氧化石墨烯对多壁碳纳米管掺配水泥砂浆强度、压敏性能与微观结构的影响

杨森; 王远贵; 齐孟; 魏致强; 石家宜; 詹达富; 王琴; 袁小亚

doi:10.13801/j.cnki.fhclxb.20210716.005

氧化石墨烯对多壁碳纳米管掺配水泥砂浆强度、压敏性能与微观结构的影响

doi: 10.13801/j.cnki.fhclxb.20210716.005

杨森^1,,
王远贵^1,,
齐孟^2,,
魏致强^2,,
石家宜^1,,
詹达富^3,,
王琴³,
袁小亚^1, ,

1.
重庆交通大学　材料科学与工程学院，重庆 400074
2.
重庆交通大学　土木工程学院，重庆 400074
3.
北京交通大学　土木与交通工程学院，北京 100044

基金项目: 国家自然科学基金(51402030)；重庆市基础科学与前沿技术研究专项基金(cstc2017jcyjBX0028)；重庆市教育委员会科学技术研究项目(KJZD-K201800703)

详细信息

通讯作者:
袁小亚，博士，教授，硕士生导师，研究方向为纳米复合材料、建筑功能材料、高性能水泥混凝土等领域　E-mail：yuanxy@cqjtu.cn

中图分类号: TU528
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出版历程
- 收稿日期: 2021-05-28
- 修回日期: 2021-07-08
- 录用日期: 2021-07-09
- 网络出版日期: 2021-07-19
- 刊出日期: 2022-03-23

Effect of graphene oxide on mechanical properties, piezoresistivity and microstructure of cement mortar blended with multi-walled carbon nanotubes

YANG Sen^1
,,
WANG Yuangui^1
,,
QI Meng^2
,,
WEI Zhiqiang^2
,,
SHI Jiayi^1
,,
ZHAN Dafu^3
,,
WANG Qin³,
YUAN Xiaoya^{1
, ,}

1.
College of Materials Science and Engineering, Chongqing Jiaotong University, Chongqing 400074, China
2.
School of Civil Engineering, Chongqing Jiaotong University, Chongqing 400074, China
3.
School of Civil and Traffic Engineering, Beijing Jiaotong University, Beijing 100044, China

摘要

摘要: 多壁碳纳米管(MWCNTs)对水泥基材料可起到增强增韧的作用。但MWCNTs易在水泥浆体中团聚，目前国内外对如何深化氧化石墨烯(GO)在水泥浆体中分散MWCNTs的报道较为罕见。采用吸光度试验考察了木质素磺酸钠(MN)存在时，GO对MWCNTs在模拟水泥水化孔隙液的饱和氢氧化钙溶液(CH)中分散性能的影响，并研究了GO对MWCNTs掺配砂浆力学性能、电热性能、电阻率及压敏性的影响。吸光度测试表明MN、GO、MWCNTs质量比为3∶1∶9时，MWCNTs分散达到最佳，力学性能测试表明当MWCNTs、GO最佳掺量分别为0.45wt%、0.05wt%时，28天抗折抗压强度比相同MWCNTs掺量的试件分别提高了27.3%、20.9%，电阻率降低了18.2%，电阻变化率提高了72.6%。微观结构测试表明GO能进一步促进MWCNTs在水泥基材料中分散，促进水泥水化进程，密实了水泥石结构，对MWCNT掺配砂浆强度有协同增长作用，提高了压敏性能。本研究采用GO分散MWCNT的方法可扩展到其他碳基纳米增强剂，并为发展自感知智能化水泥基材料提供了一种新的途径。
- 碳纳米管 /
- 氧化石墨烯 /
- 分散 /
- 压敏性 /
- 力学性能
Abstract: Multi-walled carbon nanotubes (MWCNTs) can strengthen and toughen cement-based materials. However, MWCNTs tend to agglomerate in cement paste. Up to now, there are few reports about how to improve the dispersion of MWCNTs by graphene oxide (GO) in cement paste. The effect of GO on the dispersion of MWCNTs in saturated calcium hydroxide solution (CH) used for simulated cement pore solution in the presence of sodium lignosulfonate (MN) was investigated by absorbance test, and the effects of GO on the mechanical properties, electrothermal properties, resistivity and pressure sensitivity of mortars containing MWCNTs were studied. The absorbance test shows that when the mass ratio of MN, GO and MWCNTs is 3∶1∶9, the dispersion of MWCNTs reaches the best. The mechanical properties test shows that when the optimal contents of MWCNTs and GO are 0.45wt% and 0.05wt% by the cement mass respectively, the 28 days flexural and compressive strength of the specimens are increased by 27.3% and 20.9%, the resistivity is reduced by 18.2%, and the resistance change rate is increased by 72.6%. The microstructure test shows that GO could further promote the dispersion of MWCNTs in cement-based materials, accelerate the hydration process of cement, densify the structure of cement paste. The synergy of GO and MWCNT increases the mechanical and durability and self-sensing properties of the cement mortar. In this study, the method to disperse MWCNT assisted by GO can be further extended to other carbon-based nano-reinforcing agents, and provides a new way for the development of self-sensing and intelligent cement-based materials.
- carbon nanotube /
- graphene oxide /
- dispersion /
- piezoresistivity /
- mechanical properties

