热场发射扫描式电子显微镜JEOL JSM7000F
扫描电子显微镜的构造和工作原理
扫描电子显微镜的构造和工作原理扫描电子显微镜（Scanning Electron Microscope，SEM）是一种常用的高分辨率显微镜，它通过使用聚焦的电子束来替代传统显微镜中使用的光束，从而能够观察到非常小尺寸的物体或细节。
SEM的构造和工作原理如下：构造：1.电子源：SEM使用热电子发射或场致发射的方式产生电子束。
常用的电子源是热丝电子枪，其中一个被称为热阴极的钨丝加热电子产生材料，产生电子束。
2. 电子透镜系统：SEM中有两个电子透镜，分别称为透镜1（即准直透镜）和透镜2（即聚经透镜）。
透镜1和透镜2的作用是使电子束呈现较小的束斑（electron beam spot），从而提高分辨率和放大率。
3. 检测系统：SEM的检测系统包括两个主要部分，即二次电子检测器（Secondary Electron Detector，SED）和回散射电子检测器（Backscattered Electron Detector，BED）。
SED主要用于表面形貌观察，它能够检测到由扫描电子激发的二次电子。
BED则用于分析样品的成分和区分不同物质的特性。
4.微控样品台：SEM中的样品台可以精确调整样品位置，使其与电子束的路径重合，并且可以在不同的方向上转动，以便于观察不同角度的样品。
5.显示和控制系统：SEM使用计算机控制系统来控制电子束的扫描和样品台的移动，并将观察结果显示在计算机屏幕上。
工作原理：1.电子束的生成：SEM中的电子源产生高能电子束。
电子源加热电子发射材料，如钨丝，产生高速电子束。
2.电子透镜系统的聚焦：电子束经过透镜1和透镜2的聚焦，使其呈现出较小的束斑。
3.样品的扫描：样品台上的样品被置于电子束的路径中，并通过微控样品台控制样品的位置和方向。
电子束扫描过样品表面，通过电磁透镜和扫描线圈控制电子束的位置。
4.二次电子和回散射电子的检测：电子束与样品相互作用时，会产生二次电子和回散射电子。
二次电子是由电子束激发样品表面产生的电子，可以用来观察样品的表面形貌。
场发射扫描电子显微镜安全操作及保养规程
场发射扫描电子显微镜安全操作及保养规程电子显微镜是一种高精度的仪器，操作时需要遵循一定的安全规程和保养措施，以确保仪器的正常运行和使用者的安全。
下面是电子显微镜的安全操作和保养规程，供参考。
一、电子显微镜的安全操作规程：1.进入实验室前，要穿戴好实验室专用工作服，并佩戴好相应的防护用品，如手套、眼镜和口罩等。
2.在操作电子显微镜之前，应先了解设备的基本知识，熟悉仪器的使用方法和操作步骤。
3.在使用电子显微镜之前，要确保仪器的电源已经关闭，并检查仪器的相关连接线是否牢固。
4.在进行样品准备时，应使用专用工具进行操作，避免直接用手触摸样品和仪器部件。
5.在开机之前，应确认好样品装载台、真空系统和冷凝系统等设备是否运行正常。
6.在启动电子显微镜之前，要确保室内的温度和湿度适宜，尽量避免环境中的尘埃和静电干扰。
7.在启动电子显微镜后，应根据实际需要进行相关参数的调整，如电子束强度、放大倍数和对比度等。
8.在放大和观察样品时，要注意不要过度放大或观察过长时间，以免对样品和仪器造成损坏。
9.在操作电子显微镜时，要保持室内环境的安静和稳定，避免不必要的震动和干扰。
10.在关闭电子显微镜之前，要先将相关参数调整到初始位置，然后将电源关闭，并检查仪器是否有异常情况。
二、电子显微镜的保养规程：1.每天使用电子显微镜之前，要先清理设备外部的尘埃和杂物，并定期清洁仪器的内部部件，如样品台和镜筒等。
2.定期检查电子显微镜的电源线和电源插头是否有损坏或老化现象，并及时更换或维修。
3.定期检查仪器的真空系统和冷凝系统，保持其正常运行状态，如有异常情况，应及时修理或更换相关部件。
4.定期检查仪器的操作系统、数据存储系统和软件程序等，确保其正常运转和更新。
5.定期校准电子显微镜的各项参数和功能，以确保仪器的精度和准确性。
6.在仪器长时间不使用时，要将其储存在干燥、清洁和稳定的环境中，以免仪器受潮、腐蚀或受损。
7.在操作电子显微镜时，要避免使用尖锐或硬物品接触样品、仪器内部或镜筒，以免划伤或损坏仪器。
MerlinCompact热场发射扫描电子显微镜操作手册-北京大学分析
Merlin Compact 热场发射扫描电子显微镜操作手册预约平台 地址仪器状态北京大学化学学院B 区B145 联系电话TEM & SEM LABORATORY6275 4552电镜使用注意事项1、 禁止测试的样品：潮湿、挥发样品绝对禁止进入样品室。
粉末样品2、 禁止自行操作主机部件：没有授权的主机部件、面板、屏幕按钮均禁止触碰。
需反复用洗耳球吹扫样品，防止悬浮颗粒污染真空系统。
3、 装样过程要求全程佩戴手套（用户自行准备），仪器使用过程不得带手套触碰面板。
4、 样品舱放气需检查阀门气压：高纯氮气分阀出口气压<0.05 MPa.5、 加电压前需确定仪器真空状态：电子枪真空<5×10-9 mbar 、样品舱真空<2×10-5mbar ；若真空大于规定数值，禁止继续操作。
6、 禁止用U 盘在主机电脑上拷贝数据：本实验室建有局域网，应在数据电脑上使用光盘拷取。
7、 禁止在电镜室内饮食饮水，大声攀谈：饮料、食物严格禁止带入电镜室，更不允许放在仪器操作台上！电镜使用结束后要将使用过的工具归位，样品台自行清理干净，产生的废弃物及时扔进垃圾箱。
MERLIN Compact仪器简介1、仪器性能指标分辨率：1.0 nm @ 15 kV; 1.9 nm @ 1 kV; 0.8 nm @ 30 kV（STEM 模式）功能：二次电子像、背散射电子像、元素分析、EBSD分析加速电压：0.02–30 kV束流：12 pA–100 nA放大倍数：12倍–2,000,00倍之间电子枪：热场发射肖特基电子枪，束流稳定性优于0.2%/h探测器：高效的镜筒内置二次电子探测器（in-lens Duo），Everhart Thornley 二次电子探测器样品室：330 mm（ф）× 270 mm（h）图像处理：储存分辨率高达32768 × 24576 像素；多种积分和平均模式。
JSM-7800F扫描电镜
提高空间分辨率，能进行 100纳米级清晰的面分布测试。
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JSM-7800F的特长
Point.1
浸没式肖特基场发射电子枪
大电流(200nA 15kV)、长时间稳定、长寿命 (发射体保证3年)
PPooinint.t2.2
超超级级混混合合式式物物镜镜 :: SSHHLL
