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材料导报  2019, Vol. 33 Issue (4): 644-649    https://doi.org/10.11896/cldb.201904015
  无机非金属及其复合材料 |
基于Rietveld/XRD(内标法)水泥浆体物相演变定量表征与非晶定量公式修正
赵丕琪,梁辰,孙传奎,刘红花,王守德,芦令超
济南大学山东省建筑材料制备与测试技术重点实验室,济南 250022
Quantitative Characterization for Phase Evolution of Cement Paste Based
on Rietveld/XRD (Internal Standard Method) and Correction Formula
for Amorphous Phase
ZHAO Piqi, LIANG Chen, SUN Chuankui, LIU Honghua, WANG Shoude, LU Lingchao
Shandong Provincial Key Laboratory of Preparation and Measurement of Building Materials, University of Jinan, Jinan 250022
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摘要 基于Rietveld/XRD精修方法,借助GSAS-EXPGUI软件,研究既定水化龄期普通硅酸盐水泥浆体物相组成的定量表征,并结合Ca(OH)2的热分析定量结果以及熟料矿物与自由水的量化匹配关系研究Rietveld定量结果的可靠性。研究结果表明,干燥水化样品中Ca(OH)2的Rietveld定量结果与热分析定量结果具有较好的一致性,当水化1 d、3 d、7 d和28 d龄期时,其绝对误差分别为1.2%、0.7%、0.3%和0.8%,且随着水化龄期的延长,样品的相对误差显著降低。结合水泥浆体物相演变的Rietveld定量表征发现,熟料矿物的消耗程度与自由水的消耗程度存在较好的线性相关性(相关系数R2=0.996),反映了其Rietveld定量表征具有较高的可靠性。在此过程中,提出了基于内标法改进型的非晶相定量公式,并建立了水泥浆体自由水与相应干燥样品化学结合水的数学关系。
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赵丕琪
梁辰
孙传奎
刘红花
王守德
芦令超
关键词:  Rietveld/XRD法  物相演变  水泥水化  定量分析    
Abstract: Based on Rietveld/XRD method, the quantitative characterization of the phase composition for ordinary Portland cement paste at a given hydration was investigated via GSAS-EXPGUI software, and the reliability of the quantitative results was further probed by combining with the thermal analysis of Ca(OH)2, as well as the quantitative matching relationship of clinker minerals and free water. The results indicated that the Rietveld quantitative results of Ca(OH)2 in dry hydration samples agreed well with that of the thermal analysis, their absolute errors were 1.2%,0.7%,0.3% and 0.8% when hydrated for 1 d, 3 d, 7 d and 28 d ages, respectively. Besides, the relative errors were significantly decreased with the increase of hydration age. It was found that there was a satisfactory linear correlation (correlation coefficient R2=0.996) between the degree of consumption of clinker minerals and free water, reflecting the high reliability of Rietveld quantitative characterization. In this process, an ameliorated amorphous phase quantitative formula based on the internal standard method was proposed, and the mathematical relationship between the free water of cement paste and the chemical bonding water of corresponding drying samples was established.
Key words:  Rietveld/XRD method    phase evolution    cement hydration    quantitative analysis
               出版日期:  2019-02-25      发布日期:  2019-03-11
ZTFLH:  TQ172  
基金资助: 国家自然科学基金(51602126);中国博士后科学基金(2017M622118);济南大学博士后/博士基金(XBH1716/XBS1661);济南大 学科技计划项目(XKY1730)
作者简介:  赵丕琪,济南大学,讲师。2015年7月毕业于同济大学,获得博士学位,主要从事水泥基材料制备与应用研究。
引用本文:    
赵丕琪, 梁辰, 孙传奎, 刘红花, 王守德, 芦令超. 基于Rietveld/XRD(内标法)水泥浆体物相演变定量表征与非晶定量公式修正[J]. 材料导报, 2019, 33(4): 644-649.
ZHAO Piqi, LIANG Chen, SUN Chuankui, LIU Honghua, WANG Shoude, LU Lingchao. Quantitative Characterization for Phase Evolution of Cement Paste Based
on Rietveld/XRD (Internal Standard Method) and Correction Formula
for Amorphous Phase. Materials Reports, 2019, 33(4): 644-649.
链接本文:  
http://www.mater-rep.com/CN/10.11896/cldb.201904015  或          http://www.mater-rep.com/CN/Y2019/V33/I4/644
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