扫描电子显微镜的应用及若干问题的讨论课件.pptx

1、Copyright2011 Hitachi High-Technologies Corporation All Rights RCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.电镜功能及原理新技术及前沿应用正确的使用方法选择电镜的注意事项主要内容主要内容Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.电子显微镜电子显微镜扫描电镜扫描电镜SEM透射电镜透射电镜TEM台台式式电电镜镜钨钨灯灯丝丝扫扫描描电电镜

2、镜场场发发射射扫扫描描电电镜镜120KV200KV300KV超高压透射超高压透射冷场发射冷场发射扫描电镜扫描电镜热场发射热场发射扫描电镜扫描电镜一、电子显微镜的分类一、电子显微镜的分类Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.4光学显微镜和大型扫描电镜对比光学显微镜和大型扫描电镜对比Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.硅藻硅藻Copyright2011 Hitachi High-Tech

3、nologies Corporation All Rights Reserved.硅藻硅藻Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.7波斯合欢树的花粉叶蓟属植物火球状花粉Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.8普通家蝇黄蜂的头部Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.9黄蜂的头部Copy

4、right2011 Hitachi High-Technologies Corporation All Rights Reserved.电子显微镜的功能电子显微镜的功能1、高分辨率、高分辨率2、大景深、大景深3、元素和、元素和结结构分析构分析d=0.61/nsin 光学显微镜的极限分辨率为光学显微镜的极限分辨率为200nm，放大倍率最大，放大倍率最大2000倍。倍。扫描电镜的分辨率可以达到扫描电镜的分辨率可以达到3nm甚至更小，放大倍率可到甚至更小，放大倍率可到几万几万倍倍至至一百万一百万倍。倍。f=aDdM)2.0(EDX能能谱仪谱仪分析分析 为什么需要用扫描电镜观察样品为什么需要用扫描电镜

5、观察样品形貌？形貌？Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.形貌观察形貌观察表面微表面微观观形貌形貌成分成分衬衬度度图图像像扫扫描描电镜电镜的功能的功能电子显微镜的功能电子显微镜的功能Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.元素与结构分析元素与结构分析EBICEBIC测测PNPN结结C_K3kVN_K3kVTa:360nmSiC:160nmSiN:240nmAl:500-600nmMagn

6、ificationx80kEDXEDX或或WDXWDX的元素定性或定量分析的元素定性或定量分析EBSDEBSD测测晶粒取向晶粒取向CLCL阴极阴极荧荧光光图图像像电子显微镜的功能电子显微镜的功能Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.电子显微镜的功能电子显微镜的功能Copyright2011 Hitachi High-Technologies Cor

7、poration All Rights Reserved.15Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.16Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.人眼分辨率示意图人眼分辨率仪器分辨率有效放大倍数仪器放大倍率和分辨率的关系人眼分辨率一定，获得高的分辨率需要大的放大倍数。电镜图像是如何形成的？电镜图像是如何形成的？17Copyright2011 Hitachi High-Technologie

8、s Corporation All Rights Reserved.电镜图像是如何形成的？电镜图像是如何形成的？Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.电子束和样品表面相互作用产生的信号类型19SEBSEEDX能谱Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.2010010,0001能能 量量(eV)(eV)(入射电子能量入射电子能量:10,000eV)10,000eV)SEBSE产产额额 SE

9、SE和和BSEBSE的电子能量幅度的电子能量幅度50Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.21SampleSample：BaCOBaCO3 3/TiO/TiO2 2VaccVacc：1 k1 kV VMagnificationMagnification：x x 7 70k0kSEBSESESE和和BSEBSE信号信号Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.C CAuAuCopyright

10、2011 Hitachi High-Technologies Corporation All Rights Reserved.X射线的产生射线的产生Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.24Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.25全球最高分辨率全球最高分辨率原子原子级级全息全息电电子子显显微微镜镜（点分辨率可达（点分辨率可达43pm）超超强强分析功能分析功能电电子子显显微微镜镜原子原