①超高分辨率(1kV 1.2nm➡选配功能0.8nm@1kV ） ②①②最超最适高适合分合于于辨磁率磁性(性1材材kV料料1的的.2观观nm察察➡和和选EE配BBSS功DD分分能析析0.8((n样样m@品品1k附附V 近近）没没有有磁磁场场))
JEOL Only
测试时间60秒
（实时）
用定性图谱的测试时间可进行元素面分布 用低加速电压可在短时间内进行高空间分辨率的元素面分布测试
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应用实例2. 高空间分辨率的EDS分析 样品 ： IC 截面 定量面分布 (重量%)
是JEOL独自研发的新型卓越透镜
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Semi-in-lens和Out-lens的不同和特长
Semi-in-lens物镜超级混合式物镜Out-lens物镜
工作距离短
透镜磁场
①超高分解率观察
工作距离短 擅长高分辨率观察
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We Provide JSEuOpLe介r H绍ybrid Lheignhs performance
扫描电子显微镜原理
扫描电子显微镜原理
扫描电子显微镜（Scanning Electron Microscope, SEM）是一种利用电子束照射样本表面，通过采集样本散射的次级电子、反射电子、透射电子等生成显微图像的设备。
其原理与传统光学显微镜不同，利用电子束的波粒二象性和电子与物质相互作用的性质来获得高分辨率的图像。
扫描电子显微镜由电子光源、电子光学系统、样本台以及信号检测和图像处理系统等组成。
首先，电子显微镜的电子光源发射出高能电子束，通常通过热丝发射电子的方式。
这些电子束会经过准直和聚焦装置，使其成为一束细且聚焦的电子束。
接下来，样本被放置在扫描电子显微镜的样本台上。
样本表面会与入射电子束相互作用，产生不同的信号。
其中，主要信号包括次级电子（Secondary Electron, SE）、反射电子（Backscattered Electron, BE）以及透射电子（Transmitted Electron, TE）。
次级电子主要由入射电子与样本表面原子的相互作用而产生，其被采集并转化为图像。
反射电子主要是在样本内部物质的相互作用下被散射回来的电子，同样被采集和转化为图像。
透射电子则是透过样本的电子，其传感元件可将其图像化。
这些信号被接收后，经过放大和转换为电子图像信号。
电子图像信号可以通过荧光屏或者光电二极管进行观测和记录。
最后，通过图像处理系统将电子信号转化为高分辨率的图像，该图像具有较高的对比度和分辨率，可以用来观察样本的细微特征。
扫描电子显微镜以其高分辨率和强大的观察能力被广泛应用于材料科学、生命科学、纳米技术以及表面科学等领域。
JSM-7800F扫描电镜
Point.3
用新型探测器过滤电子能量
自由选择来自样品表面的信息
12
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超级混合式物镜(SHL)
Semi-in-lens物镜
Out-lens物镜
超级混合式物镜
SHL集中了semi-in-lens和out-lens两者的长处 是JEOL独自研发的新型卓越透镜
能量过滤器
UED 高位探测器
信号
二次电子 大角度背散射 电子
信息
表面形貌 成分 晶体取向
由过滤器选择
过滤器电压：-360V
20
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通过新型探测器检测信号
USD 高位二次电子探测器
信号
二次电子
信息
表面形貌 边缘效应
out-lens
稳定度・重现性 高加速 分辨率 低加速 分辨率
低倍率观察
低倍率观察
15
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超级混合式物镜(SHL)的功能评估
超级混合式物镜 semi-in-lens
稳定度・重现性
稳定度・重现性 稳定度・重现性 高加速 分辨率 低加速 分辨率 观察绝 缘体 观察 磁性 材料 EBSD
一：仪器介绍
1
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超高分辨率 FE —— マスタ タイトル 超高分解能 FE-SEM 超高分辨率场发射扫描电子显微镜 の書式設定 JSM-7800F JSM-7800F 介绍のご紹介
JEOL JSM-7500FA 场发射扫描电子显微镜使用说明书
Instructions f or o perating J EOL J SM-‐7500FA a nalytical field e mission s canning e lectron m icroscope a t Nanomicroscopy C enterVersion 2.1 (April 2011)Juuso K orhonen (***********************)Latest v ersion o f t his d ocument c an a lways b e d ownloaded f rom:k.fi/en/instruments/sem/jsm-‐7500fa/SEM-‐instructions.pdfOfficial i nformationNew u ser t rainingInexperienced u sers h ave a c ouple o f o ptions, l isted b elow i n t he o rder o f preference.1.Ask f or t raining f rom t he m ost e xperienced S EM u ser o f y ourresearch g roup.2.Attend t o t he c ourses T fy-‐125.4313 a nd T fy-‐125.4314 M icroscopyof n anomaterials (5+5 c r). T hey a re l ectured e ach s pring b y P rof.Janne R uokolainen.3.Ask o ne o f t he a dministrators t o a rrange a t raining s ession.a.Small g roups o f 2-‐3 p eople a re p referred f or t he t rainings.Allow s ome t