煅烧硅灰石粉对硫氧镁水泥力学性能的影响

李知俊; 胡智淇; 关岩; 毕万利

doi:10.13801/j.cnki.fhclxb.20230511.004

煅烧硅灰石粉对硫氧镁水泥力学性能的影响

doi: 10.13801/j.cnki.fhclxb.20230511.004

1.
辽宁科技大学　土木工程学院，鞍山 114051
2.
大连理工大学　建设工程学部，大连 116081
3.
辽宁科技大学　材料与冶金学院，鞍山 114051

基金项目: 国家重点研发计划(2020YFC1909304)

详细信息

通讯作者:
关岩，硕士，副教授，硕士生导师，研究方向为新型镁质胶凝材料　E-mail: 15841293909@163.com

中图分类号: TU525.9；TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2023-03-08
- 修回日期: 2023-04-19
- 录用日期: 2023-05-06
- 网络出版日期: 2023-05-12
- 刊出日期: 2024-01-01

Effect of calcined wollastonite powder on mechanical properties of magnesium sulfade cement

LI Zhijun¹,
HU Zhiqi²,
GUAN Yan^{3
, ,},
BI Wanli³

1.
School of Civil Engineering, Liaoning University of Science and Technology, Anshan 114051, China
2.
Department of Construction Engineering, Dalian University of Technology, Dalian 116081, China
3.
School of Materials and Metallurgy, Liaoning University of Science and Technology, Anshan 114051, China

Funds: National Key R&D Plan of China (2020YFC1909304)

摘要

摘要: 为增强硫氧镁水泥(MOS)的力学性能，本文以煅烧前后硅灰石粉末(WS)作为外掺料，研究了其对 MOS 力学性能的影响，并利用DSC-TG、XRD、FTIR、NMR、SEM、压汞法(MIP)对煅烧前后(1000℃)的硅灰石粉和 WS/MOS 混合体系进行分析。试验表明，煅烧可以激发硅灰石粉中²⁹Si的水化活性，并且煅烧后的硅灰石粉在镁碱环境中可以激发其水化活性导致WS/MOS复合材料的性能更优。硅灰石能增强MOS的力学性能，同时煅烧后的硅灰石粉对WS/MOS复合体系强度的增幅更明显，当煅烧后WS掺量为20wt%时，MOS 28天的抗折强度和抗压强度达到最大值，分别为11.4 MPa和63.4 MPa，增量可达71.4%和21.2%。WS优化了MOS孔隙结构，降低了MOS大于100 nm的孔的比例，煅烧后的WS与MOS具有良好的界面相容性，更有利于MOS的力学性能的提升。
- 硅灰石 /
- 煅烧 /
- MOS /
- 力学性能 /
- 微观结构
Abstract: To enhance the mechanical properties of magnesium oxysulfade (MOS) cement, wollastonite powder (WS) was utilized as an additive before and after calcination to study its effect on the mechanical properties of MOS. The WS and WS/MOS composite system before and after calcination (1000℃) were analyzed by DSC-TG, XRD, FTIR, NMR, SEM, and mercury intrusion porosimetry (MIP). The results show that calcination stimulates the hydration activity of ²⁹Si in WS, and the calcined WS stimulates its hydration activity in magnesium alkali environment, resulting in better performance of WS/MOS composite materials. WS enhances the mechanical properties of MOS, and the strength of WS/MOS composite system with the calcined WS increases more significantly. The bending strength and compressive strength of MOS on the 28 days reach their maximum values when the after calcination WS content is 20wt%, which are 11.4 MPa and 63.4 MPa, respectively, with increments of 71.4% and 21.2%. WS optimizes the pore structure and reduces the proportion of pores larger than 100 nm in MOS. The calcined WS has good interface compatibility with MOS, which is more conducive to improving the mechanical properties of MOS.
- wollastonite /
- calcination /
- MOS /
- mechanical properties /
- microstructure

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图 1 LBM 和 WS 的粒度分布

Figure 1. Partical size distribution of LBM and WS

D₁₀, D₅₀, D₉₀—Volume content of particles less than this size accounts for 10%, 50%, 90% of all particles; dV/dlgD—Differential statistics of particle size distribution

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图 2 WS的TG和DSC曲线

Figure 2. TG and DSC curves of WS

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图 3 煅烧前后WS的SEM图像

Figure 3. SEM images of WS before and after calcination

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图 4 煅烧前后WS及煅烧后浸水20天的WS的XRD图谱

