少层石墨烯对水泥净浆流动性能及力学性能的影响

何威; 许吉航; 焦志男

doi:10.13801/j.cnki.fhclxb.20211112.001

少层石墨烯对水泥净浆流动性能及力学性能的影响

doi: 10.13801/j.cnki.fhclxb.20211112.001

何威^{1, 2, 3, ,},
许吉航^{1, 2, 3},
焦志男^{1, 2, 3}

1.
河北省土木工程绿色建造与智能运维重点实验室，秦皇岛 066004
2.
河北省建筑低碳清洁供热技术创新中心，秦皇岛 066004
3.
燕山大学　建筑工程与力学学院，秦皇岛 066004

基金项目: 国家自然科学基金(51578477)

详细信息

通讯作者:
何威，博士，教授，研究方向为水泥基复合材料　 E-mail：hewei@ysu.edu.cn

中图分类号: TB332
计量
- 文章访问数: 867
- HTML全文浏览量: 401
- PDF下载量: 44
- 被引次数: 0
出版历程
- 收稿日期: 2021-09-22
- 修回日期: 2021-10-27
- 录用日期: 2021-11-03
- 网络出版日期: 2021-11-15
- 刊出日期: 2022-11-01

Effect of few-layer graphene on the fluidity and mechanical properties of cement paste

HE Wei^{1, 2, 3
, ,},
XU Jihang^{1, 2, 3},
JIAO Zhinan^{1, 2, 3}

1.
Hebei Provincial Key Laboratory of Green Construction and Intelligent Operation in Civil Engineering, Qinhuangdao 066004, China
2.
Hebei Building Low-carbon Clean Heating Technology Innovation Center, Qinhuangdao 066004, China
3.
School of Civil Engineering and Mechanics, Yanshan University, Qinhuangdao 066004, China

摘要

摘要: 系统研究了少层石墨烯(FLG)对水泥净浆流动性能和力学性能(抗压强度和抗折强度)的影响，通过SEM、XRD、EDS剖析了FLG对净浆力学性能影响的作用机制。同时利用AFM、Raman、SEM等技术表征了FLG的层数和结构。结果表明：FLG的层数在3~6层，呈现六角型蜂窝结构，有层间堆叠现象。FLG的掺入能降低净浆的流动性，净浆3 天和28 天抗压强度分别提升了27.84%和13.52%，3 天和28天抗折强度分别提升了12.92%和19.68%。FLG具有模板效应，能够促进水泥水化产物的生长，改变水化晶体的形状、尺寸，使其有形成完整、致密的趋势，使净浆结构更加密实。
- 少层石墨烯 /
- 水泥净浆 /
- 流动性 /
- 力学性能 /
- 水化产物
Abstract: The effects of few-layer graphene (FLG) on the fluidity and mechanical properties (compressive strength and flexural strength) of cement paste were systematically studied. The mechanism of the effect of FLG on the mechanical properties of cement paste was analyzed by SEM, XRD and EDS. Meanwhile, the layers and structures of FLG were characterized by AFM, Raman and SEM techniques. The results show that the number of FLG layers is 3-6, showing a hexagonal honeycomb structure with interlayer stacking. The incorporation of FLG can reduce the fluidity of the paste. The 3 days and 28 days compressive strength values of the paste increase by 27.84% and 13.52%, respectively, and the 3 days and 28 days flexural strength values increase by 12.92% and 19.68%, respectively. The template effect of FLG can promote the growth of cement hydration products, change the shape and size of hydration crystals, and make it form a complete and dense trend, and make the paste structure more dense.
- few-layer graphene /
- cement paste /
- fluidity /
- mechanical properties /
- hydration products

HTML全文

图 1 少层石墨烯(FLG)模拟图 (a) 及外观 (b)

Figure 1. Simulation diagram (a) and appearance (b) of few-layer graphene (FLG)

下载: 全尺寸图片幻灯片

图 2 机械搅拌加超声分散制备FLG分散液

Figure 2. Preparation of FLG dispersion by mechanical agitation and ultrasonic dispersion