ime t o g ather e nough p eople f or t he g roup.b.Training i s d one u sing a p ractice s ample a nd p ersonalsamples a re u sually n ot i maged.Experienced u sers c an c ontact o ne o f t he a dministrators f or a s hort introduction t o t he e quipment.Every n ew u ser h as t o b e a pproved b y o ne o f t he a dministrators b efore t hey are a llowed t o u se t he S EM o n t heir o wn. T he a dministrator k eeps a s hort (15-‐30 m in) s ession w here t he e ssential s kills o f t he u ser a re c hecked. User a pplicationUser a pplication h as t o b e f illed i n o rder t o g ain r eservation a ccess t o a ny o f the N MC e quipment. T he f orm c an b e f ound f romk.fi/en/documents/nmc_user_application_form.pdf a nd i t i s returned t o o ne o f t he a dministrators f or a pproval.PricingBilling i s d one u sing t he c urrent N MC p rice l ist. C ontact P rof. J anne Ruokolainen f or t he m ost c urrent l ist. P lease n ote t hat i ndividual t raining given b y t he a dministrators w ill a lso b e c harged.Precautions – r ead c arefully•Always c heck t he l iquid n itrogen l evel a nd f ill i f n ecessary.o First u ser o f t he d ay a lways f ills t he t ank.•Keep a ll p arts c lean a nd c lean t hem i f n ecessary w ith e thanol.o Wear g loves w hen h andling h olders.•Fill t he l og b ook o n t he c omputer.o Mark a ny s trange b ehavior o r p roblems t o t he l og b ook.•If s omething i s m issing f rom t he S EM o r f rom t he s ample p reparation room (e.g. g loves, e thanol, h olders, c arbon t ape), p lease i nform o ne o fthe a dministrators (send e mail o r c all).•Use o nly f eatures y ou a re t rained t o u se. F or e xample, d o n ot u se EDS o r R BEI i f y ou d on’t k now h ow t o o perate t hem s afely.•Use o f U SB s ticks i s s trictly p rohibited d ue t o s ecurity i ssues a nd hardware i ncompatibility.•Stay c alm a nd u se y our c ommon s ense.•Contact a dministrators i f y ou a re i n d oubt. C ontact i nformation i s found o n t he l ast p age o f t hese i nstructions.Quick s tartup p rocedure1.Turn o n b oth m onitors a nd c heck t hat S EM s oftware a nd u sage l og(Excel) a re r unning. S tart t hem i f n ecessary. L og i n a s G uest (nopassword).2.Check t he l iquid n itrogen l evel a nd f ill i f n ecessary. T he f irst u serof t he d ay a lways f ills t he t ank.3.Fill t he u sage l og:a.Date, s tart t ime (and e nd t ime).b.Your n ame (and t he n ame o f y our h ost i f y ou d o n ot h avereservation p ermissions).c.Vacuum l evels b efore s tarting.d.Amount o f f illed l iquid n itrogen (write “0” i f y ou o nlychecked t he l evel).e.Write n otes a nd c omments t o t he l ast f ield i s n ecessary.f.Save t he f ile (Ctrl-‐S).4.Prepare y our s ample.5.Insert s ample i nto m icroscope:a.Press E xchange p osition.b.Press a nd h old V ENT f or c a. 1 s ec. O pen s