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生料中粗颗粒XRD分析制样细度的确定 |
Determination of sample fineness for XRD analysis of coarse particles in raw meal |
投稿时间:2025-04-09 修订日期:2025-05-30 |
DOI: |
中文关键词: 生料 粗颗粒矿相 XRD 制粉细度 |
英文关键词: Raw meal Coarse grained mineral phase XRD Powder fineness |
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中文摘要: |
生料筛析试验后,对其筛上物研磨制粉进行XRD物相分析,是进一步得到生料中粗颗粒碳酸盐类或石英类矿相含量的关键步骤,而筛上物研磨制粉的细度水平对Rietveld全谱拟合定量分析结果会产生较大影响。本文对125μm和63μm筛析试验筛上物分别研磨至全部通过150μm、80μm和45μm进行XRD检测和Rietveld全谱拟合对比分析,发现仅研磨至全部通过150μm方孔筛时,所制得的粉体较粗,压片制样进行XRD检测时有明显的颗粒感,Rietveld全谱拟合收敛时的精修可靠性因子(RWP)大于8%,影响分析结果准确性;而研磨至全部通过80μm或45μm方孔筛时,RWP均低于8%,且筛上物研磨至全部通过45μm方孔筛时的RWP相对更低一些,但考虑研磨全部通过45μm方孔筛的制样效率较低,因此,筛析试验筛上物研磨至全部通过80μm方孔筛制备粉末样品用于XRD检测分析更为合适。 |
英文摘要: |
After the raw meal sieve analysis test, XRD phase analysis of the milled powder on the sieve is a key step in further obtaining the content of coarse carbonate or quartz mineral phases in the raw meal. The fineness level of the milled powder on the sieve has a significant impact on the quantitative analysis results of Rietveld full spectrum fitting. This article compares and analyzes the XRD detection and Rietveld full spectrum fitting of the 125 μ m and 63 μ m sieve samples that were ground to pass through 150 μ m, 80 μ m, and 45 μ m respectively. It was found that only when ground to pass through the 150 μ m square pore sieve, the resulting powder was coarser, and there was a significant particle feel when pressed for XRD detection. The refinement reliability factor (RWP) of Rietveld full spectrum fitting convergence was greater than 8%, which affected the accuracy of the analysis results; When ground to pass through either the 80 μ m or 45 μ m square sieve, the RWP is lower than 8%, and the RWP of the sieved material is relatively lower when ground to pass through the 45 μ m square sieve. However, considering the lower sample preparation efficiency of grinding all through the 45 μ m square sieve, it is more suitable to prepare powder samples for XRD detection and analysis by grinding the sieved material to pass through the 80 μ m square sieve. |
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