{"id":64,"date":"2026-03-06T11:23:21","date_gmt":"2026-03-06T03:23:21","guid":{"rendered":"http:\/\/111.229.143.96\/?p=64"},"modified":"2026-03-13T11:17:44","modified_gmt":"2026-03-13T03:17:44","slug":"%e9%99%b6%e7%93%b7%e6%a0%b7%e5%93%81","status":"publish","type":"post","link":"https:\/\/www.huolanlab.com\/index.php\/2026\/03\/06\/%e9%99%b6%e7%93%b7%e6%a0%b7%e5%93%81\/","title":{"rendered":"SEM\u6d4b\u8bd5\u6848\u4f8b-\u9676\u74f7\u6837\u54c1"},"content":{"rendered":"

<\/path><\/svg><\/p>\n\n\n\n
\"\"<\/figure>\n\n\n\n

\u5b8c\u5168\u4e0d\u5bfc\u7535\u7684\u9676\u74f7\u6837\u54c1\uff0c\u5728\u4e0d\u55b7\u91d1\u7684\u60c5\u51b5\u8bdd\uff0c\u91c7\u7528\u4f4e\u7535\u538b\u9ad8\u5206\u8fa8\u6210\u50cf\u6280\u672f\uff0c\u53ef\u6e05\u6670\u89c2\u5bdf\u5230\u5176\u8868\u9762\u7684\u7eb3\u7c73\u53f0\u9636\u72b6\u7ed3\u6784\u3002<\/p>\n\n\n

<\/path><\/svg><\/p>\n\n\n

Tips<\/h3>\n\n\n\n

\u9676\u74f7\u901a\u5e38\u5177\u6709\u786c\u5ea6\u9ad8\u3001\u5bfc\u7535\u6027\u5dee\uff08\u591a\u6570\u9676\u74f7\uff09\u3001\u7ed3\u6784\u81f4\u5bc6\u6216\u591a\u5b54<\/strong>\u7b49\u7279\u70b9\uff0c\u9488\u5bf9\u9676\u74f7\u6837\u54c1\u7684\u7279\u6027\uff0c\u6d4b\u8bd5\u7684\u4fa7\u91cd\u70b9\u5728\u4e8e\u5982\u4f55\u83b7\u5f97\u5e72\u51c0\u7684\u3001\u771f\u5b9e\u7684\u3001\u5177\u6709\u826f\u597d\u5bf9\u6bd4\u5ea6\u7684\u8868\u9762\/\u65ad\u9762\u4fe1\u606f<\/strong>\uff0c\u540c\u65f6\u8981\u5c0f\u5fc3\u6837\u54c1\u5236\u5907\u5bf9\u8868\u9762\u7684\u7834\u574f\u3002<\/p>\n\n\n

1. 样品制备：难点在于”硬”和”脆”<\/h5>\n\n\n\n

\u9676\u74f7\u6750\u6599\u786c\u5ea6\u9ad8\u3001\u8106\u6027\u5927\uff0c\u5236\u5907\u7684\u5173\u952e\u5728\u4e8e\u83b7\u5f97\u4e00\u4e2a\u5e73\u6574\u3001\u65e0\u5e94\u529b\u7684\u89c2\u5bdf\u9762\u3002<\/p>\n\n\n