ecuring l atch. W ait.c.Open c hamber a nd i nsert h older a long t he d irection o f t hearrows.d.Close c hamber.e.Press a nd h old E VAC f or c a. 1 s ec. W ait u ntil b linking s tops.f.Operate t he r od t o m ove t he s ample t o t he s tage. I f y ou’re n otabsolutely c ertain h ow t o d o t his, r ead t he d etailedinstructions!g.Take o ut t he r od.6.Wait u ntil v acuum l evel r eaches l ess t han 5⋅10-‐4 P a.7.Set E mission c urrent t o 10 μA.8.Select A cceleration v oltage.9.Press O bservation O N.Shutdown p rocedure1.Press O bservation O FF t o t urn o ff a cceleration v oltage.2.Press E xchange p osition.3.Take o ut h older u sing t he r od.4.Press a nd h old V ENT f or c a. 1 s ec. O pen s ecuring l atch. W ait.5.Open c hamber a nd t ake o ut t he h older.6.Close c hamber.7.Press a nd h old E VAC f or c a. 1 s ec.8.Mark e nding t ime a nd o bservations t o U sage l og a nd s ave f ile (Ctrl-‐S).9.Set S EM M onitor s oftware t o n ormal s ettings:a.Exchange p osition p ressed (green).b.Mode: S EMc.Magnification: m inimum f or b oth S EM a nd L Md.Probe c urrent: 810.Turn o ff s pecial f eatures y ou h ave u sed: I mage r otation, d ynamicfocus, e tc.11.If y ou m ade a ny c hanges i n t he O peration S ettings m enu, c hangethem t o n ormal v alues (scan s peeds, i mage f unction, e tc.).12.Clean t he h olders w ith e thanol i f n ecessary.13.Clean t ables. I f y ou w ant t o s tore y our s amples, m ark t hem w ith y ourname a nd p ut t hem o nto a s helf. T hings l eft o n t he t able a re t hrowninto t he t rash.14.Transfer y our i mages f rom t he s mall c omputer o n t he b ack t able.You c an f ind y our f iles a t t he n etwork d rive c alled H arley.e U SB s tick, S SH, e mail, o r b urn a C D.b.The f iles c annot b e t ransferred d irectly f rom t he S EMcomputer d ue t o s ecurity r easons.15.Turn o ff m onitors. D o n ot l og o ut f rom t he s oftware o r c lose t heExcel l og b ook.Changing s ample1.Press O bservation O FF t o t urn o ff a cceleration v oltage.2.Press E xchange P osition t o m ove t he s tage t o c orrect p osition.3.Take s ample o ut b y o perating t he r od.4.Press a nd h old V ENT f or c a. 1 s ec. t o f lush c hamber a nd o pen l atch.Wait.5.Open c hamber a nd t ake o ut s ample (pull a long t he a rrows, n ot u p).6.Change s ample a nd i nsert h older a long t he a rrows.7.Close c hamber a nd s ecure w ith l atch.8.Press a nd h old E VAC f or c a. 1 s ec. W ait u ntil b linking s tops.9.Insert s ample b y o perating t he r od. T ake o ut r od.10.Wait u ntil c hamber v acuum r eaches 5⋅10-‐4 P a b efore t urning o nacceleration v oltage.Special f eaturesThis i s o nly a q uick r eference. S pecial t raining i s r equired t o u se R BEI o r E DS, because o f s afety i ssues.Infrared c ameraYou c an s ee i nside t he c hamber u sing t he i nfrared c amera.1.Switch