1979年标准参考材料的认证:用于晶石尺寸分析的粉末衍射线形状标准
James P Cline1, Marcus H Mendenhall1, Joseph J Ritter1,2
1National Institute of Standards and Technology, Gaithersburg, MD 20899 USA.
概括
一个新的国家标准与技术研究所 (NIST) 标准参考材料 (SRM) 为氧化粉末提供了经过认证的晶石尺寸. 这种材料有助于分析粉末衍射线形状的扩展,以准确地表征纳米材料.
科学领域:
- 材料科学 材料科学 材料科学
- 晶体学 晶体学是指结晶学.
- 纳米技术纳米技术
背景情况:
- 粉末衍射对于确定晶石大小至关重要,但准确的分析需要可靠的标准.
- 在衍射模式中线形的扩大受晶体体大小,堆叠断层和微流线等因素的影响.
- 现有的结晶体尺寸分析方法在背景确定和依赖模型的解释方面可能会带来挑战.
研究的目的:
- 开发和认证标准参考材料 (SRM) 用于使用粉末衍射进行精确的晶石尺寸分析.
- 为方法验证提供具有明确特征的氧化 (ZnO) 粉末,具有明显的晶体体尺寸.
- 为了比较从模型独立的里叶变换方法和基本参数方法获得的晶体体尺寸结果.
主要方法:
- 开发了两种ZnO粉末,平均晶体体大小约为15nm和60nm.
- 在先进光子源使用高分辨率粉末衍光仪和实验室衍光仪收集数据.
- 采用修改后的两步配置程序来提取福里埃变换和分析衍射数据.
- 使用基本参数方法进行分析,并使用各种扩展模型.
主要成果:
- 该NIST SRM由两个ZnO粉末组成,呈现晶体尺寸分布和特有的衍射线扩展.
- 独立于模型的里叶变换分析产生了平均列长 (L面积和L体积).
- 基本参数方法的结果与富里叶变换结果一致,在L面积值方面发现了微小的差异.
结论:
- 开发的SRM提供了可靠的标准,通过粉末衍射来确定晶体的尺寸.
- 里叶变换和基本参数方法都对分析晶体体大小有效,后者产生经过认证的格子参数.
- 该SRM有助于提高纳米材料表征的准确性和可比性.
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