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Article(id=1319970569358004378, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319987712212452222, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20230420, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1687104000000, receivedDateStr=2023-06-19, revisedDate=1689609600000, revisedDateStr=2023-07-18, acceptedDate=null, acceptedDateStr=null, onlineDate=1792635107601, onlineDateStr=2026-10-22, pubDate=1708358400000, pubDateStr=2024-02-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792635107601, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792635107601, creator=13701087609, updateTime=1792635107601, updator=13701087609, issue=Issue{id=1319987712212452222, tenantId=1146029695717560320, journalId=1263187385517883426, year='2024', volume='52', issue='2', pageStart='371', pageEnd='736', issueExtLink='null', onlineDate='null', pubDate='1708358400000', pubDateStr='2024-02-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792639194777, creator='13701087609', updateTime=1792641910689, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1319999103631737580, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319987712212452222, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1319999103631737581, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1319987712212452222, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=513, endPage=521, ext={EN=ArticleExt(id=1319970569555136667, articleId=1319970569358004378, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Growth of Different Cationic Layered Double Hydroxides Films on Carbon Steel Surfaces and Alkali and Corrosion Resistances, columnId=1319726165087077079, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Article, runingTitle=null, highlight=null, articleAbstract=
Introduction

Steel corrosion is particularly severe in marine environments with a high concentration of chloride ions, which causes huge economic losses and also hinders engineering construction in coastal areas. Coating treatment is one of the common methods to protect steel from corrosion. Conventional thicker organic coatings are prone to local breakage, reduced mechanical interlocking force between steel and concrete, and being easy to deteriorate. Since the anions and cations of layered double hydroxides (LDH) both are tunable, this designability gives them a variety of potentials for metal corrosion protection, such as physical barrier, chlorine fixation, corrosion inhibition and chemical self-repair. In this paper, Mg/Al-NO3--LDH and Zn/Al-NO3--LDH films were grown in-situ on the surface of steel Q235 by an electrodeposition-hydrothermal method, and their adaptability in a simulated high-alkaline concrete environment and corrosion inhibition performance in NaCl solution were investigated.

Methods

The in-situ growth of LDH film on steel surface includes electrodeposition and hydrothermal treatment. In the electrodeposition, a three-electrode system was used, with a steel sheet as a working electrode, an Ag/AgCl electrode as a reference electrode, and a platinum sheet as a counter electrode. The electrolyte solution consisted of 50 mL of 0.045 mol/L Mg(NO3)2·6H2O and 0.015 mol/L Al(NO3)3·9H2O, and the steel sheet was immersed in the electrolyte solution to stabilize it for 500 s, and then a potential of -1.5 V was applied for 300 s. The hydrothermal treatment used a hydrothermal solution consisting of 50 mL of 0.06 mol/L Mg(NO3)2·6H2O and 0.02 mol/L Al(NO3)3·9H2O. NH3·H2O was added dropwise to adjust the pH value of the solution to 9. Subsequently, the electrodeposited steel sheet was vertically placed into a Teflon®-lined autoclave containing the hydrothermal solution, and reacted in a homogeneous reactor at 90 ℃ for 18 h. After the reaction was completed and cooled down to room temperature, the sheet with the film was removed and named M1. Similarly, the obtained sample was named Z1 when replacing Mg(NO3)2·6H2O with Zn(NO3)2·6H2O. To examine the adaptability of the two samples in a high-alkaline concrete environment, the samples M1 and Z1 were immersed in saturated Ca(OH)2 solution for 24 h and then taken out, resulting in samples named M2 and Z2, respectively.

The crystal structures of the different samples were characterized using a model D8 Advance X-ray diffractometer (Bruker Co., Germany, λ=0.154 06 nm). Sample's functional groups and chemical bonds were detected using a model Spotlight 200 Fourier transform infrared spectrometer (PerkinElmer Co., USA). The surface morphology and chemical composition of the samples were determined by a model APREO S high-resolution scanning electron microscope with an X-ray energy spectrometer (Thermo scientific Co., The Netherlands). The impedance and corrosion resistance of the four samples in 3.5% (mass fraction) NaCl solution were analyzed via electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization in a ParStat 4000 electrochemical workstation (AMETEK Co., USA).