c amera o n f rom t he b utton o n t he t able.2.From S EM s oftware s elect N avigator -‐> I nfrared c amera3.Turn c amera o ff w hen u sing R BEI o r E DS.Probe c urrent m eterProbe c urrent m eter c an b e u sed t o c heck t he c urrent g oing t o t he s ample. I t is m ost i mportant i n E DS a nalysis.1.Insert t he d etector b y c hecking P CD f rom t he b ottom r ight c orner o fSEM s oftware.2.Take o ut d etector a fter y ou h ave r ead t he c urrent f rom t he S EMsoftware.Retractable b ackscattering d etector (RBEI)Backscattering d etector i s u sed t o d istinguish b etween e lements o n t he sample.1.Set w orking d istance t o 8 m m o r m ore.a.Inserting R BEI w ith l ess t han 8 m m b etween t he s ample a ndthe o bjective l ens w ill r esult i n s erious d amage.2.Turn o ff i nfrared c amera.3.Insert d etector b y c hecking R BEI f rom t he b ottom r ight c orner o f t heSEM s oftware.4.Select C OMPO o r T OPO f or i mage m ode (same m enu a s S EM a nd L M)and u ser a s low s canning s peed f or o bservation.X-‐ray a nalysis (EDS)This g uide i s n ot a dequate f or p roper o peration o f E DS, b ut i s o nly a q uick reference f or t rained u sers.1.Set w orking d istance t o e xactly 8 m m.a.Focus w ith Z h eight u sing t he r ing o f t he s croll w heel i nsteadof F OCUS.2.Insert R BEI.3.Turn o n b ias v oltage b y c licking t he l ightning i ndicator.a.Wait u ntil c ount r ate s tabilizes.4.Select A nalysis f rom t he r ight s ide o f S EM s oftware.5.Click D T (dead t ime) a nd s elect T4 f rom t he l ist.6.Adjust p robe c urrent s o D T b ecomes g reen (around 20-‐30 %) a ndcount r ate i s c a. 2000-‐3000 c ps.7.Take s pectra, l ine s can, o r m apping u sing t he a ppropriate b uttons.8.When a sked a bout s aving t o a n etwork d rive, s elect O K.9.Save t he a nalysis b efore e xiting a nalysis m ode i n o rder t o b e a ble t oreturn t o t he a nalysis l ater.a.Exporting o nly s aves t he i mage a nd y ou c annot r eturn t omake m ore a nalysis o n t he d ata.10.When y ou a re f inished w ith a nalysis, t urn o ff t he b ias v oltage a ndtake o ut R BEI.Saving E DS s pectraIf y ou w ant t o b e a ble t o p lot y our E DS s pectrum, s elect E xport a nd t hen select M SA f ile. I t w ill s ave t he s pectrum i n a c ompatible f ile f or u se i n O rigin, Excel, o r s ome o ther p lotting p rogram.Detailed i nstructionsOperating t he r od (sample e xchange m echanism)This p rocedure d escribes h ow t o u se t he s ample e xchange m echanism i norder t o e ither r emove o r i nsert a s ample h older i nto/from t he m icroscope.Read t his s ection c ompletely t hrough b efore p roceeding a nd m ake s ure t hatyou u nderstand e very s tep.Precondition: T he e xchange c hamber i s i n v acuum a nd t he d oor s eparatingit f rom t he m icroscope i s o pen. C onfirm t hat E VAC l