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图 1 四电极布置(左)及压敏性加载装置(右)

Figure 1. Four electrode arrangement (left) and pressure sensitive loading device (right)

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图 2 GO、MN、MWCNTs溶液的紫外可见吸收光谱

Figure 2. UV-visible absorption spectra of GO, MN, MWCNTs solutions

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图 3 MN含量对GO在饱和CH溶液中吸光度的影响

Figure 3. Effect of content of MN on the absorbance of GO in saturated CH solution

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图 4 不同GO溶液体系的Zeta电位图

Figure 4. Zeta potential diagram of different GO solutions

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图 5 GO掺量对MWCNTs在饱和CH溶液中吸光度的影响

Figure 5. Effect of GO content on the absorbance of MWCNTs in saturated CH solution

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图 6 不同GO/MWCNTs掺量的28天胶砂SEM图像：(a) Blank；(b) 0.45%MNCNTs/C；(c) 0.45%MWCNTs-GO/C；(d) 0.45%MWCNTs-MN/C；(e) 0.05%GO/C；(f) 0.05%GO-MN/C；(g) 0.45%MWCNTs-MN-GO/C

Figure 6. SEM images of mortars with different amounts of GO/MWCNTs for 28 days: (a) Blank; (b) 0.45%MNCNTs/C; (c) 0.45%MWCNTs-GO/C; (d) 0.45%MWCNTs-MN/C; (e) 0.05%GO/C; (f) 0.05%GO-MN/C; (g) 0.45%MWCNTs-MN-GO/C

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图 7 不同含量GO/MWCNTs的3天砂浆XRD图谱

Figure 7. XRD spectra of mortars with different amounts of GO/MWCNTs for 3 days ((a) Blank; (b) 0.045%MWCNTs/C; (c) 0.05%GO/C; (d) 0.045%MWCNTs-MN/C; (e) 0.05%GO-MN/C; (f) 0.045%MWCNTs-GO/C; (g) 0.045%MWCNTs-MN-GO/C)

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图 8 GO对MWCNTs掺配砂浆电阻率的影响

Figure 8. Influence of GO on the resistivity of the mortars blended MWCNTs

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图 9 GO掺量对MWCNTs掺配砂浆电热性能的影响

Figure 9. Effect of GO content on electrothermal property of mortar blended with MWCNTs

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图 10 不同掺量MWCNTs 的砂浆压敏曲线(a)、不同掺量GO对MWCNTs掺配砂浆压敏性的影响(b)

Figure 10. Piezoresistivity curves of mortar with different contents of MWCNTs (a), and effect of GO content on the piezoresistivity of cement mortar blended with MWCNTs (b)

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表 1 水泥物理性能

Table 1. Physical properties of the cement

Water requirement of normal consistency/%	Specific surface area/(m²·kg⁻¹)	Density/ (g·cm⁻³)	Setting time/ min		Flexural strength/ MPa		Compression strength/ MPa
Water requirement of normal consistency/%	Specific surface area/(m²·kg⁻¹)	Density/ (g·cm⁻³)	Initial	Final	3 days	28 days	3 days	28 days
27.8	351	3.15	136	224	5.1	6.3	25.6	43.4

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表 2 多壁碳纳米管(MWCNTs)性能指标

Table 2. Performance indicators of multi-walled carbon nanotubes (MWCNTs)

Purity/%	Length/μm	Specific surface area/(m²·g⁻¹)	Diameter/nm
98.5	~50	245	8-20

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表 3 含有不同含量木质素磺酸钠(MN)的饱和氢氧化钙(CH)溶液的配制

Table 3. Preparation of saturated calcium hydroxide solution (CH) with different contents of sodium lignosulfonate (MN)

Sample	Water/mL	Ca(OH)₂/g	PC/mL	GO/mL	MN^①/g
X1	90	0.16	0.05	10	0
X2	90	0.16	0.05	10	1∶1
X3	90	0.16	0.05	10	2∶1
X4	90	0.16	0.05	10	3∶1
X5	90	0.16	0.05	10	4∶1
X6	90	0.16	0.05	10	5∶1
Notes: ①—Content of MN is its ratio to GO; PC—Polycarboxylate; GO—Graphene oxide.

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表 4 用于Zeta电位测试的GO溶液组成

Table 4. Composition of GO solution for Zeta potential test

Sample	Water/mL	Ca(OH)₂/g	GO/mL	PC/mL	MN^①
Y1	90	0.16	10	0	0
Y2	90	0.16	10	0.05	0
Y3	90	0.16	10	0.05	1∶1
Y4	90	0.16	10	0.05	2∶1
Y5	90	0.16	10	0.05	3∶1
Y6	90	0.16	10	0.05	4∶1
Y7	90	0.16	10	0.05	5∶1
Note: ①—Content of MN is its mass ratio to GO.

