Article(id=1320107577187353548, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107562284986563, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20250596, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1754496000000, receivedDateStr=2025-08-07, revisedDate=1757520000000, revisedDateStr=2025-09-11, acceptedDate=null, acceptedDateStr=null, onlineDate=1792667772814, onlineDateStr=2026-10-22, pubDate=1783526400000, pubDateStr=2026-07-09, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792667772814, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792667772814, creator=13701087609, updateTime=1792667772814, updator=13701087609, issue=Issue{id=1320107562284986563, tenantId=1146029695717560320, journalId=1263187385517883426, year='2026', volume='54', issue='8', pageStart='2577', pageEnd='2948', issueExtLink='null', onlineDate='null', pubDate='1787155200000', pubDateStr='2026-08-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792667769261, creator='13701087609', updateTime=1792720485859, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1320328671789957452, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107562284986563, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1320328671789957453, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107562284986563, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=2795, endPage=2808, ext={EN=ArticleExt(id=1320107578059768781, articleId=1320107577187353548, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Performance Evolution of Modified Steel Fiber UHPC Under Coupling Effect of Compound Salts Erosion and Freeze-Thaw Cycles, columnId=1263922769897599102, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Articles, runingTitle=null, highlight=null, articleAbstract=
Introduction

The western region of China is characterized by high altitude, significant diurnal temperature variations, and extensive saline soil distribution. Under the coupled effect of freeze-thaw cycles and salt attack, the service life of local concrete structures decreases significantly, resulting in substantial economic losses. Although steel fiber-reinforced ultra-high performance concrete (UHPC) exhibits an enhanced freeze-thaw resistance, it faces a challenge of underutilization of fiber strength due to the limitations imposed by fiber-matrix interface degradation and inherent matrix risks. In this study, ethylenediaminetetraacetic acid (EDTA) treated steel fibers replaced conventional steel fibers to enhance the mechanical properties and freeze-thaw resistance of UHPC via improving the fiber-concrete matrix interface performance.

Methods

In this study, steel fibers were modified using the EDTA method. First, 0.05 mol/L CaCl2 and 0.05 mol/L Na2CO3 solutions were prepared separately, and 1% EDTA was added to Na2CO3 solution. Subsequently, the steel fibers were immersed in a mixed solution of CaCl2, Na2CO3, and EDTA for 6 h. Finally, the fibers were washed with distilled water. Based on the measured concentrations of SO42- and Cl- in saline soil from Golmud, this study employed a 133.6 g/L NaCl and 19.5 g/L MgSO4 solutions to simulate the corrosive environment for freeze-thaw tests. This study investigated the effect of combined salt attack-freeze-thaw cycles on the fiber-matrix interfacial bond strength, pull-out energy, relative dynamic elastic modulus, mass loss ratio, compressive strength, and flexural strength of UHPC. The phase composition and microstructure were characterized by X-ray diffraction (XRD), mercury intrusion porosimetry (MIP) and scanning electron microscopy (SEM), revealing the microscopic mechanisms of performance degradation. In addition, a freeze-thaw damage model for UHPC was also established based on the two-parameter Weibull distribution function.

