (ja) 電解用陰極及び電解用陰極の製造方法
TWI525225B (zh) 鍍鉬電解質及形成含鉬鍍層方法
TWI802731B (zh) 適於從電解池的電解質溶液電鍍或電澱積金屬用之電極及其製法，以及從電解質溶液電鍍或電澱積金屬用之未分隔電解池，和從電解質溶液電鍍或電澱積金屬之製法
JP2008156684A (ja) 塩酸電解用の陽極電極
JP2019108580A (ja) 不溶性陽極及び不溶性陽極の製造方法
JP2020535319A (ja) 少なくとも処理対象の基体に亜鉛−ニッケル合金層を電着させる方法
JP2006265707A (ja) 白金の被覆方法
JPH03240987A (ja) 有機物電解用電極及びその製造方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20181012