应用案例｜扫描电镜和氩离子抛光在样品成分分析中的应用-医疗器械网

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应用案例｜扫描电镜和氩离子抛光在样品成分分析中的应用

来源：纳克微束（北京）有限公司分类：产品评测 2024-02-23 15:15:08 12阅读次数

场发射扫描电镜是功能材料分析、微纳结构观测、结构组分分析等不可缺少的基本工具，其中，高分辨场发射扫描电镜在亚纳米级别材料的形貌观察和尺寸检测方面具有简便、可操作性强的优势，在纳米科学、半导体工业、能源材料、生命科学、材料科学和环境科学等领域有着巨大需求且发挥巨大作用。

扫描电镜在分析材料样品组分时，其制备方法很关键。不合适的制样可能会导致形貌失真、成分比例误差大等后果。近年来，随着三离子束研磨仪的普及，它的应用领域也越来越广泛。离子束研磨技术几乎是唯一一个适用于任何材质样品，获得高质量切割截面或抛光平面的解决方案。使用该技术对样品进行处理，样品受到形变或损伤的可能性最低，可暴露出样品内部真实的结构信息。

以金属丝样品为例，其包含铂（Pt）和镍（Ni）两种成分。在使用Leica EM TIC3X 三离子束研磨前，其在扫描电镜下的形貌如下图1所示，从BSE图上我们可以分辨出亮度高的Pt元素、亮度低Ni元素，但两种成分之间并没有明显的界限。此外，样品表面存在一些黑色的污染物，这可能会影响Pt和Ni的定量分析。

图1 离子研磨前金属丝截面BSE图

然而，该样品在经过Leica EM TIC3X三离子束研磨后，其真实的截面结构如下图2所示（FE1050电镜结果），样品表面平整、干净无污染，且Pt和Ni两种成分有明显的分界。EDS结果（图3）显示样品由Pt和Ni两种元素组成，元素序数较低的Ni位于样品中间，而元素序数较高的Pt位于样品边缘。

图2 离子研磨后金属丝截面BSE图

图3 离子研磨后金属丝截面EDS结果

小结，获得样品真实结构信息是进行电镜表征的关键，因此在上机前用户需要选择合适的样品处理方法。

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[8]未定义数组索引: page
[2]Declaration of app\common\model\TechNewsCategory::getList($filter = Array) should be compatible with app\common\model\BaseModel::getList($filter = Array, $sort = Array)
[8]未定义数组下标: 0
[2]Declaration of app\common\model\TechNews::getAllList($filter = Array, $limit = 10, $order = Array, $with = Array) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\Company::getAllList($filter = Array, $limit = 20) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8]未定义数组索引: center
[8]Only variables should be passed by reference
[2]Declaration of app\common\model\TechNewsComment::getAllList($filter = Array, $limit = 16) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8192]Function create_function() is deprecated
[8192]Function create_function() is deprecated
[8]未定义数组索引: area
[8]未定义数组索引: st
[2]Declaration of app\common\model\Topic::getList($filter = Array) should be compatible with app\common\model\BaseModel::getList($filter = Array, $sort = Array)
[2]Declaration of app\common\model\Topic::getAllList($filter = Array, $field = 'id,md5,tit...', $limit = 0) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\TopicInfoList::getAllList($filter = Array, $limit = 8) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\News::getAllList($filter = Array, $limit = 16, $order = Array, $with = Array) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8]未定义数组索引: center
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: goods_list
[8]未定义数组下标: 0
[8]未定义数组索引: center
[8]未定义数组索引: center
[8]未定义数组索引: center
[8]未定义数组索引: center
[8]未定义数组索引: center
[8]未定义数组索引: wtt_list

