Journal of Jilin University(Engineering and Technology Edition) ›› 2023, Vol. 53 ›› Issue (5): 1322-1330.doi: 10.13229/j.cnki.jdxbgxb.20210918

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

Chao XIE1(),Qi-cai WANG1,2(),Ben-tian YU1,Sheng LI1,2,Xiao-xu LIN1,Zhi-ming LU3   

  1. 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

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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

CLC Number: 

  • TB332

Fig.1

Coating film samples"

Fig.2

Positional relationship between sample and detector"

Fig.3

Micromorphology of AFM probe tip"

Table 1

Influence coefficient of pyramid number on force-indentation result"

棱锥数（n）影响系数（C0）棱锥数（n）影响系数（C0）
31.777101.300
41.491151.285
51.398201.280
61.355501.274
81.316

Fig.4

Sress condition of probe in each stage of test curve"

Fig.5

Relative motion position of sample-AFM tip system in experiment"

Fig.6

Force-indentation depth curve of each coating film"

Table 2

Calculated elasticity modulus data for coating films"

试件编号E/MPaR2
F106.1180.978
F156.3630.957
F206.9170.986
F256.6390.964
F306.5120.948

Fig.7

Positron annihilation lifetime spectrum for each sample"

Fig.8

Spectrum unfolding fitting factor for each sample"

Fig.9

o-Ps annihilation lifetime of each sample"

Fig.10

o-Ps annihilation intensity of each sample"

Fig.11

Aerage free volume radius and content of each sample"

Table 3

Calculated date of grey correlation degree"

试件编号初值化序列差序列相关系数
X0'XR'XF'ΔR-0ΔF-0γ0R （k）γ0F （k）
F101110011
F151.040 045 7670.991 054 9040.944 326 9910.048 990 8620.095 718 7760.802 727 3410.675 605 203
F201.130 598 2350.937 075 8790.731 853 4180.193 522 3560.398 744 8170.507 416 7150.333 308 356
F251.085 158 5490.975 015 4230.842 142 3540.110 143 1260.243 016 1950.644 117 6990.450 644 743
F301.064 400 1310.980 876 0020.891 120 5070.083 524 1280.173 279 6230.704 730 4090.534 981 621
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