ight i s l it a nd n otblinking. D epending o n w hether y ou a re i nserting o r t aking o ut a s ample, t heholder m ight b e i n t he e xchange c ompartment (HLDR l ight i s o ff) o r i nsidethe m icroscope (HLDR l ight i s o n).See t he v ideo o n t he c omputer d esktop f or a d emonstration. U PDATE: T hefigures a re f rom a n o ld v ersion o f r od.1.Push t he b ar i nside t he m icroscope b y f ollowing t he p rocedure:a.Lower t he r od t o h orizontal l evel, w hile l ightly h olding i tback.b.Let t he r od b e p ulled i n s lowly.c.Push t he b ar g ently a ll t he w ay i nside u ntil i t s tops (d).•There i s a l ittle r esistance a t t he f inal c ouple o fcentimeters.•The s ample s hould b e n ow e ither r eleased f romthe b ar o r a ttached t o i t (depending o n w hetheryou a re i nserting o r r emoving t he h older).•If y ou h ave n ot p ushed t he s ample a ll t he w ayinside a nd s tart t o p ull b ackwards t here i s adanger t hat t he s ample h older w ill f all t o t hebottom t he s ample c ompartment. I f t his h appens,the w hole s ample c ompartment h as t o b e o pened.Contact S EM a dministrators i n t his c ase.2.Pull t he b ar o ut f rom t he m icroscope u sing t he f ollowingprocedure:a.Pull t he b ar o ut a s f ar a s i t c omes (e).•The t wo a rrows o n t he h older s hould a lign w iththe p ipe e nd.•If y ou h ave n ot p ulled f ar e nough, t he r od m ightbe d amaged d uring t he l ift.b.Lift t he r od u pwards t o v ertical.•Now y ou s hould e ither h ave t he s ample i nside t hemicroscope o r i n t he e xchange c ompartment a ndthe e xchange c ompartment i s i n v acuum.Opening t he s ample e xchange c ompartmentThe f ollowing p rocedure d escribes h ow t o b ring t he e xchangecompartment t o a tmospheric p ressure.Precondition: T here i s n o s ample i nside t he m icroscope o r i t h as b eenbrought t o t he e xchange c ompartment, a nd t he e xchange c ompartment i sin v acuum. F irst c heck t hat H LDR l ight i s o ff o n t he s ample e xchangecompartment (i.e. t here i s n o s ample i nside t he s ample c ompartment).Figure. S ample e xchange r od1.Pressurize t he e xchange c ompartment:a.Press a nd h old (for a bout 1 s econd) t he V ENT b utton o n t heexchange c ompartment.i.The b utton s tarts t o b link a nd y ou h ear s ome s ounds.ii.In a f ew s econds, t he d oor b etween t he e xchangecompartment a nd t he s ample c ompartment c loses.You c an o bserve t his b y e ar a nd b y l ooking a t t hebottom r ight c orner o f t he S EM M onitor.2.Open t he l atch a s s oon a s y ou h ear t he c lick.3.Open t he e xchange c ompartment d oor (it s hould o pen a lmost b yitself).a.You d o n ot n eed t o w ait u ntil t he p umping h as s topped.b.The c ompartment w ill c ontinue p urging f or a f ixed a mount o ftime. Y ou d o n ot h ave t o w ait u ntil i t s