1.1 本实施规程描述了在俄歇电子光谱仪和某些类型的X射线光电子光谱仪（光谱仪分析区域）中，当该区域由电子能量分析仪的电子收集透镜和孔径系统定义时，确定对检测信号有贡献的样本区域的方法。本规程仅适用于由入射X射线束激发的样品面积大于分析仪观察到的样品面积的X射线光电子能谱仪，其中光电子在从样品到分析仪入口的无场区域中移动。这里描述的一些方法需要安装辅助电子枪，以在样本上产生可变能量的电子束（“电子枪方法”）。其他实验需要具有锐边的样品，例如覆盖有均匀清洁层（例如金（Au）或银（Ag））的晶片，并进行切割以获得长边（“锐边”）- 边缘方法”）。 1.2 建议将本实施规程作为一种有用的方法，用于确定分析仪在不同光谱仪操作条件下观察到的样本面积，验证样本和束对齐是否充分，以及表征电子能量分析仪的成像特性。 1.3 以国际单位制表示的数值应视为标准值。本标准不包括其他计量单位。 1.4 本标准并非旨在解决与其使用相关的所有安全问题（如有）。本标准的用户有责任在使用前制定适当的安全、健康和环境实践，并确定监管限制的适用性。 1.5 本国际标准是根据世界贸易组织技术性贸易壁垒（TBT）委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认标准化原则制定的。 ====意义和用途====== 5.1 俄歇电子能谱和X射线光电子能谱广泛用于材料的表面分析。本规程总结了确定产生检测信号的样本面积的方法( 一 )对于聚焦电子束可以在尺寸大于分析仪观察到的样本区域尺寸的区域上扫描的仪器，以及( b )通过使用具有锋利边缘的样品。 5.2 本规程旨在确定电子能量分析仪选定操作条件下的观察样本面积。观察到的样本面积取决于电子在能量分析之前是否延迟、分析仪通过能量或延迟率（如果电子在能量分析之前延迟）、选定狭缝或孔径的大小以及待测量的电子能量值。观察到的样本面积取决于这些选定的操作条件，也可能取决于样本相对于电子能量分析仪对准的充分性。 5.3 如果经常使用的样品材料具有横向不均匀性，且尺寸与分析仪观察到的样品区域尺寸相当，则可能需要知道观察到的样品区域随测量条件的变化，例如电子能量或分析仪通过能量。 5.4 本规程可提供有关特定操作条件下电子能量分析仪成像特性的有用信息。该信息有助于将分析仪性能与制造商规范进行比较。 5.5 分析仪观察到的区域形状和大小信息也可用于预测XPS实验中样品旋转时的信号强度，并评估样品操纵器的旋转轴。 5.6 本实践中所述方法的应用示例已发布 ( 1- 7. ) . 5. 5.7 有不同的方法来定义光谱仪分析区域。 ISO技术报告提供了在AES和XPS中由分析仪查看的横向分辨率、分析面积和样品面积的测定指南 ( 8. ) ，和ISO 18516:2006描述了测定AES和XPS横向分辨率的三种方法。Baer和Engelhard使用基板上定义良好的材料“点”来确定样本面积，该面积对“小面积”XPS测量的测量信号有贡献 ( 9 ) . 该面积可能是仅从仪器横向分辨率估计的面积的十倍。“边缘”或“尾部”区域的强度也可能高度依赖于透镜操作和样本对齐的充分性。Scheithauer描述了一种替代技术，其中使用不同直径的铂孔径来确定每个孔径外的“长尾”X射线对测量的铂光电子信号的贡献分数，与铂箔上的部分相比 ( 10 ) . 在商用XPS仪器上进行测试测量，该仪器具有聚焦X射线束和10μm的标称横向分辨率（根据20个位置之间的距离确定） %  和80 % 结果发现，为了将光电子信号降低到10μm，需要大约100μm和450μm的孔径 % 和1 %, 分别为最大值 ( 10 ) . 在权衡横向分辨率和可检测性时，有效分析区域的知识很重要。在扫描俄歇显微镜中，分析区域更多地取决于背散射电子的径向范围，而不是主束的半径 ( 11 , 12 , 13 ) .

