Pretreatment methods of scanning electron microscopy for typical marine geological samples
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摘要:
扫描电子显微镜（SEM）在海洋地质研究中具有重要作用，可揭示样品的微观形貌和成分特征。海洋地质样品的复杂性和多样性对前处理技术提出特殊要求，样品制备方法成为确保成像质量和数据可靠性的关键。本文系统总结了典型海洋地质样品（包括有孔虫、介形虫、颗石藻、孢粉、嗜中性微需氧铁氧化菌、冷水珊瑚、粉末沉积物及岩石碎屑）的SEM前处理方法，涵盖清洗、超声处理、干燥、固定、镀膜及测试等关键步骤。针对各类样品的理化特性（如脆弱性、高含水量、导电性差），阐述了技术要点、常见问题（如荷电效应、结构塌陷）及优化方案。优化的样品前处理流程能显著提升SEM成像分辨率和数据可靠性，为海洋地质微观分析提供技术参考和借鉴。
Abstract:Scanning electron microscopy (SEM) is an important tool for marine geological research, enabling detailed analysis of the morphology and composition of the samples. The complexity and diversity of marine geological samples require specific pretreatment techniques to ensure high-quality images and reliable data. We systematically reviewed the SEM pretreatment methods for typical marine geological samples, including foraminifera, ostracods, coccolithophores, spore-pollen, iron-oxidizing bacteria, cold-water corals, powdered sediments, and rock fragments. The main procedures including cleaning, ultrasonic treatment, drying, fixation, coating, and instrumental analysis were described in detail based on the physical and chemical properties of each sample type (e.g., fragility, high water content, poor conductivity). Common challenges, such as electron charging effects and structural collapse, were addressed with optimization strategies. Results demonstrate that optimized pretreatment protocols could greatly improve the SEM imaging resolution and data reliability, providing a robust reference for marine geological microanalysis.
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表 1 典型海洋地质样品扫描电镜前处理方法
Table 1. SEM preparation methods for typical marine geological samples
样品类型 清洗 干燥 固定 镀膜 有孔虫/介形虫 蒸馏水或试剂泡软冲洗，
63～150 μm或250 μm筛子干筛，
挑出个体颗粒自然干燥、烘箱烘干、冷冻干燥 体视显微镜下逐粒固定于导电胶样品座 5～10 nm金/碳膜
或不镀膜颗石藻 现生：1～2 L海水经0.8 μm滤膜过滤，去离子水冲洗；沉积物：0.1～0.5 g样品3 μm滤膜过滤 自然干燥或烘箱烘干 裁剪滤膜固定于样品座 10～15 nm金/碳膜
或不镀膜孢粉化石 稀盐酸、氢氟酸除杂质，蒸馏水漂洗，7 μm尼龙筛网超声过滤，
离心后试管保存烘箱烘干、真空干燥 滴管取浓缩物，显微镜下孢粉粒固定于导电胶样品座 5～10 nm金/碳膜 铁氧化菌 0.22 μm滤膜过滤菌液，去离子水冲洗；或2.5%戊二醛固定，
PBS缓冲液洗脱自然干燥或梯度酒精脱水
后晾干或冷冻干燥滤膜或样品粘于导电胶
样品座5～10 nm金膜（形貌）
或碳膜（EDS）冷水珊瑚 软毛刷去离子水超声清洗，
或稀盐酸溶解方解石节后冲洗自然干燥 环氧树脂包埋抛光或固定于样品座 5～20 nm金膜（形貌）
或碳膜（EDS）粉末沉积物 乙醇/丙酮/去离子水低功率超声清洗 烘箱烘干或冷冻干燥或自然干燥 洒落法或悬浊液法滴涂于
样品座10～20 nm金膜（形貌）
或碳膜（EDS）岩石/碎屑 压缩空气/软毛刷清洁断面；
抛光片用无尘布擦拭自然干燥或烘箱干燥或
真空干燥用导电胶固定于样品座 5～20 nm金膜（形貌）
或碳膜（EDS）说明：导电胶样品座是指双面导电胶贴在SEM样品座表面，酸浓度、干燥温度等参数参见正文。 
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