11、子级级分辨率开展分析分辨率开展分析（专为维专为维多利多利亚亚大学定制的大学定制的HF3300V）全球最高加速全球最高加速电压电压超高超高压压透射透射电电子子显显微微镜镜（加速加速电压电压可达可达3MV）Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.电子源直径小，色差小束流大束流稳定大束流分析高分辨观察Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.样品：分子筛Copyright2011 Hitachi

12、High-Technologies Corporation All Rights Reserved.28加速电压:5 kV放大倍率:150,000 x探针电流:0.7 nA分析时间：15 min样品：Cu2O/Au nano particles 放大倍率：150,000 x探头：YAGBSEAuCu2OCu2O/Au 纳米颗粒低加速电压下获得的高分辨面分布样品提供者：京都大学，化学研究所 Prof.Toshiharu Teranishi探测器:Oxford X-Max 150Copyright2011 Hitachi High-Technologies Corporation All Righ

13、ts Reserved.需要得到一个平滑的面？29BSEEBSDEDS 元素質量濃度%K0.080.04 Ca0.160.04内部成分、层厚晶粒尺寸、取向定性、定量分析EBICP-N结位置颗粒内部结构BSE光学特性CLCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.加工过程截面制作割断超薄切片树脂包埋粗研磨精细研磨离子研磨掰断液氮脆断SEM观察、EDS分析、EBSD分析机械研磨树脂、真空排气设备Maruto研磨工具FIB加工Copyright2011 Hitachi High-Technologie

14、s Corporation All Rights Reserved.离子研磨系统Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.50 um5 umGaNLED芯片内部構造観察SU8000観察条件試料：LED素子内部構造照射電圧：V観察条件：LA-BSE半导体材料应用半导体材料应用-离子研磨离子研磨Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.5umPt100 nmTiN100 nm300 nmVoidG

15、old bondingGold pad100 nmAlGN25 nmGold bondingActive layerGold padLED芯片内部構造観察半导体材料应用半导体材料应用-离子研磨离子研磨Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.SEGaAlNTiPtAu200 nm(Analysis condition)Vacc:5kVMagnification:x100 kMapping time:20 min5 um200 nmAnalyzed area Layer structure an

16、alysis by large area SDD半导体材料应用半导体材料应用-Mapping-MappingCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.35Li battery 三元材料Adaptable to cross-section making of fragile materialCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.10mSurfaceMagnified image of cro

17、ss-section5mCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.真空隔离状态样品来源：锂动力电池；观察条件：Vacc：800V；信号来源：SE同一视野空气中暴露10minCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.氧峰激增样品来源：锂动力电池；观察条件：Vacc：3kV；信号来源：BSE真空隔离状态空气中暴露10min同一视野Copyright2011 Hitachi High-Technol

18、ogies Corporation All Rights Reserved.SU8010SU8200IM4000SU-70气体保护装置手套箱Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.40Specimen load lock chamberSU70/6600/4800/8000*with Special load lock chamberIM4000 Air protection systemAir protection sample holderAir protection holderSam

19、ple set on the sample stub.Cap is attached to a holder.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Specimen:Negative electrode of lithium-ion battery(a)With air protection ion milling(b)With air exposure after air protection ion milling(Air exposure time:10minutes)SEM ima

20、ge(signal:BSE)SEM image(signal:BSE)The left side image(a)shows that the structure of Negative electrode is clearly observed when Cross-section milling with Air Protection Holder is used while deformation(expansion)of the structure is observed in the right side image(b)if without Air Protection Holde

21、r.离子束加工后Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.BF/DF-STEM Sample：Carbon nanotubeVacc：30kVMag：x 250kModel：SU8020通过透射附件实现扫描透射功能通过透射附件实现扫描透射功能 Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.43MI4050NX9000（三维实时观察）NX20001.4 STEMEBSDEDSE-T SEArIBSE

22、MFIB样品*专专利利第第1374861号号*Triple BeamTriple Beam是日立是日立(Hitachi Hightech(Hitachi Hightech Science)Science)注册注册商商标标Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.44Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.应用领域45ito膜膜锂电锂电池池手机主板手机主板电电容容FPCCopyright201