下载: 全尺寸图片幻灯片

图 3 FLG的微观形貌

Figure 3. Microstructure of FLG

下载: 全尺寸图片幻灯片

图 4 FLG的AFM相图

Figure 4. AFM phase diagram of FLG

下载: 全尺寸图片幻灯片

图 5 FLG高厚图

Figure 5. Height and thickness diagram of FLG

下载: 全尺寸图片幻灯片

图 6 FLG的Raman图谱

Figure 6. Raman spectrum of FLG

下载: 全尺寸图片幻灯片

图 7 FLG的XRD图谱

Figure 7. XRD pattern of FLG

下载: 全尺寸图片幻灯片

图 8 FLG的FTIR图谱

Figure 8. FTIR spectra of FLG

下载: 全尺寸图片幻灯片

图 9 FLG/PC扩展度随FLG掺量变化趋势

Figure 9. Variation trend of FLG/PC net slurry expansion with FLG content

下载: 全尺寸图片幻灯片

图 10 FLG/PC净浆3天和28天抗压强度随FLG掺量变化趋势

Figure 10. Variation trend of 3 days and 28 days compressive strength of FLG/PC net slurry with FLG content

下载: 全尺寸图片幻灯片

图 11 FLG/PC净浆3天和28天抗折强度随FLG掺量变化趋势

Figure 11. Variation trend of 3 days and 28 days flexural strength of FLG/PC net slurry with FLG content

下载: 全尺寸图片幻灯片

图 12 养护3天不同FLG掺量的FLG/PC净浆微观形貌

Figure 12. Microstructures of FLG/PC net slurry with different FLG contents after curing for 3 days

AFt—Ettringite; C-S-H—Calcium silicate hydrate

下载: 全尺寸图片幻灯片

图 13 养护28天不同FLG掺量的FLG/PC净浆微观形貌及水化产物的元素能谱图

Figure 13. Microstructures and elemental energy spectra of hydration products of FLG/PC net slurry with different FLG contents after curing for 28 days

下载: 全尺寸图片幻灯片

图 14 养护3天后不同FLG掺量的FLG/PC净浆XRD图谱

Figure 14. XRD patterns of FLG/PC net slurry with different FLG contents after curing for 3 days

CH—Calcium hydroxide; C₂S—Dicalcium silicate

下载: 全尺寸图片幻灯片

图 15 养护28天后不同FLG掺量的FLG/PC净浆XRD图谱

Figure 15. XRD patterns of FLG/PC net slurry with different FLG contents after curing for 28 days

下载: 全尺寸图片幻灯片

表 1 FLG参数

Table 1. Parameters of FLG

Type	Specific area/ (m²·g⁻¹)	Tap density/ (g·cm⁻³)	pH	Moisture/%	Mass fraction of carbon/wt%	Mass fraction of oxygen/wt%	Mass fraction of sulfur/wt%
FLG	458.55	0.022	7.10	0.54	≥98.0	＜1.0	＜0.1

下载: 导出CSV

表 2 P·O 42.5水泥化学分析结果

Table 2. Chemical analysis results of P·O 42.5 cement wt%

SiO₂	Al₂O₃	Fe₂O₃	CaO	MgO	SO₃	Na₂O	K₂O	Cl⁻	f-CaO	R₂O
21.47	7.17	3.11	60.04	2.90	2.77	0.11	0.70	0.024	0.57	0.57
Notes: f-CaO—Free calcium oxide; R₂O—Alkali oxides.

下载: 导出CSV

表 3 P·O 42.5水泥物理性能检测结果

Table 3. Physical performance test results of P·O 42.5 cement

Density/ (g·cm⁻³)	Degree of powder		Setting time			Stability	Flexural strength/MPa		Compressive strength/MPa
Density/ (g·cm⁻³)	Specific surface area/ (m²·kg⁻¹)	Screening allowance of 80 μm/%	Consistency/ %	Initial setting/ min	Final setting/ min	Ray type method/ mm	3 days	28 days	3 days	28 days
3.06	351	0.28	28.0	170	235	0.5	5.6	8.9	29.0	57.3