tops a nd y ou c anevacuate i t a s s oon a s y ou l ike.4.Now y ou h ave t he s ample c ompartment o pen a nd r eady f orloading/unloading t he s ample h older.Inserting a s amplePrecondition: T here i s n o s ample i nside t he s pecimen c hamber a nd exchange c ompartment i s i n v acuum. F irst c heck t hat H LDR l ight i s o ff o n the e xchange c ompartment (i.e. t here i s n o s ample i nside).1.Move t he s tage t o e xchange p osition:a.Click E xchange P osition o n t he S EM M onitor.i.If b utton i s n ot v isible, c lick "Specimen" f rom t herightmost e dge o f S EM M onitor.ii.Make s ure t hat E XCH P OSN i s l it o n t he e xchangecompartment, b efore p roceeding.2.Bring t he e xchange c ompartment t o a tmospheric p ressure b yfollowing p rocedure i n s ection “Opening t he s ample e xchangecompartment”. Q uick n otes:a.Press a nd h old V ENT f or c a. 1 s ec.b.Open l atch. W ait.c.Open c hamber d oor.3.Put o n g loves i f y ou d o n ot h ave t hem a lready o n.a.Parts t hat a re i n c ontact w ith t he v acuum s hould b e k eptabsolutely c lean. I f y ou h ave t ouched s ome p art, c lean t he p artwith e thanol (not a cetone).4.Insert h older t o t he s pecimen c huck:a.Slide t he s pecimen h older i nto t he s pecimen c huck a long t hearrow d irection o n t he s pecimen h older.5.Check t hat t he O-‐ring s eal o n t he d oor i s O K a nd w ipe i t w ith a c leanglove i f n eeded t o g et r id o f a ny d ust.a.If t he r ing i s r eally d irty, w ipe i t w ith e thanol o r i sopropanol(do n ot u se a cetone o r m ethanol).6.Close t he c hamber d oor a nd s ecure i t w ith t he l atch.7.Evacuate t he c ompartment b y p ressing a nd h olding E VAC (forabout 1 s econd). T he l ight w ill s tart b linking.a.Wait u ntil t he l ight s tops b linking a nd t he d oor s eparatingthe e xchange c ompartment i s c losed. Y ou c an o bserve t hisfrom t he b ottom r ight p art o f t he S EM M onitor.8.Insert t he s ample h older i nside t he m icroscopea.Refer t o s ection “Operating t he r od” i f i n d oubt.9.A p opup w indow s hould a ppear o n t he S EM M onitor. N ow s elect t heappropriate h older a nd s et t he o ffset v alue.a.If p opup d oes n ot a ppear, t ake o ut t he h older a nd i nsert i tagain.10.Wait u ntil t he v acuum l evel r eaches 9.6·10-‐5 P a (if t hat i s n otpossible, w ait a t l east u ntil 5·10-‐4 P a).Taking o ut s amplePrecondition: T here i s a s ample i nside t he m icroscope a nd e xchange compartment i s i n v acuum. F irst c heck t hat H LDR l ight i s o n o n t he s ample exchange c ompartment (i.e. t here i s a s ample i nside) a nd E VAC l ight i s o n and n ot b linking.1.Click O bservation O FF t o t urn o ff a cceleration v oltage.2.Click E xchange P osition t o m ove t he s ample h older t o t he e xchangeposition.a.Make s ure t hat E XCH P OSN i s l it o