蒸养条件对电解锰渣水泥胶砂力学性能与微观形貌的影响

付勇; 乔宏霞; 冯琼; 薛翠真; 李言奇; 贾振宇

蒸养条件对电解锰渣水泥胶砂力学性能与微观形貌的影响

付勇^{1, 2},
乔宏霞^{1, 2, ,},
冯琼^{1, 2},
薛翠真^{1, 2},
李言奇^{1, 2},
贾振宇^{1, 2}

1.
兰州理工大学土木工程学院, 兰州 730050
2.
甘肃省先进土木工程材料工程研究中心, 兰州 730050

基金项目: 国家自然科学基金(U21 A20150；52178216)；国家自然科学基金青年基金(52008196；52108219)；甘肃省科技计划资助(23 JRRA799; 23 JRRA813)；重庆市科技局重点项目(cstc2021 jscx-jbgs0029)

详细信息

通讯作者:
乔宏霞，博士，教授，博士生导师，研究方向为固废资源化利用　E-mail: qiaohongxia@lut.edu.cn

中图分类号: TU528
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- 文章访问数: 101
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- 被引次数: 0
出版历程
- 收稿日期: 2024-01-24
- 修回日期: 2024-02-28
- 录用日期: 2024-03-07
- 网络出版日期: 2024-04-16
- 刊出日期: 2024-12-15

Effect of steam curing conditions on mechanical properties and microstructure of electrolytic manganese residue cement mortar

FU Yong^{1, 2},
QIAO Hongxia^{1, 2
, ,},
FENG Qiong^{1, 2},
XUE Cuizhen^{1, 2},
LI Yanqi^{1, 2},
JIA Zhenyu^{1, 2}

1.
School of Civil Engineering, Lanzhou University of Technology, Lanzhou 730050, China
2.
Gansu Advanced Civil Engineering Materials Engineering Research Center, Lanzhou 730050, China

Funds: National Natural Science Foundation of China (U21 A20150; 52178216)；Youth Fund of the National Natural Science Foundation of China (52008196; 52108219)；Gansu Provincial Science and Technology Programme Grants (23 JRRA799; 23 JRRA813)；Key projects of Chongqing Science and Technology Bureau(cstc2021 jscx-jbgs0029)

摘要

摘要: 研究了不同煅烧温度(200℃和800℃)电解锰渣(EMR)火山灰活性及掺入0wt%、10wt%、20wt% EMR水泥胶砂在80℃蒸养7 h、7 d和标准养护3 d、28 d条件下力学性能、水化产物与孔隙特征分布。采用低场核磁共振技术、XRD定量表征及SEM微观形貌共同揭示了EMR对水泥胶砂的水化产物、孔径分布及孔隙率等影响规律，并探究了不同养护条件对EMR水泥胶砂水化进程的影响。结果表明：800℃煅烧EMR火山灰活性明显高于200℃煅烧火山灰活性，当800℃煅烧EMR替代量为10wt%时，初凝、终凝时间和标准稠度用水量分别为对照组的1.52、1.06和1.05倍，而蒸养7 h、7 d抗压强度分别高于标养3 d和28 d抗压强度，而抗折强度仅仅在蒸养7 d时高于对照组17.3%；纯水泥胶砂的水化产物主要为纤维状C-S-H和片状CH，而EMR水泥胶砂中由于硫酸盐含量较高，除了上述水化产物之外，在蒸养或标养条件下均可观察到石膏相与针棒状AFt的存在，标准养护28d时，CH、AFt和无定性含量分别为14.50%、11.75%和46.25%，与蒸养7 d衍射峰基本相似。另外，蒸养7 h与标准养护3 d对比孔隙率减少1.44%，蒸养7 d与标准养护28 d对比孔隙率减少0.06%。综上，蒸养可以提高800℃煅烧EMR火山灰活性，同时还可以加速EMR水泥胶砂的水化进程和细化其内部孔结构，进而提高了胶砂的力学性能。
- 电解锰渣 /
- 火山灰活性 /
- 蒸养 /
- 水化产物
Abstract: The pozzolanic activity of electrolytic manganese residue (EMR) at different calcination temperatures (200℃ and 800℃), and the distribution of mechanical properties, hydration products, and pore characteristics of cement mortar with 0wt%, 10wt% and 20wt% EMR, subjected to 80℃ steam curing for 7 h and 7 d, as well as standard curing for 3 d and 28 d, were studied. The effects of EMR on the hydration products, pore size distribution and porosity of cement mortar were revealed by low field nuclear magnetic resonance technology, XRD quantitative characterization and SEM microstructure. The effects of different curing conditions on the hydration process of EMR cement mortar were also investigated. The results show that the pozzolanic activity of EMR calcined at 800℃ is significantly higher than that of EMR calcined at 200℃. When the substitution amount of EMR calcined at 800℃ is 10%, the initial setting time, final setting time and water requirement of normal consistency are 1.52, 1.06 and 1.05 times that of the control group, respectively. The compressive strength of steam-cured 7 h and 7 d is higher than that of standard-cured 3 d and 28 d, respectively, while the flexural strength is only 17.3% higher than that of the control group at 7 d. The hydration products of pure cement mortar are mainly fibrous C-S-H and sheet-like CH, while in EMR cement mortar, due to the high sulfate content, in addition to the above hydration products, the presence of gypsum phase and needle shaped AFt can be observed under steam curing or standard curing conditions. The CH, AFt and amorphous contents are 14.50%, 11.75% and 46.25% after 28 days of standard curing. These values are similar to the diffraction peaks after 7 days of steam curing. In addition, the porosity of steam-cured 7 h is 1.44% lower than that of standard curing 3 d, and the porosity of steam-cured 7 d is 0.06% lower than that of standard curing 28 d. In summary, steam curing can improve the pozzolanic activity of EMR calcined at 800℃, accelerate the hydration process, and refine the internal pore structure, thereby improving the mechanical properties of the mortar.
- electrolytic manganese residue /
- pozzolanic activity /
- steam curing /
- hydration products