23、1 Hitachi High-Technologies Corporation All Rights Reserved.贴壁细胞贴壁细胞，固定脱水处理，固定脱水处理Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.保存

24、脆弱样品结构及其相互关系：图为带有卵的蛛丝；背景为保存脆弱样品结构及其相互关系：图为带有卵的蛛丝；背景为“勿忘我勿忘我”花瓣及花粉花瓣及花粉Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Penicillin (P chrysogenum)盘尼西林（青霉素）Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation

25、 All Rights Reserved.Bacteria:Staphylococcus aureus 金黃色葡萄球菌Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.样品名称：假冒冬虫夏草粉末 假冒的冬虫夏草粉末有成分假冒的冬虫夏草粉末有成分差别差别Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.冰淇淋护肤霜凝胶岩石中油滴Copyright2011 Hitachi High-Technologies Co

26、rporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.硫酸盐颗粒富钛合包壳颗粒烟尘集合体颗粒铁氧化物颗粒氧化铁颗粒群富铬、铅的颗粒Copyright2011 Hi

27、tachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.磁控管62Copyright2011 Hitachi H

28、igh-Technologies Corporation All Rights Reserved.63铝铝金属金相结构金相WC-CoCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.金属材料高分辨观察马氏体15nmCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.分辨率高分辨率高，显显微微结结构清晰可辨构清晰可辨真真实实，图图片所展示的片所展示的是真是真实实的的样样品形貌和品形貌和结结构构景深好景深好，图图像

29、没有像没有局域的欠焦或局域的欠焦或过过焦焦现现象象信噪比好信噪比好，没有明，没有明显显的雪花状噪声的雪花状噪声衬衬度适中度适中，图图像中无像中无论论黑区或白区的黑区或白区的细节细节都能看清楚都能看清楚如何如何评评价价扫扫描描电镜图电镜图片片三、观察常见的问题-影响因素Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.信噪比信噪比对图对图片的影响片的影响信噪比差信噪比差信噪比好信噪比好三、观察常见的问题-影响因素Copyright2011 Hitachi High-Technologies Corpor

30、ation All Rights Reserved.损伤损伤后的假像后的假像真真实实形貌形貌样品：锂电池隔膜加速加速电压电压比比对样对样品的品的损伤损伤三、观察常见的问题-影响因素Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.12mm长的螺钉最小5倍的放大倍数Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.荷荷电电现现象象观察常见的问题-荷电Copyright2011 Hitachi High-Tech

31、nologies Corporation All Rights Reserved.70能量范能量范围围(eV)(eV)产产生强度生强度二次二次电电子子背散射背散射电电子子荷电的干扰Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.如何消除荷电现象？1.样品喷镀（Au，Pt，C）2.低真空观察3.低电压、低电流观察（最佳解决方案）Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.为什么不能喷镀？Uncoatin

32、gCoating真实信息真实信息被掩盖Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.消除荷电现象低真空观察-eeGGNon-conductive specimen低真空观察的不足：空气浓度高，电子束散射强，分辨率和信噪比严重下降加速电压高，样品激发体积大，无法观察表面Accelerating voltage:15kVSample:Normal paperSignal amplification6Pa30Pa150PaCharge-up reductionCopyright2011 Hitachi

33、High-Technologies Corporation All Rights Reserved.10Pa15Pa30Pa空气浓度对荷电的影响消除荷电现象低真空观察Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.低加速电压下生物样品的观测 样品：昆虫触角样品：昆虫触角Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.低加速电压下生物样品的观测 大肠杆菌，固定脱水处理大肠杆菌，固定脱水处理Copyright

34、2011 Hitachi High-Technologies Corporation All Rights Reserved.制样所需工具及材料：77Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.1、与样品台接触面保持平整；2、固定：采用导电胶带绑缚，固定性强的液体胶，或采用样品夹持台；3、镶嵌类样品的电荷牵引；4、不导电样品的喷金处理。OR78Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.1、保持样

