Kemmenoe B H, Bullock G R
J Microsc. 1983 Nov;132(Pt 2):153-63. doi: 10.1111/j.1365-2818.1983.tb04267.x.
Gold, platinum and tungsten films were deposited by low energy input (7 mA, 450 V), or high deposition rate (80 mA, 1500 V), diode sputter coating and by ion beam sputter coating. Film structures on Formvar coated grids and on the surface of coated erythrocytes, resin embedded, sectioned, and recorded at high magnification in a TEM were compared using computer-assisted measurements and analysis of film thickness and grain size. The average grain size of the thinnest gold and platinum films was relatively independent of the mode or rate of deposition but as the film thickness increased, significant differences in grain size and film structure were observed. Thick platinum or gold films deposited by low energy input sputter coating contained large grain size and electron transparent cracks; however, more even films with narrower cracks but larger grain size were produced at high deposition rates. Ion beam sputter coated gold had relatively large grain size in 10 nm thick films, but beyond this thickness the grains coalesced to form a continuous film. Platinum films deposited by ion beam sputter coating were even and free of electron transparent cracks and had a very small grain size (1-2 nm), which was relatively independent of the film thickness. Tungsten deposition either by low energy input or ion beam sputter coating resulted in fine grained even films which were free of electron transparent cracks. Such films remained granular in substructure and had a grain size of about 1 nm which was relatively independent of film thickness. Tungsten films produced at high deposition rates were of poorer quality. We conclude that thick diode sputter coated platinum and gold films are best deposited at high deposition rates provided the specimens are not heat sensitive, the improvement in film structure being more significant than the slight increase in grain size. Thick diode or ion beam sputter coated gold films should be suitable for low resolution SEM, and thin discontinuous gold films for medium resolution SEM. Diode sputter coated platinum should be suitable for medium resolution SEM and ion beam sputter coated platinum for medium and some high resolution SEM. 1-5 nm thick tungsten films, deposited by low energy input or ion beam sputter coating should be suitable for high resolution SEM, particularly where contrast is of less importance than resolution.
通过低能量输入（7毫安，450伏）或高沉积速率（80毫安，1500伏）的二极管溅射镀膜以及离子束溅射镀膜来沉积金、铂和钨薄膜。使用计算机辅助测量和分析薄膜厚度及晶粒尺寸，比较了在福尔马膜涂层网格上以及包被红细胞表面上的薄膜结构，这些红细胞经树脂包埋、切片，并在透射电子显微镜下以高倍率记录。最薄的金膜和铂膜的平均晶粒尺寸相对独立于沉积模式或速率，但随着薄膜厚度增加，观察到晶粒尺寸和薄膜结构存在显著差异。通过低能量输入溅射镀膜沉积的厚铂膜或金膜包含大晶粒尺寸和电子透明裂缝；然而，在高沉积速率下会产生裂缝更窄但晶粒尺寸更大的更均匀薄膜。离子束溅射镀膜的金在10纳米厚的薄膜中具有相对较大的晶粒尺寸，但超过此厚度后晶粒会合并形成连续薄膜。通过离子束溅射镀膜沉积的铂膜均匀且无电子透明裂缝，并且具有非常小的晶粒尺寸（1 - 2纳米），这相对独立于薄膜厚度。通过低能量输入或离子束溅射镀膜沉积的钨会形成细晶粒均匀薄膜，且无电子透明裂缝。这种薄膜在亚结构中保持颗粒状，晶粒尺寸约为1纳米，相对独立于薄膜厚度。在高沉积速率下制备的钨膜质量较差。我们得出结论，只要样本对热不敏感，厚二极管溅射镀膜的铂和金薄膜最好在高沉积速率下沉积，薄膜结构的改善比晶粒尺寸的轻微增加更为显著。厚二极管或离子束溅射镀膜的金薄膜应适用于低分辨率扫描电子显微镜，薄的不连续金薄膜适用于中等分辨率扫描电子显微镜。二极管溅射镀膜的铂应适用于中等分辨率扫描电子显微镜，离子束溅射镀膜的铂适用于中等分辨率和一些高分辨率扫描电子显微镜。通过低能量输入或离子束溅射镀膜沉积的1 - 5纳米厚的钨薄膜应适用于高分辨率扫描电子显微镜，特别是在对比度不如分辨率重要的情况下。