HTML全文

图 1 EMR的微观形貌

Figure 1. Microscopic morphology of EMR

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图 2 EMR的物相分析

Figure 2. Physical phase analysis by EMR

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图 3 OPC和EMR的粒径分布

Figure 3. Particle size distribution of OPC and EMR

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图 4 OPC和EMR的傅里叶红外光谱

Figure 4. Fourier infrared spectra of OPC and EMR

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图 5 纯水泥浆体与EMR水泥浆体工作性能：(a)凝结时间；(b)标准稠度用水量与体积安定性

Figure 5. Working performance of pure cement paste and EMR cement paste: (a) Setting time; (b) Water requirement of normal consistency and Soundness

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图 6 EMR水泥胶砂抗压强度：(a)10%；(b)20%

Figure 6. EMR cement mortar compressive strength: (a)10%; (b)20%

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图 7 EMR水泥胶砂抗折强度：(a)10%；(b)20%

Figure 7. EMR cement mortar flexural strength: (a)10%; (b)20%

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图 8 EMR²⁰⁰和EMR⁸⁰⁰ 在40℃下固化8 d后的Frattini结果

Figure 8. Frattini results of EMR²⁰⁰ and EMR⁸⁰⁰ cured at 40℃ for 8 d

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图 9 EMR²⁰⁰和EMR⁸⁰⁰ 的Frattini试验与SAI试验相关性

Figure 9. Correlation between Frattini test and SAI test for EMR²⁰⁰ and EMR⁸⁰⁰

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图 10 EMR²⁰⁰和EMR⁸⁰⁰在40℃的密封塑料瓶中养护1、3、7和28 d: (a)SL消耗试验，(b)SL消耗试验与Frattini试验相关性，(c) SL消耗试验与28 d SAI之间的相关性

Figure 10. EMR²⁰⁰ and EMR⁸⁰⁰ are cured in sealed plastic bottles at 40℃ for 1,3,7 and 28 days: (a)SL consumption test, (b)correlation between SL consumption test and Frattini test, (c)correlation between SL consumption test and 28 d SAI

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图 11 蒸养7 h后E-0组试件的微观形貌和EDS能谱

Figure 11. Microstructure and EDS energy spectrum of E-0 group specimens after steam curing for 7 h

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图 12 蒸养7 h 后E²⁰⁰-10组试件的微观形貌和EDS能谱

Figure 12. Microstructure and EDS energy spectrum of E²⁰⁰-10 group specimens after steam curing for 7 h

