不同参数优化对ZSM-5分子筛的扫描电子显微镜图像影响

王馨楠; 高占明

doi:10.16495/j.1006-3757.2023.02.011

不同参数优化对ZSM-5分子筛的扫描电子显微镜图像影响

doi: 10.16495/j.1006-3757.2023.02.011

大连理工大学化工学院分析测试中心，辽宁大连　116024

详细信息

作者简介:
王馨楠（1985−），女，工程师，主要从事微观材料的扫描电子显微镜表征与能谱分析研究，E-mail：wangxinnan@dlut.edu.cn

中图分类号: O657; O762
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- 文章访问数: 45
- HTML全文浏览量: 10
- PDF下载量: 8
- 被引次数: 0
出版历程
- 收稿日期: 2023-02-03
- 录用日期: 2023-04-10
- 修回日期: 2023-04-10
- 刊出日期: 2023-06-30

Effect of Different Parameters of Scanning Electron Microscopic Images of ZSM-5 Zeolite

Analysis & Research Center of the School of Chemical Engineering, Dalian University of Technology, Dalian 116024, Liaoning China

摘要

摘要: 扫描电子显微镜是一种常用的表征工具，可直观观察样品表面微观形貌. 由于分子筛样品中的硅铝成分而造成的二次电子产率低、耐电子束程度差、导电性不佳等特性，采用扫描电子显微镜进行形貌表征时会出现信号弱、荷电效应、表面细微结构损失等问题. 扫描电子显微镜表征时，加速电压、束斑尺寸、工作距离等是普遍的调节参数. 通过优化上述参数，对ZSM-5分子筛的扫描电子显微镜成像质量进行研究. 结果表明，低加速电压、束斑尺寸为3.0、工作距离小于5 mm时，对样品测试即可获得高质量扫描电子显微镜图像. 对比发现，镀膜后成像质量反而变差.
- 扫描电子显微镜 /
- ZSM-5分子筛 /
- 加速电压 /
- 束斑 /
- 工作距离
Abstract: Scanning electron microscopy (SEM) is a common tool for the visual characterization of the microstructural morphology of the surface of samples. However, for zeolite samples, due to the low secondary electron yield, poor resistance to electron beams and bad conductivity, etc. caused by the silica and alumina components. The problems such as weak signal, charge effect, small loss of surface structure, and so on often emerge at the performance of SEM characterization of zeolite. The accelerating voltage, spot size, work distance etc. are the common adjustment parameters. By optimizing the above parameters, the SEM image quality of ZSM-5 zeolite was studies. The results showed that high quality scanning electron microscopic images can be obtained for sample testing at a low accelerating voltage, a spot size of 3.0 and a work distance of less than 5 mm. The contrast showed that the SEM images of ZSM-5 zeolite were the worst after coating platinum on the sample.
- SEM /
- ZSM-5 zeolite /
- acceleration voltage /
- spot size /
- work distance

HTML全文

图 1 样品1、2、3的X射线衍射图谱

Figure 1. X-Ray diffraction patterns of Sample 1, 2, 3

下载: 全尺寸图片幻灯片

图 2 样品1在不同加速电压下的扫描电子显微镜图像

（a）1 kV，（b）2 kV，（c）3 kV，（d）5 kV，（e）10 kV

Figure 2. Images of scanning electron microscope (SEM) of Sample 1 with different acceleration voltages

(a) 1 kV, (b) 2 kV, (c) 3 kV, (d) 5 kV, (e) 10 kV

下载: 全尺寸图片幻灯片

图 3 样品2在不同加速电压下的扫描电子显微镜图像

（a）1 kV，（b）2 kV，（c）3 kV，（d）5 kV，（e）10 kV

Figure 3. SEM images of Sample 2 with different acceleration voltages

(a) 1 kV, (b) 2 kV, (c) 3 kV, (d) 5 kV, (e) 10 kV

下载: 全尺寸图片幻灯片

图 4 样品3在不同束斑尺寸下的扫描电子显微镜图像

（a）2.0，（b）3.0，（c）4.0，（d）5.0

Figure 4. SEM images of Sample 3 with different spot sizes

(a) 2.0, (b) 3.0, (c) 4.0, (d) 5.0

下载: 全尺寸图片幻灯片

图 5 样品3在不同工作距离下的扫描电子显微镜图像

（a）3.6 mm，（b）8.6 mm

Figure 5. SEM images of Sample 3 with different work distances

(a) 3.6 mm, (b) 8.6 mm

下载: 全尺寸图片幻灯片

图 6 样品3在1 kV下（a）镀膜前（b）镀膜后的扫描电子显微镜图像

Figure 6. SEM images of Sample 3 (a) before and (b) after platinum coating with acceleration voltage of 1 kV