    \n
  • \n块状陶瓷：<\/strong>
      \n
    • \n观察表面：<\/strong> 如果是直接观察烧结表面或原始表面，通常用乙醇超声清洗去除表面浮尘即可。注意：<\/strong> 超声时间不宜过长，防止引入微裂纹或使晶界受损。<\/li>\n\n\n\n
    • \n观察断面（最常用）：<\/strong> 为了观察陶瓷的内部晶粒形貌、晶界、气孔分布，通常需要进行断口分析<\/strong>。
        \n
      • \n方法：<\/strong> 在样品上预先用小刀划一个浅槽，然后用外力（如锤子敲击或三点弯曲）沿槽口将样品折断。<\/li>\n\n\n\n
      • \n要点：<\/strong> 务必获得新鲜的、未受污染的断面<\/strong>。手触摸过的断面会有油脂污染，影响观察，此时需用丙酮或酒精进行短时清洗。<\/li>\n<\/ul>\n<\/li>\n\n\n\n
      • \n观察抛光面：<\/strong> 如果需要观察气孔率、相分布或进行能谱面分析，需要对样品进行镶嵌、研磨和抛光<\/strong>。抛光后的样品需要热腐蚀或化学腐蚀<\/strong>以显露晶界。<\/li>\n<\/ul>\n<\/li>\n\n\n\n
      • \n粉末状陶瓷：<\/strong>
          \n
        • 这与纳米花粉末的制备方法一致：取少量粉末超声分散在乙醇中，滴在硅片或导电胶上，干燥后吹去浮粉。<\/li>\n\n\n\n
        • \n注意：<\/strong> 如果是易团聚的纳米陶瓷粉，分散是关键。<\/li>\n<\/ul>\n<\/li>\n<\/ul>\n\n\n
          2. 导电性处理：荷电效应的抑制<\/h5>\n\n\n\n

          \u7edd\u5927\u591a\u6570\u9676\u74f7\uff08\u5982\u6c27\u5316\u94dd\u3001\u6c27\u5316\u9506\u3001\u6c2e\u5316\u7845\u7b49\uff09\u90fd\u662f\u7edd\u7f18\u4f53\u6216\u9ad8\u963b\u534a\u5bfc\u4f53\uff0c\u5728\u7535\u5b50\u675f\u8f70\u51fb\u4e0b\u6781\u6613\u4ea7\u751f\u8377\u7535\u6548\u5e94<\/strong>\uff08\u56fe\u50cf\u8fc7\u4eae\u3001\u51fa\u73b0\u6761\u7eb9\u3001\u5f02\u5e38\u8df3\u52a8\uff09\u3002<\/p>\n\n\n

            \n
          • \n必须镀膜：<\/strong> 除非你的电镜有低真空模式，否则常规高真空SEM观察陶瓷必须喷金或喷碳。
              \n
            • \n喷金\/铂：<\/strong> 适用于形貌观察<\/strong>。由于陶瓷表面通常比较致密，喷金时要确保样品台旋转倾斜<\/strong>，使凹凸不平的断面或表面都能镀上连续导电层，否则凹陷处会因电荷积累而显得漆黑一片。<\/li>\n\n\n\n
            • \n喷碳：<\/strong> 适用于后续要做能谱分析<\/strong>的样品。因为金的峰（Mα）会与硫（S）、氯（Cl）等元素的峰重叠，且碳膜对X射线的吸收较小，定量更准。<\/li>\n<\/ul>\n<\/li>\n\n\n\n
            • \n低真空模式：<\/strong> 如果电镜有低真空或环境扫描模式，可以不镀膜直接观察。利用气体分子中和电荷，对陶瓷这种硬质绝缘体非常友好，还能保留样品原始状态，方便后续清洗或处理。<\/li>\n<\/ul>\n\n\n
              3. 成像参数：追求”景深”与”清晰度”<\/h5>\n\n\n\n

              \u9676\u74f7\u7684\u65ad\u53e3\u901a\u5e38\u975e\u5e38\u7c97\u7cd9\uff0c\u6709\u8d77\u4f0f\u7684\u6676\u7c92\u548c\u6df1\u5b54\u3002<\/p>\n\n\n