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图 13 蒸养7 h后E⁸⁰⁰-10组试件的微观形貌和EDS能谱

Figure 13. Microstructure and EDS energy spectrum of E⁸⁰⁰-10 group specimens after steam curing for 7 h

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图 14 蒸养7 d 后E-0组试件的微观形貌和EDS能谱

Figure 14. Microstructure and EDS energy spectrum of E-0 group specimens after steam curing for 7 d

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图 15 蒸养7 d 后E²⁰⁰-10组试件的微观形貌和EDS能谱

Figure 15. Microstructure and EDS energy spectrum of E²⁰⁰-0 group specimens after steam curing for 7 d

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图 16 蒸养7 d 后E⁸⁰⁰-10组试件的微观形貌和EDS能谱

Figure 16. Microstructure and EDS energy spectrum of E⁸⁰⁰-0 group specimens after steam curing for 7 d

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图 17 标养28 d纯水泥胶砂E-0的水化产物

Figure 17. Hydration products of 28 d standard curing pure cement mortar E-0

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图 18 标养28 d后E²⁰⁰-10的水化产物

Figure 18. Hydration products of E²⁰⁰-10 after 28 d of standard curin

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图 19 标养28 d后E⁸⁰⁰-10的水化产物

Figure 19. Hydration products of E⁸⁰⁰-10 after 28 d of standard curing

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图 20 不同养护条件下纯水泥胶砂与EMR水泥胶砂的XRD图谱

Figure 20. XRD patterns of pure cement mortar and EMR cement mortar under different curing conditions

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图 21 标准养护28 d条件下纯水泥胶砂与EMR水泥胶砂

Figure 21. Pure cement mortar and EMR cement mortar under standard curing for 28 days

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图 22 不同养护条件下纯水泥胶砂与EMR水泥胶砂T₂图谱：(a)E-0；(b)E²⁰⁰-10；(c) E²⁰⁰-20；(d) E⁸⁰⁰-10；(e) E⁸⁰⁰-20；(f)孔隙率

Figure 22. T₂ spectra of pure cement mortar and EMR cement mortar under different curing conditions: (a)E-0; (b)E²⁰⁰-10; (c) E²⁰⁰-20; (d) E⁸⁰⁰-10; (e)E⁸⁰⁰-20; (f) Porosity

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表 1 普通硅酸盐水泥(OPC)和电解锰渣(EMR)的化学组成

Table 1. Chemical composition of ordinary portland cement (OPC) and electrolytic manganese residue (EMR) wt%

Material	Al₂O₃	SiO₂	Fe₂O₃	CaO	SO₃	MgO	Other
OPC	6.57	19.34	3.22	47.95	1.23	1.58	4.06
EMR²⁰⁰	11.85	39.72	5.92	10.07	24.47	1.22	6.75
EMR⁸⁰⁰	10.79	37.03	6.66	12.29	24.60	1.24	7.21

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表 2 EMR水泥胶砂的配比与养护条件

Table 2. Proportioning and curing conditions of EMR cement mortar

Sample	OPC/ g	EMR/ g	Sand/ g	Water/ g	Curing condition
E-0	450	0	1350	225	80℃ steam curing for 7 h (S7 h) 80℃ steam curing for 7 d (S7 d) Standard curing 3 d (N3 d), Standard curing 28 d (N28 d)
E²⁰⁰-10	405	45	1350	225
E²⁰⁰-20	360	90	1350	225
E⁸⁰⁰-10	405	45	1350	225
E⁸⁰⁰-20	360	90	1350	225
Notes: “E-0”indicates control specimen; E²⁰⁰-10, where “E²⁰⁰” indicates an EMR calcination temperature of 200℃, “10” indicates an EMR substitution rate of 10 %, and other similar specimens.

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表 3 EMR²⁰⁰和EMR⁸⁰⁰在8 d时Frattini测试结果

Table 3. Frattini test results of EMR²⁰⁰ and EMR⁸⁰⁰ at 8 d

Material	[OH] mmol/L	[CaO] mmol/L	Theoretical max. [CaO] mmol/L	[CaO] reduction%
Sand	52.8	9.68	9.25	−4.4
EMR²⁰⁰	58.9	6.34	7.97	20.45
EMR⁸⁰⁰	54.0	6.30	8.79	28.3

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