下载: 导出CSV

表 4 FLG/水泥(PC)净浆复合材料试件编号

Table 4. Specimen number of FLG/portland cement (PC) net slurry composite

Specimen	FLG content/wt%
0wt%FLG/PC	0.00
0.02wt%FLG/PC	0.02
0.04wt%FLG/PC	0.04
0.06wt%FLG/PC	0.06
0.08wt%FLG/PC	0.08
0.1wt%FLG/PC	0.10
0.5wt%FLG/PC	0.50
1wt%FLG/PC	1.00

下载: 导出CSV

表 5 养护28天FLG/PC净浆复合材料水化产物的元素组成及质量分数

Table 5. Elemental composition and mass fraction of hydration products of FLG/PCnet slurry composite after curing for 28 days

Element content/wt%	0wt%FLG/PC	0.04wt%FLG/PC	1wt%FLG/PC
C	8.17	13.04	6.70
O	50.74	51.77	43.84
Mg	0.36	0.69	0.47
Al	2.73	1.74	4.57
Si	7.89	7.80	10.51
S	1.71	1.21	1.50
K	1.02	1.66	1.95
Ca	27.38	22.09	30.46

下载: 导出CSV

参考文献(31)

[1]	LI V C. High-performance and multifunctional cement-based composite material[J]. Engineering,2019,5(2):250-260. doi: 10.1016/j.eng.2018.11.031
[2]	PEYVANDI A, SOROUSHIAN P, FARHADI N, et al. Evaluation of the reinforcement efficiency of low-cost graphite nanomaterials in high-performance concrete[J]. KSCE Journal of Civil Engineering,2018,22(10):3875-3882. doi: 10.1007/s12205-018-0168-6
[3]	FU C, XIE C Y, LIU J, et al. A comparative study on the effects of three nano-materials on the properties of cement-based composites[J]. Materials,2020,13(4):857. doi: 10.3390/ma13040857
[4]	SUMESH M, ALENGARAM U J, JUMAAT M Z, et al. Incorporation of nano-materials in cement composite and geopolymer based paste and mortar—A review[J]. Construction and Building Materials,2017,148:62-84. doi: 10.1016/j.conbuildmat.2017.04.206
[5]	HE W, JIAO Z N, WANG Y W, et al. Research on the mechanical properties and electrical conductivity of cement mortar based on recycled nano-iron boride[J]. Waste Disposal & Sustainable Energy,2021, 3(2):1-10.
[6]	PAUL S C, ROOYEN A V, VAN ZIJL G P A G, et al. Properties of cement-based composites using nanoparticles: A comprehensive review[J]. Construction and Building Materials,2018,189:1019-1034. doi: 10.1016/j.conbuildmat.2018.09.062
[7]	PAUL S C, VAN ROOYEN A S, VAN ZIJL G P A G, et al. Properties of cement-based composites using nanoparticles: A comprehensive review[J]. Construction and Building Materials, 2018, 189: 1019-1034.
[8]	SINGH L P, ALI A, TYAGI I, et al. Durability studies of nano-engineered fly ash concrete[J]. Construction and Building Materials,2019,194(10):205-215.
[9]	ALWASH D, KALFAT R, DU H J, et al. Development of a new nano modified cement based adhesive for FRP strengthened RC members[J]. Construction and Building Materials,2021,277(1):122318.
[10]	PAWEL S, MOHAMED A E, DIETMAR S. The influence of nanomaterials on the thermal resistance of cement-based composites—A review[J]. Nanomaterials,2018,8(7):465. doi: 10.3390/nano8070465
[11]	ZHAO Z, QI T, ZHOU W, et al. A review on the properties, reinforcing effects, and commercialization of nanomaterials for cement-based materials[J]. Nanotechnology Reviews,2020,9(1):303-322. doi: 10.1515/ntrev-2020-0023
[12]	PRASAD H, SITARAM N. Performance of nano materials for the strength development in concrete cube used as partial replacement for cement at different temperatures[J]. Materials Today: Proceedings,2021,45(6):7253-7258.
[13]	FAKHRY Z, SALMAN A J, ALQADHI R. Microstructural analysis for cement mortar with different nano materials[J]. Materials Science Forum,2020,1002:615-626. doi: 10.4028/www.scientific.net/MSF.1002.615
[14]	GEIM A K. Graphene: Status and prospects[J]. Science,2009,324(5934):1530-1534. doi: 10.1126/science.1158877