Results and discussion

The EDTA modification induces a longitudinal exfoliation on steel fiber surfaces, resulting in a significantly increased roughness. The interfacial bond strength and pull-out energy are enhanced by 22.2% and 66.7%, respectively. Correspondingly, the compressive strength and flexural strength of UHPC are improved by 2.5% and 12%. The enhanced fiber-matrix interfacial bond strength and pull-out energy increase the ultimate tensile stress required for unstable propagation of microcracks in UHPC, effectively inhibiting the initiation and development of microcracks. This mechanism thereby enhances its freeze-thaw resistance. After 500 cycles of water-freezing and salt solution freezing tests, the EDTA-treated steel fiber-reinforced UHPC demonstrates significantly superior performance, compared to conventional steel fiber UHPC in all critical metrics i.e., interfacial bond strength, pull-out energy, compressive strength, flexural strength, relative dynamic elastic modulus, mass loss ratio, and porosity. After 500 freeze-thaw cycles in water, the bond strength of plain steel fiber UHPC and modified steel fiber UHPC are decreased by 40.4% and 27.8%, respectively. Their pullout energy are declined by 29.7% and 50.6%, respectively. The relative dynamic elastic modulus are decreased by 5.26% and 4.57%, respectively. The masses are reduced by 0.46% and 0.45%, respectively. The compressive strengths are decreased by 16.6% and 16%, respectively, and the flexural strengths are decreased by 26.1% and 20.6%, respectively. After 500 salt solution freeze-thaw cycles, the bond strength of plain steel fiber UHPC and modified steel fiber UHPC are decreased by 41.3% and 39.3%, respectively. The pullout energies are declined by 40.5% and 54.2%, respectively. The relative dynamic elastic modulus are dropped by 5.44% and 5.25%. The masses are reduced by 0.5% and 0.48%. The compressive strengths are decreased by 21.4% and 20.3%, respectively, and the flexural strengths are decreased by 29.3% and 25.2%, respectively. The XRD patterns reveal that after 500 salt solution freeze-thaw cycles, some expansive products such as ettringite and gypsum are formed within the UHPC. The expansive stresses generated by these products induce crack initiation and propagation, thereby degrading the performance of the UHPC. MIP indicates that freeze-thaw cycles result in an increased porosity in UHPC. In both water-freezing and salt solution freeze-thaw environments, the porosity of modified steel fiber UHPC is lower than that of plain steel fiber UHPC. SEM images reveal that during debonding of modified steel fibers from the matrix, a greater amount of weak matrix material adhering to the fiber surfaces is carried away. This phenomenon demonstrates that modified steel fibers establish a stronger interfacial bonding with the cementitious matrix. Based on the predictions by the Weibull model, the critical freeze-thaw cycles for EDTA-treated and conventional steel fiber-reinforced UHPC are predicted to be 1610 and 1270 cycles under water-freezing exposure, and 1220 and 1150 cycles under salt solution-freezing exposure, respectively. The results indicate that in the both environments, fiber modification treatment can effectively enhance the freeze-thaw resistance of UHPC and significantly improve its durability.

Couclusions

The results demonstrated that EDTA modification treatment enhanced the strength and fiber-matrix interfacial bonding performance of UHPC, inhibited micro-crack propagation, thereby slowing the deterioration rate of properties such as relative dynamic elastic modulus and strength during freeze-thaw cycles, reduced mass loss, and improved the freeze-thaw resistance of UHPC. The freeze-thaw damage model predicted that EDTA-modified steel fiber UHPC could have a 26.8% increase in freeze-thaw cycle resistance under water-freezing conditions and a 6.1% improvement under salt solution-freezing environments, compared to conventional steel fiber UHPC. This study could offer a reference for the durability de-sign of UHPC structures in cold saline soil regions of western China.

, authors=Ling QIN1, Xianqi ZHANG1, Jiuwen BAO1, Xiaojian GAO2, Jianwei Sun1, authorsList=Ling QIN, Xianqi ZHANG, Jiuwen BAO, Xiaojian GAO, Jianwei Sun, authorCompany=null, correspAuthors=Jianwei Sun, authorNote=

QIN Ling (1993-), female, Ph.D., Associate Professor. E-mail:

, correspAuthorsNote=
{SUN} Jianwei (1991-), male, Ph.D., Associate Professor. E-mail:
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中国西部地区海拔高、昼夜温差大、盐渍土广泛分布,混凝土结构面临复合盐蚀-冻融循环耦合作用问题。为提高超高性能混凝土(UHPC)抗盐溶液冻融性能,采用乙二胺四乙酸(EDTA)法改性钢纤维制备UHPC,研究了复合盐蚀-冻融循环耦合作用对UHPC纤维-基体界面粘结强度、拔出能以及UHPC相对动弹性模量、质量损失率、抗压强度、抗折强度等宏观性能的影响,并利用X射线衍射分析、压汞法分析、扫描电子显微镜分析等测试分析了UHPC物相组成、微观结构特征演变规律,揭示了UHPC性能劣化微观机理。此外,基于二参数Weibull分布函数建立了UHPC冻融损伤模型。研究结果表明:EDTA改性处理可提高UHPC的强度及纤维-基体界面粘结性能,抑制微裂缝发展,从而减缓冻融过程中UHPC相对动弹性模量、强度等性能的劣化速度,减少质量损失,提高了UHPC抗冻融性能。冻融损伤模型预测改性钢纤维UHPC在水冻和盐溶液冻融环境下抗冻融循环次数较普通钢纤维UHPC分别提高26.8%和6.1%。研究为西部寒冷盐渍土地区UHPC的耐久性设计提供了参考。

, authors=秦玲1, 张先起1, 鲍玖文1, 高小建2, 孙建伟1, authorsList=秦玲, 张先起, 鲍玖文, 高小建, 孙建伟, authorCompany=null, correspAuthors=孙建伟, authorNote=

秦玲(1993—),女,博士,副教授。

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孙建伟(1991—),男,博士,副教授。
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复合盐蚀-冻融循环耦合作用下改性钢纤维超高性能混凝土性能演变规律
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秦玲 1 , 张先起 1 , 鲍玖文 1 , 高小建 2 , 孙建伟 1
硅酸盐学报 | 研究论文 2026,54(8): 2795-2808
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硅酸盐学报 |研究论文 2026 , 54 (8) : 2795 -2808
复合盐蚀-冻融循环耦合作用下改性钢纤维超高性能混凝土性能演变规律
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秦玲1 , 张先起1, 鲍玖文1, 高小建2, 孙建伟1
作者信息
  • 1.青岛理工大学土木工程学院,山东 青岛 266520
  • 2.哈尔滨工业大学土木工程学院,哈尔滨 150090
通讯作者:
孙建伟(1991—),男,博士,副教授。
作者简介:

秦玲(1993—),女,博士,副教授。

Performance Evolution of Modified Steel Fiber UHPC Under Coupling Effect of Compound Salts Erosion and Freeze-Thaw Cycles
Ling QIN1 , Xianqi ZHANG1, Jiuwen BAO1, Xiaojian GAO2, Jianwei Sun1
Affiliations
  • 1.School of Civil Engineering, Qingdao University of Tech-nology, Qingdao 266520, Shandong, China
  • 2.School of Civil Engineering, Harbin Institute of Technology, Harbin 150090, China
  • Corresponding Author:
    {SUN} Jianwei (1991-), male, Ph.D., Associate Professor. E-mail:

    QIN Ling (1993-), female, Ph.D., Associate Professor. E-mail:

出版时间: 2026-07-09 doi: 10.14062/j.issn.0454-5648.20250596
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中国西部地区海拔高、昼夜温差大、盐渍土广泛分布,混凝土结构面临复合盐蚀-冻融循环耦合作用问题。为提高超高性能混凝土(UHPC)抗盐溶液冻融性能,采用乙二胺四乙酸(EDTA)法改性钢纤维制备UHPC,研究了复合盐蚀-冻融循环耦合作用对UHPC纤维-基体界面粘结强度、拔出能以及UHPC相对动弹性模量、质量损失率、抗压强度、抗折强度等宏观性能的影响,并利用X射线衍射分析、压汞法分析、扫描电子显微镜分析等测试分析了UHPC物相组成、微观结构特征演变规律,揭示了UHPC性能劣化微观机理。此外,基于二参数Weibull分布函数建立了UHPC冻融损伤模型。研究结果表明:EDTA改性处理可提高UHPC的强度及纤维-基体界面粘结性能,抑制微裂缝发展,从而减缓冻融过程中UHPC相对动弹性模量、强度等性能的劣化速度,减少质量损失,提高了UHPC抗冻融性能。冻融损伤模型预测改性钢纤维UHPC在水冻和盐溶液冻融环境下抗冻融循环次数较普通钢纤维UHPC分别提高26.8%和6.1%。研究为西部寒冷盐渍土地区UHPC的耐久性设计提供了参考。