下载: 全尺寸图片幻灯片

参考文献(19)

[1]	王占琴, 祁桂红, 张银光. X射线荧光光谱法测定不同类型分子筛中氧化物的含量[J]. 分析测试技术与仪器,2009,15(2):118-123 doi: 10.3969/j.issn.1006-3757.2009.02.011 WANG Zhanqin, QI Guihong, ZHANG Yinguang. Determination of oxides in zeolites by X-ray fluorescence spectrometry[J]. Analysis and Testing Technology and Instruments,2009,15 (2):118-123. doi: 10.3969/j.issn.1006-3757.2009.02.011
[2]	储刚, 陈刚. 测定ZSM-5分子筛SiO₂/Al₂O₃比的X射线衍射分析新方法[J]. 分析测试技术与仪器,1994(4):35-38 CHU Gang, CHEN Gang. SiO₂/Al₂O₃ ratio of ZSM-5 zeolite determined by X-ray diffraction analysis[J]. Analysis and Testing Technology and Instruments,1994 (4):35-38.
[3]	李巧玲, 叶云. HDPE/CaCO₃断口样品制作与分析[J]. 分析测试技术与仪器,2003,9(2):119-121 doi: 10.3969/j.issn.1006-3757.2003.02.014 LI Qiaoling, YE Yun. Preparation and analysis of HDPE/CaCO₃ section SEM sample[J]. Analysis and Testing Technology and Instruments,2003,9 (2):119-121. doi: 10.3969/j.issn.1006-3757.2003.02.014
[4]	郑娜, 徐丽, 沈素丹, 等. 扫描电子显微镜和能谱分析高性能热塑性板材[J]. 分析测试技术与仪器,2022,28(3):254-259 ZHENG Na, XU Li, SHEN Sudan, et al. Analysis of high-performance thermoplastic plates based on scanning electron microscopy and energy dispersive spectrometry[J]. Analysis and Testing Technology and Instruments,2022,28 (3):254-259.
[5]	陈超, 樊海丽, 蔡志威, 等. 扫描电子显微镜在缓释微球制剂表征中的应用进展[J]. 分析测试技术与仪器,2022,28(2):132-138 CHEN Chao, FAN Haili, CAI Zhiwei, et al. Progress in characterization of controlled release microspheres using scanning electron microscope[J]. Analysis and Testing Technology and Instruments,2022,28 (2):132-138.
[6]	任艳军, 秦素平. 扫描电镜非最佳条件操作考察[J]. 分析测试技术与仪器,2008,14(1):59-61 doi: 10.3969/j.issn.1006-3757.2008.01.014 REN Yanjun, QIN Suping. Study on scanning electron microscope working at nonoptimum observation conditions[J]. Analysis and Testing Technology and Instruments,2008,14 (1):59-61. doi: 10.3969/j.issn.1006-3757.2008.01.014
[7]	李剑平. 扫描电子显微镜对样品的要求及样品的制备[J]. 分析测试技术与仪器,2007,13(1):74-77 doi: 10.3969/j.issn.1006-3757.2007.01.017 LI Jianping. Requirements and preparation of scanning electron microscope sample[J]. Analysis and Testing Technology and Instruments,2007,13 (1):74-77. doi: 10.3969/j.issn.1006-3757.2007.01.017
[8]	冯善娥, 高伟建. 扫描电镜附EDS能谱仪的使用与维护[J]. 分析测试技术与仪器,2014,20(2):115-117 FENG Shane, GAO Weijian. Operation and maintenance of SEM & EDS[J]. Analysis and Testing Technology and Instruments,2014,20 (2):115-117.
[9]	阮涛, 李琼, 马彤梅, 等. 场发射扫描电镜条件对几种特殊样品形貌的影响[J]. 实验技术与管理,2020,37(2):50-53 doi: 10.16791/j.cnki.sjg.2020.02.012 RUAN Tao, LI Qiong, MA Tongmei, et al. Effect of field emission scanning electron microscopy conditions on the morphology of several special samples[J]. Experimental Technology and Management,2020,37 (2):50-53. doi: 10.16791/j.cnki.sjg.2020.02.012