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表 5 含有不同含量GO的饱和CH溶液的配制

Table 5. Preparation of saturated CH solution with different contents of GO

Sample	Water/mL	Ca(OH)₂/g	PC/mL	MWCNTs/g	MN^①	GO^②
Z1	100	0.16	0.05	0.01	0	0
Z2	100	0.16	0.05	0.01	3∶1	9∶1
Z3	100	0.16	0.05	0.01	3∶1	5∶1
Z4	100	0.16	0.05	0.01	3∶1	3∶1
Z5	100	0.16	0.05	0.01	3∶1	1∶1
Z6	100	0.16	0.05	0.01	3∶1	1∶3
Z7	100	0.16	0.05	0.01	3∶1	1∶5
Z8	100	0.16	0.05	0.01	3∶1	1∶9
Z9	100	0.16	0.05	0.01	0	1∶9
Z10	100	0.16	0.05	0.01	3∶1	0
Notes: ①—Content of MN is its mass ratio to GO; ②—Content of GO is its mass ratio to MWCNTs.

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表 6 不同GO掺量的水泥砂浆配合比

Table 6. Mix ratios of cement mortars with different contents of GO

Sample	MN^①/%	GO^①/%	MWCNTs^①/%	C/g	S/g	W/g	PC/g
Blank	0	0	0	450	1350	165	2.7
0.45%MWCNTs-GO/C	0	0.05	0.45	450	1350	165	2.7
0.45%MWCNTs-MN/C	0.15	0	0.45	450	1350	165	2.7
0.15%MN/C	0.15	0	0	450	1350	165	2.7
0.05%GO/C	0	0.05	0	450	1350	165	2.7
0.05%GO-MN/C	0.15	0.05	0	450	1350	165	2.7
0.09%MWCNTs-MN-GO/C	0.03	0.01	0.09	450	1350	165	2.7
0.27%MWCNTs-MN-GO/C	0.09	0.03	0.27	450	1350	165	2.7
0.45%MWCNTs-MN-GO/C	0.15	0.05	0.45	450	1350	165	2.7
0.63%MWCNTs-MN-GO/C	0.21	0.07	0.63	450	1350	165	2.7
0.81%MWCNTs-MN-GO/C	0.27	0.09	0.81	450	1350	165	2.7
0.09%MWCNTs/C	0	0	0.09	450	1350	165	2.7
0.27%MNCNTs/C	0	0	0.27	450	1350	165	2.7
0.45%MNCNTs/C	0	0	0.45	450	1350	165	2.7
0.63%MNCNTs/C	0	0	0.63	450	1350	165	2.7
0.81%MNCNTs/C	0	0	0.81	450	1350	165	2.7
Notes: ①—Mass ratio to cement; C—Cement; S—Sand; W—Water.

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表 7 GO含量对MWCNTs掺配胶砂抗折抗压强度的影响

Table 7. Effect of GO content on the flexural strength and compressive strength of mortar blended with MWCNTs

Sample	Flexural strength (MPa)/Increase rate (%)		Compressive strength (MPa)/Increase rate (%)
Sample	3 days	28 days	3 days	28 days
Blank	5.5/0	6.8/0	27.5/0	44.5/0
0.45%MWCNTs-GO/C^②	8.2/15.5	9.8/11.4	38.5/5.5	63.5/10.8
0.45%MWCNTs-MN/C^②	7.7/8.5	9.5/8.0	38.3/4.9	61.5/7.3
0.15%MN/C^①	5.1/−7.3	6.2/−8.8	25.3/−8.0	39.5/−11.2
0.05%GO/C^①	6.0/9.1	7.6/11.8	32.1/16.7	53.6/20.4
0.05%GO-MN/C^①	6.4/16.4	8.9/30.9	34.8/26.5	58.6/31.7
0.09%MWCNTs-MN-GO/C^②	6.5/12.1	7.8/6.8	34.4/21.1	55.8/15.1
0.27%MWCNTs-MN-GO/C^②	7.4/13.8	9.1/19.7	37.5/18.7	58.6/14.5
0.45%MWCNTs-MN-GO/C^②	8.5/19.7	11.2/27.3	42.5/16.4	69.3/20.9
0.63%MWCNTs-MN-GO/C^②	8.1/8.0	9.8/4.3	41.2/9.0	65.4/9.9
0.81%MWCNTs-MN-GO/C^②	6.4/4.9	8.2/5.1	32.1/7.7	54.1/9.7
0.09%MWCNTs/C^①	5.8/5.5	7.3/7.4	28.4/3.3	48.5/9.0
0.27%MNCNTs/C^①	6.5/18.2	7.6/11.8	31.6/14.9	51.2/15.1
0.45%MNCNTs/C^①	7.1/29.1	8.8/29.4	36.5/32.7	57.3/28.8
0.63%MNCNTs/C^①	7.6/38.2	9.4/38.2	37.8/37.5	59.5/33.7
0.81%MNCNTs/C^①	6.1/10.9	7.8/14.7	29.8/8.4	49.3/10.8
Notes: ①—Control group is blank; ②—Control group is 0.09%MWCNTs/C-0.81%MNCNTs/C respectively which contains the same MWCNTs content.

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