西南石油大学 新能源与材料学院，油气藏地质及开发工程全国重点实验室，四川成都 610500
引用格式：
胡陈，张春梅，苏晓悦，等 . 海泡石纤维表面包覆二氧化硅增强油井水泥的力学性能［J］.中国粉体技术，2024，30（4）：51-61.
HU C， ZHANG C M， SU X Y， et al. Mechanical properties of oil well cement reinforced by the silica-coated surface of sepiolite fiber［J］.China Powder Science and Technology，2024，30（4）：51−61.
DOI：10.13732/j.issn.1008-5548.2024.04.005
收稿日期：2023-11-13，修回日期：2024-02-19，上线日期：2024-06-19。
基金项目：国家自然科学基金项目，编号：42207206；文昌 9-7 油田多分支复杂结构井固井方案及工作液体系研究，编号：CCL2022RCPS0702PSN；四川省科技厅自然科学基金面上项目，编号：24NSFSC1580。
第一作者简介：胡陈（1998—），男，硕士生，研究方向为纤维增强水泥。E-mail：1459553632@qq. com。
通信作者简介：
张春梅（1977—），女，副教授，博士，硕士生导师，研究方向为固井新材料研发。E-mail：200531010045@swpu. edu. cn；
程小伟（1977—），男，教授，博士，四川省学术和技术带头人，博士生导师，研究方向为先进胶凝材料及其在固井中应用。E-mail：chengxw@swpu. edu. cn。
摘要：【目的】 降低天然海泡石纤维的吸水性，提高海泡石纤维水泥浆的流动性能，改善水泥石的力学性能。【方法】 通过酸-水热法对天然海泡石纤维进行除杂提纯，并采用正硅酸乙酯（tetraethyl orthosilicate， TEOS）水解在海泡石纤维表面包覆二氧化硅降低海泡石纤维的吸水性，探究海泡石纤维对油井水泥的浆体性能、力学性能影响；运用X射线衍射分析、热分析和扫描电子显微镜分析等方法表征水泥石的物相组成、水化程度及微观形貌。【结果】 改性水泥的海泡石纤维最
优质量分数为 5%，固化 7 d的水泥石抗压、抗拉强度较未改性的分别提高了 10.98%、10.58%；海泡石纤维质量分数为5% 的改性水泥石的峰值应力为 35.76 MPa，峰值应变为 3.97×10-2 。海泡石纤维表面包覆 SiO2后，在较低质量分数下（5%）就能够促进水泥水化。【结论】 改性海泡石纤维水泥浆的流动性优于未改性的；在纤维掺量和养护时间相同的情况下，改性海泡石纤维水泥石的抗压强度和抗拉强度均高于未改性的；改性海泡石纤维对水泥石的增韧强化能力高于未改性海泡石纤维。
Objective Fiber reinforcement proves to be an effective approach in enhancing the mechanical properties of oil well cement.Sepiolite fibers， known for their remarkable dispersibility in cement slurry and strong bonding to the cement matrix， are promising candidates. However， the presence of high impurity levels and significant water absorption in natural sepiolite fibers not only hinder the fluidity of cement slurry but also compromise the compressive and tensile strengths of cement paste， thereby constraining the broader utilization of sepiolite fibers in cement-based materials. To overcome these challenges，this study employed a hydrochloric acid-hydrothermal purification method to refine natural sepiolite fibers， followed by surface coating with SiO2 using tetraethyl orthosilicate （TEOS）.The impact of modified sepiolite fibers on the properties of cement slurry，mechanical strength，and microstructure of oil well cement was systematically investigated. The findings and methodologies presented in this study offer valuable insights into harnessing sepiolite fibers in various applications involving cement-based materials.
Methods This study focused on the purification of natural sepiolite fibers using the HCl-hydrothermal method， followed by the coating of SiO2 on the purified sepiolite surface using TEOS to produce modified sepiolite fibers. Scanning electron microscopy （SEM） was employed to characterize both unmodified and modified sepiolite fibers. Subsequently， these fibers were separately incorporated into cement slurry to evaluate their impact on flowability and rheological properties. Additionally， the mechanical properties of the resulting cement paste， including compressive strength， tensile strength， and stress-strain curves， were examined to evaluate the influence of sepiolite fibers. The reinforcement mechanism of both unmodified and modified sepiolite fibers in oil well cement was analyzed using X-ray diffraction （XRD）， thermal analysis （TGA）， and SEM.
Results and Discussion Unmodified sepiolite fibers exhibited a needle-like， columnar morphology with a smooth surface， while modified sepiolite fibers displayed a thin film coating. Energy-dispersive X-ray spectroscopy （EDS） analysis revealed an increased Si content on the surface of the modified sepiolite fibers， indicating SiO2 attachment from the TEOS hydrolysis. The specific surface area of unmodified sepiolite fibers decreased from 4.518 m2 /g to 2.598 m2 /g after SiO2 coating， attributed to SiO2 forming in and filling the internal pores of the fibers. Cement slurry containing modified sepiolite fibers showed superior flowability with improved rheological properties compared to unmodified fibers. This improvement was attributed to the SiO2 coating reducing water absorption of the fiber， and weakening binding and adsorption of solvents by the bundled fiber structure of sepiolite， thus enhancing slurry flowability. At the same mass fraction of sepiolite fibers， cement-based material with modified fibers exhibited higher compressive and tensile strengths compared to those with unmodified fibers under identical curing times. Optimal mechanical properties were observed at 5% mass fraction of modified sepiolite fibers. After 7 days of curing， the compressive and tensile strengths of the modified sepiolite fiber cement-based material were 10.98% and 10.58% higher， respectively，than those of the unmodified sepiolite fiber cement slurry. The stress-strain curve from uniaxial compression demonstrated a significant increase in peak stress and strain of cement paste with sepiolite fiber addition， alongside a reduction in its elastic modulus. Specifically， at a 5% mass fraction of modified sepiolite fibers， the cement paste exhibited a peak stress of 35.76 MPa and a strain of 3.97×10-2 ， indicating significant reinforcing and toughening properties. The toughening and strengthening effects of modified sepiolite fibers on the cement paste exceeded those of unmodified fibers. Sepiolite fiber addition did not induce the formation of new phases in the cement paste. Unmodified fibers inhibited cement hydration， while a 5% mass fraction of modified fibers facilitated it. Microscopic morphology results showed improved adherence of modified fibers to hydration products， leading to enhanced bonding with the cement matrix. Modified sepiolite fibers improved cement paste toughness through mechanisms involving fiber fracture and pull-out.
Conclusion This study investigated the impact of SiO2-coated sepiolite fibers on the properties and mechanical characteristics of oil well cement slurry. The introduction of SiO2 coating onto the fiber surface effectively reduced water absorption and enhanced the flowability of cement slurry containing sepiolite fibers. Optimal performance was achieved with a 5% mass fraction of SiO2-coated sepiolite fibers， significantly enhancing the mechanical properties and toughness of oil well cement slurry. Furthermore,the interface bonding between SiO2-coated sepiolite fibers and the cement matrix was notably improved. The preparation process for SiO2-coated sepiolite fibers was found to be simple and compatible with cement slurry， offering valuable insights for their application in cement-based materials.
Keywords：sepiolite fiber； oil well cement； mechanical property； silica
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