HU Dexin, SHAN Yuxi, WANG Hailiang, et al. Microstructure and self-repairing performance of granular loaded graphene oxide composite cement-based materials[J]. Acta Materiae Compositae Sinica, 2024, 41(6): 3079-3091. DOI: 10.13801/j.cnki.fhclxb.20231025.002
Citation: HU Dexin, SHAN Yuxi, WANG Hailiang, et al. Microstructure and self-repairing performance of granular loaded graphene oxide composite cement-based materials[J]. Acta Materiae Compositae Sinica, 2024, 41(6): 3079-3091. DOI: 10.13801/j.cnki.fhclxb.20231025.002

Microstructure and self-repairing performance of granular loaded graphene oxide composite cement-based materials

Funds: Natural Science Foundation of China (51872137)
More Information
  • Received Date: August 27, 2023
  • Revised Date: September 30, 2023
  • Accepted Date: October 19, 2023
  • Available Online: October 24, 2023
  • To improve the dispersion performance of graphene oxide (GO) in the cement materials, nano SiO2 and CaCO3 powder were used as support of the GO and the SiO2-GO (SG) and SiO2-CaCO3-GO (SCG) were prepared. The effects of the SG and SCG on the mechanical strength, self-repairing performance, hydration products and microstructure of the cement materials were studied. The results show that the mechanical strength of the cement material is improved as the addition of SG and SCG, the flexural strength and compressive strength of the cement-based materials with SCG at 28 days are improved by 7.3% and 18.7%, respectively. The self-repairing performance of SCG composite cement is also improved which shows a higher compressive strength repairing rate of about 110.6% and a higher water permeability repairing rate of 100%. The crack area testing shows that SCG has a more significant repair effect on cracks in the cement materials. XRD analysis shows that the early stage cement hydration is accelerated as the addition of SG and SCG, especially for the SCG, the hydration degree at 3 days is obviously improved. TG analysis shows that with the extension of hydration age, a higher reaction degree of Ca(OH)2 and SiO2 is achieved in the SCG composite cement, compared with the early 3 days hydration stage, the Ca(OH)2 content of SCG composite cement at 28 days reduces to 14.90%. Microstructure analysis shows that the SCG has better compatibility with the cement, more hydrate calcium silicate (C-S-H) gels in the late hydration stage is generated and the microcracks of cement could be filled, which makes the excellent self-repairing performance of the SCG composite cement.
  • Objective 

    The self-repairing of cement-based materials is an effective way for the improvement of the durability performance. The addition of graphene oxide (GO) has a toughening and strengthening effect on cement-based materials, which has a positive effect on the micro-crack self-healing of the cement-based materials. In this paper, highly dispersion of GO in cement-based materials is achieved by granular loaded method, and the effects of GO incorporation on mechanical properties, self-repairing properties, hydration products and microstructure of cement-based materials were studied.

    Method 

    SiO-GO (SG) and SiO-CaCO-GO (SCG) were prepared by granular loaded method, nano-SiO and CaCO powder as the support of GO, the effects of incorporation of SG and SCG on the mechanical properties of cement-based materials were studied. The self-repairing properties of the cement-based materials were characterized by compressive strength repairing rate, water permeability repairing rate and crack repairing rate. The effects of granular loaded GO on the hydration products of cement-based materials were analyzed by XRD; the hydration process of cement-based materials were analyzed by TG; the effect of granular loaded GO on the microstructure of cement-based materials were analyzed by SEM-EDS, and the related mechanism of granular loaded GO on the self-repairing properties of cement-based materials was proposed.

    Results 

    According to the test results of mechanical properties, under the same dosage, the flexural strength of SCG/CE sample at 28d reached 8.8 MPa, increased by 7.3% compared with the blank sample, and the flexural strength of SiO/CE and SG/CE decreased slightly. The compressive strength of SCG/CE sample at 28d was 57.2 MPa, increased by 18.7% compared with the blank sample, which was significantly higher than that of SiO/CE and SG/CE samples. SCG/CE specimens showed better repair ability than the other specimens. Among them, the compressive strength repair rate reached 110.6%, and the water permeability repair rate and surface crack repair rate reached 100% after 28d repairing. XRD and TG analysis showed that SCG/CE had a higher hydration degree at different curing age, the content of Ca(OH) further decreased from 15.77% at 3d to 14.90% at 28d. It also can be seen from the SEM of each sample that the connection between the particles and the cement matrix in the SCG/CE specimen is more close, more hydration products produced on the surface of the plate SCG particles. EDS spectra also showed that the Ca/Si mass ratio of SCG/CE was higher than the other samples, with the advancement of hydration age, particles participate in hydration, and the hydration degree of SCG is higher, which also take a good explanation for the better self-repairing performance of SCG/CE samples: due to the high dispersion of SCG and good interfacial compatibility with cement, SCG/CE samples have better self-repairing properties. When micro-cracks appeared, SCG in the micro-crack could react with the Ca, the generation of C-S-H gel products filled the micro-cracks of the cement, resulting in the improvement of the mechanical strength of the cement, the self-repairing behavior is beneficial for the enhancement of the durability of the cement-based materials.Conclusions: With the special two-dimensional nanostructure, GO can be used as a nucleation site to promote cement hydration and regulate hydration products of cement-based materials, and the mechanical performance, microstructure and durability of cement-based materials could be improved by the high dispersion of GO in the cement. In this paper, SCG particles with a stronger compatibility with cement-based materials were prepared by granular loaded method, which allowed GO to be highly dispersed and realized the self-repairing properties of cement-based materials,the mechanism of the action of SCG on the self-repairing performance of cement-based materials was analyzed, the study provide some guidance for the self-repairing performance of GO in cement-based materials.

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