超高性能混凝土  /  改性钢纤维  /  冻融循环  /  力学性能  /  微观结构
Introduction

The western region of China is characterized by high altitude, significant diurnal temperature variations, and extensive saline soil distribution. Under the coupled effect of freeze-thaw cycles and salt attack, the service life of local concrete structures decreases significantly, resulting in substantial economic losses. Although steel fiber-reinforced ultra-high performance concrete (UHPC) exhibits an enhanced freeze-thaw resistance, it faces a challenge of underutilization of fiber strength due to the limitations imposed by fiber-matrix interface degradation and inherent matrix risks. In this study, ethylenediaminetetraacetic acid (EDTA) treated steel fibers replaced conventional steel fibers to enhance the mechanical properties and freeze-thaw resistance of UHPC via improving the fiber-concrete matrix interface performance.

Methods

In this study, steel fibers were modified using the EDTA method. First, 0.05 mol/L CaCl2 and 0.05 mol/L Na2CO3 solutions were prepared separately, and 1% EDTA was added to Na2CO3 solution. Subsequently, the steel fibers were immersed in a mixed solution of CaCl2, Na2CO3, and EDTA for 6 h. Finally, the fibers were washed with distilled water. Based on the measured concentrations of SO42- and Cl- in saline soil from Golmud, this study employed a 133.6 g/L NaCl and 19.5 g/L MgSO4 solutions to simulate the corrosive environment for freeze-thaw tests. This study investigated the effect of combined salt attack-freeze-thaw cycles on the fiber-matrix interfacial bond strength, pull-out energy, relative dynamic elastic modulus, mass loss ratio, compressive strength, and flexural strength of UHPC. The phase composition and microstructure were characterized by X-ray diffraction (XRD), mercury intrusion porosimetry (MIP) and scanning electron microscopy (SEM), revealing the microscopic mechanisms of performance degradation. In addition, a freeze-thaw damage model for UHPC was also established based on the two-parameter Weibull distribution function.