35、品干燥；2、样品分散均匀；3、粉末样品固定牢固；79Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.样品分散于乙醇（或其它有机试剂），并用超声波分散均匀取一滴分散好的液体样品，滴在铝箔（或硅片上）80Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.膜类样品1、样品表面清洁，铺展均匀；2、样品固定良好；3、荷电有“牵引”；OR81Copyright2011 Hitachi High-Technologies

36、 Corporation All Rights Reserved.1、制样好坏关系到样品图像的质量；2、特殊样品要根据情况选择合适方法，如截面的制备与观察；3、不导电样品要进行喷金处理或改用低加速电压拍摄图片；4、粉末样品注意固定牢固，以免影响画质或污染物镜；5、大块样品注意“牵引”荷电。82Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.TM3030SU1510SU3500S-3700NSU-70SU8010SU8200SU9000IM4000台式电镜钨灯丝扫描电镜冷场发射扫描电镜热场发射扫描电镜

37、离子研磨仪SU5000Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.钨灯丝钨灯丝六硼化镧灯丝六硼化镧灯丝肖特基场发射灯丝肖特基场发射灯丝冷场发射灯丝冷场发射灯丝电子源的大小电子源的大小30um5um20nm5nm亮度亮度（A/cm2 sr)104105108109色散度色散度（eV）21.50.70.2工作温度工作温度（）280015001500RT真空度真空度(Pa)10-310-510-710-8寿命寿命150h1500h1年年35年年flash无需无需无需无需无需无需需要需要最大探针束流最大

38、探针束流大于大于1uA大于大于1uA大于大于50nA23nAZrO2分辨率稍差分辨率较好Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.冷场热场Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.热场热场冷场冷场E=10.7eVd=1530nmE=0.2eVd=5nm亮度亮度：A/cm sr探探针电针电流流：2nA程度程度Copyright2011 Hitachi High-Technologies Corp

39、oration All Rights Reserved.u电子枪的种类：场发射、LaB6或钨灯丝的电子枪u电镜的像差：球差、色差、像散、衍射差u电磁透镜的型式:内透镜、外透镜、半内透镜u环境因素:振动、磁场、噪音、接地u操作条件:加速电压、工作电流、电子束合轴、物镜光阑、扫描速率、样品处理、真空度等影响影响扫扫描描电镜电镜成像的关成像的关键键因素因素Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.样品：高分子基底的银颗粒样品：高分子基底的银颗粒 X10000加速电压：加速电压：30KV30KV加速电

40、压：加速电压：2KV2KVCopyright2011 Hitachi High-Technologies Corporation All Rights Reserved.加速电压：加速电压：3KV 放大倍率放大倍率：100K（未喷镀）（未喷镀）信号模式：信号模式：SE(U,LA40)SE/BSE信号混合像信号混合像样品：高分子球基底的样品：高分子球基底的Ag颗粒颗粒低加速电压下高分辨Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.低加速电压观察的重要性低加速电压观察的重要性1m优点：在低加速电压下，

41、入射电子的扩散区域很小，空间分辨率高，可以获得样品最表面的对比度信息；低加速电压有利于减轻样品的荷电；低加速电压对样品的损伤小。电子在样品内扩散程度的模拟（样品：硅）Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.91Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved

42、.Copyright2011 Hitachi High-Technologies Corporation All Rights Reserved.日立电镜以性能稳定、结实耐用著称日立电镜以性能稳定、结实耐用著称1 1、日立公司精湛的加工工艺和严格的质量保证体系！、日立公司精湛的加工工艺和严格的质量保证体系！2 2、零部件整机由日本日立高新技术公司生产和装配！、零部件整机由日本日立高新技术公司生产和装配！3 3、安装环境要求低（接地电阻、安装环境要求低（接地电阻小于小于100100欧姆欧姆）4 4、耗材寿命长耗材寿命长（灯丝、闪烁体、光电倍增管、光阑等）（灯丝、闪烁体、光电倍增管、光阑等）5 5、低维护成本低维护成本（灯丝价格便宜，仪器结实耐用）（灯丝价格便宜，仪器结实耐用）Copyright2011 Hitachi High-Technologies Corporation All Rights R