Results and discussion

The electrodeposition and hydrothermal method was employed to in-situ grow a dense and uniform Mg/Al-NO3--LDH film and a lamellar porous Zn/Al-NO3--LDH film on the surface of steel Q235. After immersing these two LDH films in a saturated Ca(OH)2 solution for 1 d, the lamellar structure of Mg/Al-LDH remains unchanged, and the interlayer anions are partially exchanged from NO3- to OH- due to the slightly higher affinity of OH- in the solution. Also, the lamellar structure of Zn/Al-LDH undergoes a chemical reaction due to the presence of a large amount of Ca2+ and OH-, resulting in the generated portion of Ca/Al-NO3-/OH--LDH and amorphous hydroxides remaining on the carbon steel surface. The results above indicate that Zn/Al-LDH is difficult to be stabilized in highly alkaline concrete environments since its constituents, i.e., Zn(OH)2 and Al(OH)3, both are amphoteric hydroxides. In contrast, Mg(OH)2 is an alkaline hydroxide, allowing Mg/Al-LDH to maintain a structural stability in high alkaline environments.

The EIS results show that in a 3.5% (in mass fraction) NaCl solution, the impedance of the Zn/Al-NO3--LDH film is only 3.18 Ω/cm2, whereas the Mg/Al-NO3--LDH film exhibits a greater impedance of 2 722 Ω/cm2, which is attributed to the dense structure of the Mg/Al-NO3--LDH film. The results of dynamic potentiodynamic polarization tests indicate that the corrosion protection efficiency of the Zn/Al-NO3--LDH film and the Mg/Al-NO3--LDH film for carbon steel is 63.86% and 97.43%, respectively. Clearly, the Mg/Al-NO3--LDH film is more effective in protecting carbon steel against chloride ion erosion due to its superior physical barrier and the double protection effect of "fixing chlorine".

Conclusions

Zn/Al-NO3--LDH and Mg/Al-NO3--LDH films with a high crystallinity were grown in-situ on the surface of steel Q235 by an electrodeposition-hydrothermal method for corrosion protection. The microscopy showed that the Zn/Al-NO3--LDH films were lamellar and porous, and the Mg/Al-NO3--LDH films were dense and uniform. The electrochemical results indicated that in 3.5% (in mass fraction) NaCl solution, the corrosion protection efficiency of Zn/Al-NO3--LDH film on carbon steel substrate was 63.86%, while the Mg/Al-NO3--LDH film had a higher impedance and a lower corrosion current density, and its corrosion protection efficiency was 97.43%, effectively protecting the carbon steel against chloride ion erosion. In a high-alkaline saturated Ca(OH)2 solution, the Zn/Al-NO3--LDH film exhibited an instability, leading to the formation of partially Ca/Al-NO3-/OH--LDH and amorphous hydroxides. In contrast, the Mg/Al-NO3--LDH film remained stable, and the anion exchange resulted in the formation of Mg/Al-NO3-/OH--LDH film.

, authors=Biqin DONG, Wenjie LIU, Ming PENG, Lei ZENG, Peiyu CHEN, Qingrui YANG, Shuxian HONG, authorsList=Biqin DONG, Wenjie LIU, Ming PENG, Lei ZENG, Peiyu CHEN, Qingrui YANG, Shuxian HONG, authorCompany=null, correspAuthors=Shuxian HONG, authorNote=

DONG Biqin (1975-), male, Ph.D., Professor. E-mail:

, correspAuthorsNote=
HONG Shuxian (1982-), female, Ph.D., Professor. E-mail:
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碳钢在海洋环境下的锈蚀尤为严重，层状双金属氢氧化物（LDH）因可设计性而在金属防腐上拥有巨大潜力。通过电沉积-水热法在碳钢表面原位生长Zn/Al-NO3--LDH和Mg/Al-NO3--LDH膜，并研究两者在混凝土高碱性环境下的适应性和在氯化钠溶液中的阻锈性能。结果表明：在高碱性饱和Ca（OH）2溶液中，Zn/Al-NO3--LDH膜难以稳定存在而新生成Ca/Al-NO3-/OH--LDH和部分无定形氢氧化物，Mg/Al-NO3--LDH膜则保持稳定且阴离子交换为Mg/Al-NO3-/OH--LDH膜。电化学结果显示在3.5%（质量分数）NaCl溶液中，Mg/Al-NO3--LDH膜拥有更高的阻抗和更低的腐蚀电流密度，其对碳钢基体的腐蚀保护效率高达97.43%，有效地抵御了氯离子侵蚀。

, authors=董必钦, 刘文杰, 彭铭, 曾磊, 陈沛榆, 杨清瑞, 洪舒贤, authorsList=董必钦, 刘文杰, 彭铭, 曾磊, 陈沛榆, 杨清瑞, 洪舒贤, authorCompany=null, correspAuthors=洪舒贤, authorNote=

董必钦（1975—），男，博士，教授。

, correspAuthorsNote=
洪舒贤（1982—），女，博士，教授。
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碳钢表面生长不同阳离子层状双金属氢氧化物膜及耐碱耐蚀性能
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董必钦 , 刘文杰 , 彭铭 , 曾磊 , 陈沛榆 , 杨清瑞 , 洪舒贤
硅酸盐学报 | 研究论文 2024,52(2): 513-521
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硅酸盐学报 |研究论文 2024 , 52 (2) : 513 -521
碳钢表面生长不同阳离子层状双金属氢氧化物膜及耐碱耐蚀性能
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董必钦 , 刘文杰, 彭铭, 曾磊, 陈沛榆, 杨清瑞, 洪舒贤
作者信息
  • 深圳大学土木与交通工程学院，广东省滨海土木工程耐久性重点实验室，深圳市低碳建筑材料与技术重点实验室，广东 深圳 518060
通讯作者:
洪舒贤（1982—），女，博士，教授。
作者简介:

董必钦（1975—），男，博士，教授。

Growth of Different Cationic Layered Double Hydroxides Films on Carbon Steel Surfaces and Alkali and Corrosion Resistances
Biqin DONG , Wenjie LIU, Ming PENG, Lei ZENG, Peiyu CHEN, Qingrui YANG, Shuxian HONG
Affiliations
  • College of Civil and Transportation Engineering, Guangdong Provincial Key Laboratory of Durability for Marine Civil Engineering, Shenzhen Key Laboratory for Low-carbon Construction Material and Technology, Shenzhen University, Shenzhen 518060, Guangdong, China
    • Corresponding Author:
    HONG Shuxian (1982-), female, Ph.D., Professor. E-mail:

    DONG Biqin (1975-), male, Ph.D., Professor. E-mail:

出版时间: 2024-02-20 doi: 10.14062/j.issn.0454-5648.20230420
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碳钢在海洋环境下的锈蚀尤为严重，层状双金属氢氧化物（LDH）因可设计性而在金属防腐上拥有巨大潜力。通过电沉积-水热法在碳钢表面原位生长Zn/Al-NO3--LDH和Mg/Al-NO3--LDH膜，并研究两者在混凝土高碱性环境下的适应性和在氯化钠溶液中的阻锈性能。结果表明：在高碱性饱和Ca（OH）2溶液中，Zn/Al-NO3--LDH膜难以稳定存在而新生成Ca/Al-NO3-/OH--LDH和部分无定形氢氧化物，Mg/Al-NO3--LDH膜则保持稳定且阴离子交换为Mg/Al-NO3-/OH--LDH膜。电化学结果显示在3.5%（质量分数）NaCl溶液中，Mg/Al-NO3--LDH膜拥有更高的阻抗和更低的腐蚀电流密度，其对碳钢基体的腐蚀保护效率高达97.43%，有效地抵御了氯离子侵蚀。