Results and discussion

The EDTA modification induces a longitudinal exfoliation on steel fiber surfaces, resulting in a significantly increased roughness. The interfacial bond strength and pull-out energy are enhanced by 22.2% and 66.7%, respectively. Correspondingly, the compressive strength and flexural strength of UHPC are improved by 2.5% and 12%. The enhanced fiber-matrix interfacial bond strength and pull-out energy increase the ultimate tensile stress required for unstable propagation of microcracks in UHPC, effectively inhibiting the initiation and development of microcracks. This mechanism thereby enhances its freeze-thaw resistance. After 500 cycles of water-freezing and salt solution freezing tests, the EDTA-treated steel fiber-reinforced UHPC demonstrates significantly superior performance, compared to conventional steel fiber UHPC in all critical metrics i.e., interfacial bond strength, pull-out energy, compressive strength, flexural strength, relative dynamic elastic modulus, mass loss ratio, and porosity. After 500 freeze-thaw cycles in water, the bond strength of plain steel fiber UHPC and modified steel fiber UHPC are decreased by 40.4% and 27.8%, respectively. Their pullout energy are declined by 29.7% and 50.6%, respectively. The relative dynamic elastic modulus are decreased by 5.26% and 4.57%, respectively. The masses are reduced by 0.46% and 0.45%, respectively. The compressive strengths are decreased by 16.6% and 16%, respectively, and the flexural strengths are decreased by 26.1% and 20.6%, respectively. After 500 salt solution freeze-thaw cycles, the bond strength of plain steel fiber UHPC and modified steel fiber UHPC are decreased by 41.3% and 39.3%, respectively. The pullout energies are declined by 40.5% and 54.2%, respectively. The relative dynamic elastic modulus are dropped by 5.44% and 5.25%. The masses are reduced by 0.5% and 0.48%. The compressive strengths are decreased by 21.4% and 20.3%, respectively, and the flexural strengths are decreased by 29.3% and 25.2%, respectively. The XRD patterns reveal that after 500 salt solution freeze-thaw cycles, some expansive products such as ettringite and gypsum are formed within the UHPC. The expansive stresses generated by these products induce crack initiation and propagation, thereby degrading the performance of the UHPC. MIP indicates that freeze-thaw cycles result in an increased porosity in UHPC. In both water-freezing and salt solution freeze-thaw environments, the porosity of modified steel fiber UHPC is lower than that of plain steel fiber UHPC. SEM images reveal that during debonding of modified steel fibers from the matrix, a greater amount of weak matrix material adhering to the fiber surfaces is carried away. This phenomenon demonstrates that modified steel fibers establish a stronger interfacial bonding with the cementitious matrix. Based on the predictions by the Weibull model, the critical freeze-thaw cycles for EDTA-treated and conventional steel fiber-reinforced UHPC are predicted to be 1610 and 1270 cycles under water-freezing exposure, and 1220 and 1150 cycles under salt solution-freezing exposure, respectively. The results indicate that in the both environments, fiber modification treatment can effectively enhance the freeze-thaw resistance of UHPC and significantly improve its durability.

Couclusions

The results demonstrated that EDTA modification treatment enhanced the strength and fiber-matrix interfacial bonding performance of UHPC, inhibited micro-crack propagation, thereby slowing the deterioration rate of properties such as relative dynamic elastic modulus and strength during freeze-thaw cycles, reduced mass loss, and improved the freeze-thaw resistance of UHPC. The freeze-thaw damage model predicted that EDTA-modified steel fiber UHPC could have a 26.8% increase in freeze-thaw cycle resistance under water-freezing conditions and a 6.1% improvement under salt solution-freezing environments, compared to conventional steel fiber UHPC. This study could offer a reference for the durability de-sign of UHPC structures in cold saline soil regions of western China.

ultra-high performance concrete  /  modified steel fibers  /  freeze-thaw cycle  /  mechanical properties  /  microstructure
秦玲, 张先起, 鲍玖文, 高小建, 孙建伟. 复合盐蚀-冻融循环耦合作用下改性钢纤维超高性能混凝土性能演变规律. 硅酸盐学报, 2026 , 54 (8) : 2795 -2808 . DOI: 10.14062/j.issn.0454-5648.20250596
Ling QIN, Xianqi ZHANG, Jiuwen BAO, Xiaojian GAO, Jianwei Sun. Performance Evolution of Modified Steel Fiber UHPC Under Coupling Effect of Compound Salts Erosion and Freeze-Thaw Cycles[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (8) : 2795 -2808 . DOI: 10.14062/j.issn.0454-5648.20250596
  • 国家自然科学基金(52578293; U23A20661)
  • 山东省自然科学基金(ZR2025MS707)
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doi: 10.14062/j.issn.0454-5648.20250596
  • 接收时间:2025-08-07
  • 首发时间:2026-10-22
  • 出版时间:2026-07-09
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  • 收稿日期:2025-08-07
  • 修回日期:2025-09-11
基金
国家自然科学基金(52578293; U23A20661)
山东省自然科学基金(ZR2025MS707)
作者信息
    1.青岛理工大学土木工程学院,山东 青岛 266520
    2.哈尔滨工业大学土木工程学院,哈尔滨 150090

通讯作者:

孙建伟(1991—),男,博士,副教授。
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