[10]	高翔, 朱紫瑞, 孙伟. 不同参数选择对场发射扫描电镜图像的影响[J]. 广州化工,2019,47(18):86-89 doi: 10.3969/j.issn.1001-9677.2019.18.033 GAO Xiang, ZHU Zirui, SUN Wei. Impacts of different parameters on field emission scanning electron microscopy images[J]. Guangzhou Chemical Industry,2019,47 (18):86-89. doi: 10.3969/j.issn.1001-9677.2019.18.033
[11]	Echlin P. Coating techniques for scanning electron microscopy and X-ray microanalysis[J]. Scanning Electron Microscopy,1978 (1):109-132.
[12]	万鹏, 王馨楠, 徐强, 等. 材料表面性质对扫描电镜镀膜形貌的影响[J]. 电子显微学报,2021,40(6):758-763 doi: 10.3969/j.issn.1000-6281.2021.06.018 WAN Peng, WANG Xinnan, XU Qiang, et al. The effects of the nature of the materials surface on the morphology of sputtered coating for SEM sample preparation[J]. Journal of Chinese Electron Microscopy Society,2021,40 (6):758-763. doi: 10.3969/j.issn.1000-6281.2021.06.018
[13]	李梅晔. 镀膜对FE-SEM纳米尺度形貌观察的影响[J]. 分析测试技术与仪器,2008,14(2):120-124 doi: 10.3969/j.issn.1006-3757.2008.02.012 LI Meiye. Influence of coating on the micro topography of sample observed with FE SEM[J]. Analysis and Testing Technology and Instruments,2008,14 (2):120-124. doi: 10.3969/j.issn.1006-3757.2008.02.012
[14]	张大同. 扫描电镜与能谱仪分析技术[M]. 广州: 华南理工大学出版社, 2009: 47-54.
[15]	章晓中. 电子显微分析[M]. 北京: 清华大学出版社, 2006: 175-180 ZHANG Xiaozhong. Electron microscopy and analysis[M]. Beijing: Tsinghua University Press, 2006: 175-180.
[16]	周莹, 王虎, 吴伟, 等. 加速电压的选择对FESEM图像的影响[J]. 实验室研究与探索,2012,31(10):227-230, 262 ZHOU Ying, WANG Hu, WU Wei, et al. Impact of acceleration voltage on FESEM images[J]. Research and Exploration in Laboratory,2012,31 (10):227-230, 262.
[17]	Endo A, Yamada M, Kataoka S, et al. Direct observation of surface structure of mesoporous silica with low acceleration voltage FE-SEM[J]. Colloids and Surfaces A: Physicochemical and Engineering Aspects,2010,357 (1-3):11-16.
[18]	徐泽忠. FESEM加速电压对样品表面形貌信息的影响[J]. 佳木斯大学学报(自然科学版),2018,36(1):136-137, 162 XU Zezhong. Effect of FESEM acceleration voltage on surface topography information of the sample[J]. Journal of Jiamusi University (Natural Science Edition),2018,36 (1):136-137, 162.
[19]	周宏敏, 付圣权, 李明, 等. 加速电压和束流强度对热敏感材料扫描电镜图像的影响[J]. 分析仪器,2022(2):125-129 doi: 10.3969/j.issn.1001-232x.2022.02.022 ZHOU Hongmin, FU Shengquan, LI Ming, et al. Effects of accelerating voltage and beam current on SEM images of heat sensitive materials[J]. Analytical Instrumentation,2022 (2):125-129. doi: 10.3969/j.issn.1001-232x.2022.02.022