电沉积-水热法  /  层状双金属氢氧化物  /  金属阳离子  /  耐碱性  /  耐腐蚀性
Introduction

Steel corrosion is particularly severe in marine environments with a high concentration of chloride ions, which causes huge economic losses and also hinders engineering construction in coastal areas. Coating treatment is one of the common methods to protect steel from corrosion. Conventional thicker organic coatings are prone to local breakage, reduced mechanical interlocking force between steel and concrete, and being easy to deteriorate. Since the anions and cations of layered double hydroxides (LDH) both are tunable, this designability gives them a variety of potentials for metal corrosion protection, such as physical barrier, chlorine fixation, corrosion inhibition and chemical self-repair. In this paper, Mg/Al-NO3--LDH and Zn/Al-NO3--LDH films were grown in-situ on the surface of steel Q235 by an electrodeposition-hydrothermal method, and their adaptability in a simulated high-alkaline concrete environment and corrosion inhibition performance in NaCl solution were investigated.

Methods

The in-situ growth of LDH film on steel surface includes electrodeposition and hydrothermal treatment. In the electrodeposition, a three-electrode system was used, with a steel sheet as a working electrode, an Ag/AgCl electrode as a reference electrode, and a platinum sheet as a counter electrode. The electrolyte solution consisted of 50 mL of 0.045 mol/L Mg(NO3)2·6H2O and 0.015 mol/L Al(NO3)3·9H2O, and the steel sheet was immersed in the electrolyte solution to stabilize it for 500 s, and then a potential of -1.5 V was applied for 300 s. The hydrothermal treatment used a hydrothermal solution consisting of 50 mL of 0.06 mol/L Mg(NO3)2·6H2O and 0.02 mol/L Al(NO3)3·9H2O. NH3·H2O was added dropwise to adjust the pH value of the solution to 9. Subsequently, the electrodeposited steel sheet was vertically placed into a Teflon®-lined autoclave containing the hydrothermal solution, and reacted in a homogeneous reactor at 90 ℃ for 18 h. After the reaction was completed and cooled down to room temperature, the sheet with the film was removed and named M1. Similarly, the obtained sample was named Z1 when replacing Mg(NO3)2·6H2O with Zn(NO3)2·6H2O. To examine the adaptability of the two samples in a high-alkaline concrete environment, the samples M1 and Z1 were immersed in saturated Ca(OH)2 solution for 24 h and then taken out, resulting in samples named M2 and Z2, respectively.

The crystal structures of the different samples were characterized using a model D8 Advance X-ray diffractometer (Bruker Co., Germany, λ=0.154 06 nm). Sample's functional groups and chemical bonds were detected using a model Spotlight 200 Fourier transform infrared spectrometer (PerkinElmer Co., USA). The surface morphology and chemical composition of the samples were determined by a model APREO S high-resolution scanning electron microscope with an X-ray energy spectrometer (Thermo scientific Co., The Netherlands). The impedance and corrosion resistance of the four samples in 3.5% (mass fraction) NaCl solution were analyzed via electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization in a ParStat 4000 electrochemical workstation (AMETEK Co., USA).