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[ SQL ] SHOW COLUMNS FROM `tech_news_category` [ RunTime:0.001032s ]
[ SQL ] SELECT `id`,`name` FROM `tech_news_category` WHERE `is_show` = 1 [ RunTime:0.000393s ]
[ SQL ] SELECT * FROM `tech_news_category` WHERE `parent_id` = 0 AND `is_show` = 1 ORDER BY `sort` ASC,`id` DESC [ RunTime:0.000245s ]
[ SQL ] SHOW COLUMNS FROM `company` [ RunTime:0.001151s ]
[ SQL ] SHOW COLUMNS FROM `tech_news` [ RunTime:0.000771s ]
[ SQL ] SELECT * FROM `tech_news` WHERE `md5` = 'ba7a9cdc248e969d' AND `review_status` = 1 LIMIT 1 [ RunTime:0.000531s ]
[ SQL ] SHOW COLUMNS FROM `user_info` [ RunTime:0.000793s ]
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[ SQL ] SELECT * FROM `company` WHERE `id` = 904 [ RunTime:0.000186s ]
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[ SQL ] SELECT * FROM `tech_news_text` WHERE `tech_news_id` = 2498 [ RunTime:0.019011s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_belong_category` [ RunTime:0.001130s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2498 [ RunTime:0.000947s ]
[ SQL ] SELECT * FROM `tech_news_category` WHERE `id` IN (6) [ RunTime:0.000201s ]
[ SQL ] SHOW COLUMNS FROM `user_follow` [ RunTime:0.000799s ]
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[ SQL ] SHOW COLUMNS FROM `tech_news_comment` [ RunTime:0.000803s ]
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[ SQL ] SELECT COUNT(*) AS tp_count FROM `tech_news_comment` WHERE `tech_news_id` = 2498 LIMIT 1 [ RunTime:0.000199s ]
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[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (786,316,263,642,610,375,346) [ RunTime:0.000717s ]
[ SQL ] SHOW COLUMNS FROM `topic` [ RunTime:0.001093s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `topic` WHERE `review_status` = 1 ORDER BY `id` DESC LIMIT 4 [ RunTime:0.000202s ]
[ SQL ] SHOW COLUMNS FROM `topic_info_list` [ RunTime:0.000913s ]
[ SQL ] SELECT * FROM `topic_info_list` WHERE `topic_id` = 1 ORDER BY `id` DESC LIMIT 2 [ RunTime:0.000312s ]
[ SQL ] SHOW COLUMNS FROM `news` [ RunTime:0.000872s ]
[ SQL ] SELECT * FROM `news` WHERE `id` IN (864,849) [ RunTime:0.000235s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `tech_news` WHERE `review_status` = 1 AND `is_show` = 1 ORDER BY `id` DESC LIMIT 10 [ RunTime:0.000227s ]
[ SQL ] SHOW COLUMNS FROM `user` [ RunTime:0.000787s ]
[ SQL ] SELECT `a`.* FROM `user` `a` INNER JOIN `tech_news` `b` ON `a`.`id`=`b`.`user_id` GROUP BY `a`.`id` ORDER BY `b`.`id` DESC LIMIT 10 [ RunTime:0.004989s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (592,413,444,224,13,239,598,697,394,285) [ RunTime:0.000960s ]
[ SQL ] SHOW COLUMNS FROM `seo` [ RunTime:0.000822s ]
[ SQL ] SELECT * FROM `seo` WHERE `column_type` = '16' AND `page_type` = 'tech_news' AND `info_id` = 2498 LIMIT 1 [ RunTime:0.000240s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2498 [ RunTime:0.000922s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3498 [ RunTime:0.001039s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3371 [ RunTime:0.000978s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2553 [ RunTime:0.000934s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1849 [ RunTime:0.001119s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1770 [ RunTime:0.001085s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2828 [ RunTime:0.000890s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2234 [ RunTime:0.000857s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2764 [ RunTime:0.000854s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2103 [ RunTime:0.000863s ]
[ SQL ] SELECT * FROM `user` WHERE `id` = 786 LIMIT 1 [ RunTime:0.000159s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 592 LIMIT 1 [ RunTime:0.000175s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 592 LIMIT 1 [ RunTime:0.000134s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 413 LIMIT 1 [ RunTime:0.000121s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 413 LIMIT 1 [ RunTime:0.000145s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 444 LIMIT 1 [ RunTime:0.000132s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 444 LIMIT 1 [ RunTime:0.000146s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 224 LIMIT 1 [ RunTime:0.000124s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 224 LIMIT 1 [ RunTime:0.000122s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 13 LIMIT 1 [ RunTime:0.000133s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 13 LIMIT 1 [ RunTime:0.000134s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 239 LIMIT 1 [ RunTime:0.000116s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 239 LIMIT 1 [ RunTime:0.000112s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 598 LIMIT 1 [ RunTime:0.000119s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 598 LIMIT 1 [ RunTime:0.000137s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 697 LIMIT 1 [ RunTime:0.000128s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 697 LIMIT 1 [ RunTime:0.000115s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 394 LIMIT 1 [ RunTime:0.000116s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 394 LIMIT 1 [ RunTime:0.000173s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 285 LIMIT 1 [ RunTime:0.000140s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 285 LIMIT 1 [ RunTime:0.000127s ]

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