1.1 This practice describes methods for determining the specimen area contributing to the detected signal in Auger electron spectrometers and some types of X-ray photoelectron spectrometers (spectrometer analysis area) when this area is defined by the electron collection lens and aperture system of the electron energy analyzer. The practice is applicable only to those X-ray photoelectron spectrometers in which the specimen area excited by the incident X-ray beam is larger than the specimen area viewed by the analyzer, in which the photoelectrons travel in a field-free region from the specimen to the analyzer entrance. Some of the methods described here require an auxiliary electron gun mounted to produce an electron beam of variable energy on the specimen (“electron-gun method”). Other experiments require a sample with a sharp edge, such as a wafer covered with a uniform clean layer (for example, gold (Au) or silver (Ag)) and cleaved to obtain a long side (“sharp-edge method”). 1.2 This practice is recommended as a useful means for determining the specimen area viewed by the analyzer for different conditions of spectrometer operation, for verifying adequate specimen and beam alignment, and for characterizing the imaging properties of the electron energy analyzer. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 5.1 Auger electron spectroscopy and X-ray photoelectron spectroscopy are used extensively for the surface analysis of materials. This practice summarizes methods for determining the specimen area contributing to the detected signal ( a ) for instruments in which a focused electron beam can be scanned over a region with dimensions greater than the dimensions of the specimen area viewed by the analyzer, and ( b ) by employing a sample with a sharp edge. 5.2 This practice is intended as a means for determining the observed specimen area for selected conditions of operation of the electron energy analyzer. The observed specimen area depends on whether or not the electrons are retarded before energy analysis, the analyzer pass energy or retarding ratio if the electrons are retarded before energy analysis, the size of selected slits or apertures, and the value of the electron energy to be measured. The observed specimen area depends on these selected conditions of operation and also can depend on the adequacy of alignment of the specimen with respect to the electron energy analyzer. 5.3 Any changes in the observed specimen area as a function of measurement conditions, for example, electron energy or analyzer pass energy, may need to be known if the specimen materials in regular use have lateral inhomogeneities with dimensions comparable to the dimensions of the specimen area viewed by the analyzer. 5.4 This practice can give useful information on the imaging properties of the electron energy analyzer for particular conditions of operation. This information can be helpful in comparing analyzer performance with manufacturer's specifications. 5.5 Information about the shape and size of the area viewed by the analyzer can also be employed to predict the signal intensity in XPS experiments when the sample is rotated and to assess the axis of rotation of the sample manipulator. 5.6 Examples of the application of the methods described in this practice have been published ( 1- 7 ) . 5 5.7 There are different ways to define the spectrometer analysis area. An ISO Technical Report provides guidance on determinations of lateral resolution, analysis area, and sample area viewed by the analyzer in AES and XPS ( 8 ) , and ISO 18516:2006 describes three methods for determination of lateral resolution in AES and XPS. Baer and Engelhard have used well-defined ‘dots’ of a material on a substrate to determine the area of a specimen contributing to the measured signal of a ‘small-area’ XPS measurement ( 9 ) . This area could be as much as ten times the area estimated simply from the lateral resolution of the instrument. The amount of intensity in ‘fringe’ or ‘tail’ regions could also be highly dependent on lens operation and the adequacy of specimen alignment. Scheithauer described an alternative technique in which Pt apertures of varying diameters were utilized to determine the fraction of ‘long-tail’ X-ray contributions outside each aperture on the measured Pt photoelectron signal compared to that on a Pt foil ( 10 ) . In test measurements on a commercial XPS instrument with a focused X-ray beam and a nominal lateral resolution of 10 μm (as determined from the distance between the positions for 20 %  and 80 % of maximum signal when scans were made across an edge), it was found that aperture diameters of about 100 μm and 450 μm were required to reduce the photoelectron signals to 10 % and 1 %, respectively, of the maximum value ( 10 ) . Knowledge of the effective analysis area is important when making tradeoffs between lateral resolution and detectability. In scanning Auger microscopy, the area of analysis is determined more by the radial extent of backscattered electrons than by the radius of the primary beam ( 11 , 12 , 13 ) .