[15]	TAKAI K, TSUJIMURA S, KANG F, et al. Preparation of graphene[J]. Graphene,2020:39-171.
[16]	SEDAGHAT A, RAM M K, ZAYED A, et al. Investigation of physical properties of graphene-cement composite for structural applications[J]. Journal of Composite Materials,2014,4(1):12-21. doi: 10.4236/ojcm.2014.41002
[17]	CAO M L, ZHANG H X, ZHANG C. Effect of graphene on mechanical properties of cement mortars[J]. Journal of Central South University,2016,23(4):919-925. doi: 10.1007/s11771-016-3139-4
[18]	LI G, YUAN J B, ZHANG Y H, et al. Microstructure and mechanical performance of graphene reinforced cementitious composites[J]. Composites Part A: Applied Science and Manufacturing,2018,114:188-195. doi: 10.1016/j.compositesa.2018.08.026
[19]	DIMOV D, AMIT I, GORRIE O, et al. Ultrahigh perfor-mance nanoengineerd graphene-concrete composites for multifunctional applications[J]. Advanced Functional Materials,2018,28(23):1-12.
[20]	VEGA M D, VASQUEZ M. Plasma-functionalized exfoliated multilayered graphene as cement reinforcement[J]. Composites Part A: Applied Science and Manufacturing,2019,160:573-585. doi: 10.1016/j.compositesb.2018.12.055
[21]	KIM B, TAYLOR T, TROY A, et al. The effects of graphene oxide flakes on the mechanical properties of cement mortar[J]. Computers & Concrete,2018,21(3):261-267.
[22]	LEE S J, JEONG S H, KIM D U, et al. Effects of graphene oxide on pore structure and mechanical properties of cementitious composites[J]. Composite Structures,2020,234:111709. doi: 10.1016/j.compstruct.2019.111709
[23]	HO V D, NG C T, OZBAKKALOGLU T, et al. Investigating the reinforcing mechanism and optimized dosage of pristine graphene for enhancing mechanical strengths of cementitious composites[J]. RSC Advances,2020,10(70):42777-42789. doi: 10.1039/D0RA07639B
[24]	LIU J, FU J, YANG Y, et al. Study on dispersion, mechanical and microstructure properties of cement paste incorporating graphene sheets[J]. Construction and Building Materials, 2019, 199: 1-11.
[25]	LI H Y, DING S Q, ZHANG L Q, et al. Rheological behaviors of cement pastes with multi-layer graphene[J]. Construction and Building Materials, 2021, 269: 121327.
[26]	RAO C, SUBRAHMANYAM K S, MATTE H R, et al. Graphene: Synthesis, functionalization and properties[J]. Modern Physics Letters B,2011,25(7):427-451. doi: 10.1142/S0217984911025961
[27]	NOVOSELOV K S. Nobel lecture: Graphene: Materials in the flatland[J]. Reviews of Modern Physics,2011,83(3):837-849. doi: 10.1103/RevModPhys.83.837
[28]	中国国家标准化管理委员会. 混凝土外加剂匀质性试验方法: GB/T 8077—2000[S]. 北京: 中国标准出版社, 2000. Standardization Administration of the People's Republic of China. Test method for uniformity of concrete admixture: GB/T 8077—2000[S]. Beijing: Standards Press of China, 2000(in Chinese).
[29]	中国国家标准化管理委员会. 水泥胶砂强度检测方法: GB/T 17671—1999[S]. 北京: 中国标准出版社, 1999. Standardization Administration of the People's Republic of China. Cement mortar strength testing method: GB/T 17671—1999[S]. Beijing: Standards Press of China, 1999(in Chinese).
[30]	SILVA D L, CAMPOS J L E, FERNANDES T F D, et al. Raman spectroscopy analysis of number of layers in mass-produced graphene flakes[J]. Carbon,2020,161:181-189. doi: 10.1016/j.carbon.2020.01.050
[31]	HE Y J, ZHAO X G, LU L N, et al. Effect of C/S ratio on morphology and structure of hydrothermally synthesized calcium silicate hydrate[J]. Journal of Wuhan University of Technology,2011,26(4):770-773. doi: 10.1007/s11595-011-0308-z