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掃描電子顯微術(shù) Scanning Electron Microscopy 電子顯微的一個(gè)粗略年表 1930年末:第一臺(tái)透射電子顯微鏡1935年:德國(guó)的 Knoll提出了掃描電鏡的概念 (STEM的概念 , 100mm 分辯率 ) 1938年: Von Ardenne開始進(jìn)行實(shí)驗(yàn)室研究, SEM50 mm分辨率 1942: Zworykin. Hillier, 制成了第一臺(tái)實(shí)驗(yàn)室用的掃描電鏡 今天掃描電鏡的全部基本原理 50 nm 分辨率 問題 : 貴 , 照相(曝光)時(shí)間長(zhǎng) ,電子干擾(噪聲) 結(jié)論 : SEM 不實(shí)用 ! 1948: . Oatley, 劍橋大學(xué) SEM 的歷史 ?1938年 Ardenne用一個(gè)透射電鏡 (TEM)的光柵電子束 第一次推斷了 SEM ?1942年 , Zworkin等人第一次為塊狀樣品發(fā)展了 SEM . ?1965年,第一臺(tái)商品 SEM. ?SEM的分辨率被不斷地提高從 1942 年的 50nm到今天的. ?SEM 檢測(cè)信號(hào)用于 確定成分信息 , 如 特征 X射線 , 背散射電子 ,陰極發(fā)光 , 俄歇電子和樣品電流等。 第一個(gè)掃描電鏡裝置 劍橋大學(xué), 1951年 第一臺(tái)商用掃描電鏡 High Resolution Field Emission SEM SEM images have a natural 3D look And now a look inside the SEM…. SEMScanning Electron Microscope (or microscopy) TEM Transmission Electron Microscope AEM Analytical Electron Microscope STEM Scanning Transmission Electron Microscope EPMAElectron Probe MicroAnalyzer SPMScanned Probe Microscope (STM, AFM) To see a VIRTUAL SEM, go to the following link: SEM 的構(gòu)造 氣動(dòng)保險(xiǎn)閥 掃描線圈 Signals available from SEM Signals SEM的主要性能: 1,分辨率 二次電子和俄歇電子的分辨率高,特征 X射線調(diào)制成顯微圖像的分辨率最低。 電子束進(jìn)入 輕 元素樣品 滴狀 作用體積 電子束進(jìn)入 重 元素樣品 半球狀 作用體積 SEM的分辨率即二次電子相的分辨率 電子束進(jìn)入重元素樣品后,立即向橫向擴(kuò)展,因此在分析重元素時(shí),即使電子束的束斑很細(xì)小,也不能達(dá)到較高的分辨率,此時(shí)二次電子和背散射電子之間的分辨率的差距明顯變小。 影響 SEM分辨率的三大因素: 電子束的束斑大小 , 檢測(cè)信號(hào)的類型 以及 檢測(cè)部位的原子序數(shù) SEM分辨率的測(cè)定方法: 在已知的放大倍數(shù)(一般在 10萬倍)的條件下,把在圖像上測(cè)到的最小間距除以放大倍數(shù)所得數(shù)值就是分辨率。 When theoretically considering the electron probe diameter alone, the higher the accelerating voltage, the smaller is the electron probe. However, there are some unnegligible demerits in increasing the accelerating voltage. They are mainly as follows: 1) Lack of detailed structures of specimen surfaces. 2) Remarkable edge effect. 3) Higher possibility of chargeup. 4) Higher possibility of specimen damage. In SEM, finer surface structure images can generally be obtained with lower accelerating voltages. At higher accelerating voltages, the beam peration and diffusion area bee larger, resulting in unnecessary signals (., backscattered electrons) being generated from within the specimen. And these signals reduce the image contrast and veils fine surface structures. It is especially desirable to use low accelerating voltage for observation of lowconcentration substances. 加速電壓對(duì) SEM 像的影響 Always consider Interaction Volume 掃描電子顯微術(shù):例子 The effect of Accelerating Voltage on SEM Images 30 kV 10 kV 5 kV 3 kV Specimen: Toner 墨粉 When high accelerating voltage is used as at (a), it is hard to obtain the contrast of the specimen surface structure. Besides, the specimen surface is easily charged up. The surface microstructures are easily seen at (b). (a) 30 kV x 2,500 (b) 5 kV x 2,500 Specimen: Evaporated Au particles. The image sharpness and resolution are better at the higher accelerating voltage, 25 kV. (a) 5 kV x 36,000 (b) 25 kV x 36,000 Specimen: Filter paper. At 5 kV, the microstructures of the specimen surface are clearly seen as the peration and diffusion area of incident electrons is shallow. (a) 5 kV x 1,400 (b) 25 kV x 1,400 Fig. 6 Specimen: Sintered powder. At low accelerating voltage, while surface microstructures can be observed,