Figure 4. XRD patterns of WS before and after calcination and soaking in water after WS calcination for 20 days

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图 5 煅烧后WS浸水及煅烧后的WS和MgO共混后浸水的FTIR图谱

Figure 5. FTIR spectra of calcined WS immersed in water and calcined WS mixed with MgO immersed in water

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图 6 煅烧后WS浸水及煅烧后WS和MgO共混后浸水的NMR图谱

Figure 6. NMR spectra of calcined WS immersed in water and the mixture of calcined WS and MgO immersed in water

Q₃(1Mg)—(SiO)₃-MgO; Q₂(2Mg)—(SiO)₂-(MgO)₂; Q₁(3Mg)—SiO-(MgO)₃; f₁—Chemical shift

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图 7 各组试样不同龄期的抗压强度

Figure 7. Compressive strength of each group of samples at different ages

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图 8 各组试样养护28天后的抗折强度

Figure 8. Flexural strength of each sample after 28 days of curing

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图 9 各组试样养护28天的XRD图谱

Figure 9. XRD patterns of each group of samples cured for 28 days

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图 10 养护28天的 WS/MOS复合体系孔结构的压汞法(MIP)测试

Figure 10. Mercury intrusion porosimetry (MIP) test of the pore structure of WS/MOS composite system cured for 28 days

−dV/dlgdD—Differential statistics of aperture distribution

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图 11 ((a)~(d)) 20%CW/MOS和20%CY/MOS养护28天后的SEM图像；(e) 20%CY/MOS养护28天后的EDS图谱

Figure 11. ((a)-(d)) SEM images of 20%CW/MOS and 20%CY/MOS cured for 28 days; (e) EDS spectrum of 20%CY/MOS cured for 28 days

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图 12 利用SEM观察20%CW/MOS和20%CY/MOS养护28天后的EDS图谱

Figure 12. Observation of EDS spectra of 20%CW/MOS and 20%CY/MOS cured for 28 days using SEM

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表 1 轻烧氧化镁粉(LBM)和硅灰石粉(WS)的化学组成

Table 1. Chemical composition of light burned magnesium oxide powder (LBM) and wollastonite (WS)

Component	MgO/wt%	SiO₂/wt%	CaO/wt%	Fe₂O₃/wt%	Al₂O₃/wt%	Others/wt%
LBM	83.66	7.15	1.25	0.47	0.69	6.78
WS	1.11	51.34	45.74	0.28	0.59	0.94

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表 2 试验配比

Table 2. Test ratio

Sample	Molar ratio		CA content/ wt%	WS content/ wt%
Sample	n(α-MgO)∶n(MgSO₄)	n(H₂O)∶n(MgSO₄ )	CA content/ wt%	WS content/ wt%
0%WS/MOS	8	20	0.3	—
5%CW/MOS	8	20	0.3	5
10%CW/MOS	8	20	0.3	10
15%CW/MOS	8	20	0.3	15
20%CW/MOS	8	20	0.3	20
25%CW/MOS	8	20	0.3	25
30%CW/MOS	8	20	0.3	30
5%CY/MOS	8	20	0.3	5
10%CY/MOS	8	20	0.3	10
15%CY/MOS	8	20	0.3	15
20%CY/MOS	8	20	0.3	20
25%CY/MOS	8	20	0.3	25
30%CY/MOS	8	20	0.3	30
Notes: CW—WS not calcined; CA—Citric acid; CY—WS calcined at 1000℃ for 2 h; MOS—Magnesium oxysulfade.

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表 3 WS/MOS 养护至 28天的孔径分布

Table 3. Pore size distribution of WS/MOS cured to 28 days

Sample	Total intruded volume/ (mL·g⁻¹)	Total porosity/%	Volume of pore in each range/%
Sample	Total intruded volume/ (mL·g⁻¹)	Total porosity/%	>100 nm	10-100 nm	<10 nm
0%WS/MOS	0.1294	12.9132	34.63	64.05	1.32
10%CW/MOS	0.1220	12.2003	28.88	68.54	2.58
20%CW/MOS	0.1285	12.8457	23.49	75.04	1.47
10%CY/MOS	0.1100	11.0001	26.05	71.02	2.93
20%CY/MOS	0.1101	11.0141	18.46	79.63	1.91

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