                \n
              • \n大工作距离：<\/strong> 为了获得更大的景深<\/strong>（让高低不平的区域都能看清楚），建议将工作距离适当调大（例如10-15 mm）。<\/li>\n\n\n\n
              • \n加速电压：<\/strong>
                  \n
                • \n高电压（15-20 kV）：<\/strong> 能获得更好的极限分辨率，适合观察晶粒内部的精细结构或进行高倍率观察。但过高的电压可能导致电子束穿透晶粒边界，使图像看起来有点”透”。<\/li>\n\n\n\n
                • \n低电压（5-10 kV）：<\/strong> 能够更好地反映表面细节，突出晶粒的立体感，且能有效减轻绝缘样品的荷电效应。对于未镀膜或镀膜较薄的样品，低电压优势明显。<\/li>\n<\/ul>\n<\/li>\n\n\n\n
                • \n探针电流：<\/strong> 对于抛光腐蚀后的样品，需要较大的束流以获得更好的背散射电子信号（用于区分不同相）；而对于粗糙断面，适中的束流配合二次电子探测器即可。<\/li>\n<\/ul>\n\n\n
                  4. 能谱分析：注意成分准确性<\/h5>\n\n\n\n

                  \u5982\u679c\u9700\u8981\u5bf9\u9676\u74f7\u8fdb\u884c\u80fd\u8c31\u70b9\u5206\u6790\u6216\u9762\u5206\u5e03\uff1a<\/p>\n\n\n

                    \n
                  • \n平整度要求：<\/strong> 定量能谱分析强烈建议在抛光后的平面上进行<\/strong>。粗糙的断口表面会导致X射线被遮挡或产生不规则吸收，造成定量结果偏差很大。<\/li>\n\n\n\n
                  • \n镀碳：<\/strong> 如前述，进行精确的定量分析时，喷碳优于喷金。<\/li>\n\n\n\n
                  • \n元素确认：<\/strong> 陶瓷常含有轻元素（如氧、氮、碳），这些元素的X射线产额低，容易被吸收。在分析时需要注意选择合适的工作电压，并采用标样或标准数据库进行校正。<\/li>\n<\/ul>\n\n\n
                    总结<\/h5>\n\n\n\n

                    \u9676\u74f7SEM\u6d4b\u8bd5\u7684\u6838\u5fc3\u662f “\u4e00\u4e2a\u4e2d\u5fc3\uff0c\u4e24\u4e2a\u57fa\u672c\u70b9”<\/strong> \uff1a<\/p>\n\n\n

                      \n
                    • \n一个中心：<\/strong> 获得新鲜、干净、无污染的观察面（断面\/抛光面）。<\/li>\n\n\n\n
                    • \n基本点1：<\/strong> 解决导电性问题（喷金\/碳或低真空）。<\/li>\n\n\n\n
                    • \n基本点2：<\/strong> 合理利用景深和电压来展现陶瓷晶粒的立体形貌。<\/li>\n<\/ul>\n","protected":false},"excerpt":{"rendered":"

                      \u5b8c\u5168\u4e0d\u5bfc\u7535\u7684\u9676\u74f7\u6837\u54c1\uff0c\u5728\u4e0d\u55b7\u91d1\u7684\u60c5\u51b5\u8bdd\uff0c\u91c7\u7528\u4f4e\u7535\u538b\u9ad8\u5206\u8fa8\u6210\u50cf\u6280\u672f\uff0c\u53ef\u6e05\u6670\u89c2\u5bdf\u5230\u5176\u8868\u9762\u7684\u7eb3\u7c73\u53f0\u9636\u72b6\u7ed3\u6784\u3002 Tip […]<\/p>\n","protected":false},"author":1,"featured_media":0,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"footnotes":""},"categories":[1],"tags":[],"class_list":["post-64","post","type-post","status-publish","format-standard","hentry","category-1"],"_links":{"self":[{"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/posts\/64","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/users\/1"}],"replies":[{"embeddable":true,"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/comments?post=64"}],"version-history":[{"count":3,"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/posts\/64\/revisions"}],"predecessor-version":[{"id":248,"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/posts\/64\/revisions\/248"}],"wp:attachment":[{"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/media?parent=64"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/categories?post=64"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/www.huolanlab.com\/index.php\/wp-json\/wp\/v2\/tags?post=64"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}