聚氨酯涂膜弹性模量的AFM测定及微观结构分析

doi:10.13229/j.cnki.jdxbgxb.20210918

吉林大学学报(工学版) ›› 2023, Vol. 53 ›› Issue (5): 1322-1330.doi: 10.13229/j.cnki.jdxbgxb.20210918

• 材料科学与工程 • 上一篇

聚氨酯涂膜弹性模量的AFM测定及微观结构分析

谢超¹(),王起才^1,²(),于本田¹,李盛^1,²,林晓旭¹,鲁志铭³

^1.兰州交通大学土木工程学院，兰州 730070
^2.兰州交通大学道桥工程灾害防治技术国家地方联合工程实验室，兰州 730070
^3.甘肃第七建设集团股份有限公司，兰州 730030

收稿日期:2021-09-13 出版日期:2023-05-01 发布日期:2023-05-25
通讯作者: 王起才 E-mail:327600231@qq.com;13909486262@163.com
作者简介:谢超（1990-），男，讲师，博士.研究方向：土木工程材料与结构.E-mail：327600231@qq.com
基金资助:
甘肃省自然科学基金项目(22JR5RA333);国家自然科学基金项目(51768033);长江学者和创新团队发展计划滚动项目(IRT_15R29)

Determination of elastic modulus by atomic force microscopy and microstructure analysis for polyurethane coating film

Chao XIE¹(),Qi-cai WANG^1,²(),Ben-tian YU¹,Sheng LI^1,²,Xiao-xu LIN¹,Zhi-ming LU³

^1.College of Civil Engineering，Lanzhou Jiaotong University，Lanzhou 730070，China
^2.National and Local Joint Engineering Laboratory for Disaster Prevention and Control Technology of Road and Bridge Engineering，Lanzhou Jiaotong University，Lanzhou 730070，China
^3.Gansu Seventh Construction Group Co. ，Ltd. ，Gansu Lanzhou 730030，China

Received:2021-09-13 Online:2023-05-01 Published:2023-05-25
Contact: Qi-cai WANG E-mail:327600231@qq.com;13909486262@163.com

摘要/Abstract

摘要：

为测定聚氨酯涂膜的弹性模量，建立了正三棱锥形态原子力显微镜（AFM）探针与涂膜的力学接触模型。同时，通过分析AFM的力学测试曲线，得出了探针与涂膜之间的力-压痕深度关系，并将其与力学接触模型相结合，确定了涂膜的弹性模量。此外，通过正电子湮灭技术测试了涂膜的微观结构，并与其弹性模量进行了对比分析。最后，采用灰色关联理论对微观结构参数与涂膜弹性模量的相关性进行了研究。结果表明：涂膜的弹性模量测定结果为6.118~6.917 MPa，与现有文献中聚氨酯涂膜弹性模量的研究结果一致，证明该方法测定结果准确。由于自由体积尺寸及含量的增大降低了基材对其分子链段运动的限制能力，故涂膜的弹性模量与其自由体积孔径及自由体积分数均呈负相关性，其中，涂膜的自由体积平均孔径对其弹性模量的影响程度更高。

关键词: 弹性模量, 原子力显微镜, 微观结构, 自由体积, 灰色关联度

Abstract:

In this work， the mechanical contact model between normal triangular atomic force microscopy（AFM） probe and coating film was established， which aims to measure the elastic modulus of polyurethane coating film. Whilst the force-indentation depth relationship between the probe and the coating film was obtained by analyzing the AFM's mechanical test curve， and the elastic modulus of the coating film was determined by combining the newly established model. In addition， the microstructure of the coating film was tested using positron-annihilation technology， and compared with its elastic modulus. Finally， the grey correlation theory is used to analyze the correlation between the microstructure parameters and the elastic modulus of the coating film. The results show that the elastic modulus of the coating film was measured within the region of 6.118 MPa to 6.917 MPa. This is consistent with the research results of the elastic modulus of polyurethane coating in existing literature， which guarantees the validity and accuracy of the present method. The elastic modulus of the coating film is negatively correlated with its free volume aperture and free volume fraction since that the restriction ability of the substrate to its molecular chain segment movement is significantly lowered with the increase of free volume size and content. Among them， the free volume average pore diameter of the coating film has higher effects on its elastic modulus.

Key words: elastic modulus, atomic force microscopy, microstructure, free volume, grey relational degree

中图分类号:

TB332

谢超,王起才,于本田,李盛,林晓旭,鲁志铭. 聚氨酯涂膜弹性模量的AFM测定及微观结构分析[J]. 吉林大学学报(工学版), 2023, 53(5): 1322-1330.

Chao XIE,Qi-cai WANG,Ben-tian YU,Sheng LI,Xiao-xu LIN,Zhi-ming LU. Determination of elastic modulus by atomic force microscopy and microstructure analysis for polyurethane coating film[J]. Journal of Jilin University(Engineering and Technology Edition), 2023, 53(5): 1322-1330.

图/表 14

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表1

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图6

表2

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图9

图10

图11

表3

灰色关联度的计算数据"

试件编号	初值化序列			差序列		相关系数
试件编号	$X 0'$	$X R'$	$X F'$	Δ_R_-0	Δ_F_-0	γ₀_R （k）	γ₀_F （k）
F₁₀	1	1	1	0	0	1	1
F₁₅	1.040 045 767	0.991 054 904	0.944 326 991	0.048 990 862	0.095 718 776	0.802 727 341	0.675 605 203
F₂₀	1.130 598 235	0.937 075 879	0.731 853 418	0.193 522 356	0.398 744 817	0.507 416 715	0.333 308 356
F₂₅	1.085 158 549	0.975 015 423	0.842 142 354	0.110 143 126	0.243 016 195	0.644 117 699	0.450 644 743
F₃₀	1.064 400 131	0.980 876 002	0.891 120 507	0.083 524 128	0.173 279 623	0.704 730 409	0.534 981 621

表3

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棱锥数（n）	影响系数（C₀）	棱锥数（n）	影响系数（C₀）
3	1.777	10	1.300
4	1.491	15	1.285
5	1.398	20	1.280
6	1.355	50	1.274
8	1.316

试件编号	E/MPa	R²
F₁₀	6.118	0.978
F₁₅	6.363	0.957
F₂₀	6.917	0.986
F₂₅	6.639	0.964
F₃₀	6.512	0.948

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聚氨酯涂膜弹性模量的AFM测定及微观结构分析

Determination of elastic modulus by atomic force microscopy and microstructure analysis for polyurethane coating film

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