Results and discussion

The electrodeposition and hydrothermal method was employed to in-situ grow a dense and uniform Mg/Al-NO3--LDH film and a lamellar porous Zn/Al-NO3--LDH film on the surface of steel Q235. After immersing these two LDH films in a saturated Ca(OH)2 solution for 1 d, the lamellar structure of Mg/Al-LDH remains unchanged, and the interlayer anions are partially exchanged from NO3- to OH- due to the slightly higher affinity of OH- in the solution. Also, the lamellar structure of Zn/Al-LDH undergoes a chemical reaction due to the presence of a large amount of Ca2+ and OH-, resulting in the generated portion of Ca/Al-NO3-/OH--LDH and amorphous hydroxides remaining on the carbon steel surface. The results above indicate that Zn/Al-LDH is difficult to be stabilized in highly alkaline concrete environments since its constituents, i.e., Zn(OH)2 and Al(OH)3, both are amphoteric hydroxides. In contrast, Mg(OH)2 is an alkaline hydroxide, allowing Mg/Al-LDH to maintain a structural stability in high alkaline environments.

The EIS results show that in a 3.5% (in mass fraction) NaCl solution, the impedance of the Zn/Al-NO3--LDH film is only 3.18 Ω/cm2, whereas the Mg/Al-NO3--LDH film exhibits a greater impedance of 2 722 Ω/cm2, which is attributed to the dense structure of the Mg/Al-NO3--LDH film. The results of dynamic potentiodynamic polarization tests indicate that the corrosion protection efficiency of the Zn/Al-NO3--LDH film and the Mg/Al-NO3--LDH film for carbon steel is 63.86% and 97.43%, respectively. Clearly, the Mg/Al-NO3--LDH film is more effective in protecting carbon steel against chloride ion erosion due to its superior physical barrier and the double protection effect of "fixing chlorine".

Conclusions

Zn/Al-NO3--LDH and Mg/Al-NO3--LDH films with a high crystallinity were grown in-situ on the surface of steel Q235 by an electrodeposition-hydrothermal method for corrosion protection. The microscopy showed that the Zn/Al-NO3--LDH films were lamellar and porous, and the Mg/Al-NO3--LDH films were dense and uniform. The electrochemical results indicated that in 3.5% (in mass fraction) NaCl solution, the corrosion protection efficiency of Zn/Al-NO3--LDH film on carbon steel substrate was 63.86%, while the Mg/Al-NO3--LDH film had a higher impedance and a lower corrosion current density, and its corrosion protection efficiency was 97.43%, effectively protecting the carbon steel against chloride ion erosion. In a high-alkaline saturated Ca(OH)2 solution, the Zn/Al-NO3--LDH film exhibited an instability, leading to the formation of partially Ca/Al-NO3-/OH--LDH and amorphous hydroxides. In contrast, the Mg/Al-NO3--LDH film remained stable, and the anion exchange resulted in the formation of Mg/Al-NO3-/OH--LDH film.

electrodeposition-hydrothermal  /  layered double hydroxide  /  metal cation  /  alkali resistance  /  corrosion resistance
董必钦, 刘文杰, 彭铭, 曾磊, 陈沛榆, 杨清瑞, 洪舒贤. 碳钢表面生长不同阳离子层状双金属氢氧化物膜及耐碱耐蚀性能. 硅酸盐学报, 2024 , 52 (2) : 513 -521 . DOI: 10.14062/j.issn.0454-5648.20230420
Biqin DONG, Wenjie LIU, Ming PENG, Lei ZENG, Peiyu CHEN, Qingrui YANG, Shuxian HONG. Growth of Different Cationic Layered Double Hydroxides Films on Carbon Steel Surfaces and Alkali and Corrosion Resistances[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (2) : 513 -521 . DOI: 10.14062/j.issn.0454-5648.20230420
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doi: 10.14062/j.issn.0454-5648.20230420
  • 接收时间：2023-06-19
  • 首发时间：2026-10-22
  • 出版时间：2024-02-20
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  • 收稿日期：2023-06-19
  • 修回日期：2023-07-18
基金
国家自然科学基金(52078298; 52122907; 51925805)
作者信息
    深圳大学土木与交通工程学院，广东省滨海土木工程耐久性重点实验室，深圳市低碳建筑材料与技术重点实验室，广东 深圳 518060

通讯作者:

洪舒贤（1982—），女，博士，教授。
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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