n t he e xchangecompartment b efore p roceeding.3.Bring t he s ample t o t he e xchange c ompartment b y o perating t herod.a.Refer t o s ection “Operating t he r od” i f y ou a re n ot a bsolutelycertain h ow t o d o t his.4.Pressurize t he e xchange c ompartment:a.Press a nd h old V ENT f or c a. 1 s ec u ntil i t s tarts t o b link.b.Open s ecuring l atch. W ait.c.Open c hamber d oor.5.Now y ou h ave t he s ample c ompartment o pen a nd y ou a re r eady t akeout y our s ample. I f y ou a re d one w ith t he i maging, j ust c lose t heexchange c hamber a nd e vacuate i t o therwise c ontinue w ith i nsertinga n ew s ample. D o n ot l eave t he c hamber o pen f or a l ong p eriod o ftime, b ut e vacuate i t i f n eeded.Sample h oldersSample h olders c onsist o f a b ase p art a nd a n a dapter p art (show o n t he f igure right). T here a re t hree d ifferent a dapters f or d ifferent s pecimen s tubs s hown in t he f igure b elow (a, b , c , d ).The m ost b asic h olders a re t he 12.5 m m (b-‐1) a nd 25 m m (c-‐1) a luminum “JEOL” s tubs . T hey s hould b e u sed w henever p ossible. S tubs s hould a lways b e available a t t he s ample p reparation r oom, b ut y ou c an a lso o rder y our o wn ones e .g. f rom E MS (order n umbers 75730, a nd 75700). T he u se o f r egular holders i s i ncluded i n t he o peration p rice o f t he m icroscope.Also “mini-‐stubs” a re a vailable f or u se w ith a p rovided a dapter. T hey a re preferred f or s mall s amples. T hey c an b e o rdered f rom T ed P ella (order numbers 16180, a nd 16181).For s pecial o ccasions, a H itachi a dapter (a) c an b e u sed. S pecial c are m ust b e taken w hen u sing t hese h olders, b ecause t hey l ack s ome s afety f eatures. Ask a dministrators, i f y ou h ave s pecial r equests f or h olders. T here a re a lso different k inds o f c ross-‐section h olders a vailable. A sk t he a dministrators f or more i nformation.Attaching a dapter t o b ase p arta) Make s ure t hat p arts a re n ot d irty, c lean i f n ecessary. b) Place a dapter o n t he b ase p art.c) Tighten s crew o n t he b ase p art l ightly.Figure. A ttaching a dapter t o base p art.Figure. 12.5 m m a nd 25 m m "JEOL" stubs.Figure. "Mini-‐stubs" a nd 12.5 m m a dapter.Figure. C ross-‐section holders.Sample h eightAlign t he t op o f t he s ample w ith t he g roove i nside t he J EOL a dapter p art. U se the s crew o n b ottom t o r aise o f l ower t he s ample. W hen u sing a nother holder, m ake s ure t hat h eight f rom t able t op l evel i s e xactly 25 m m.CoatingFor n on-‐conductive s amples a c oating i s u sually n eeded f or o bservation i n SEM. T his c an b e e asily p erformed b y u sing s putter c oating o f g old, p latinum, or g old-‐palladium. T here i s a s putter c oater a t N MC, w hich c an b e u sed f or this p urpose. R esolution l imiting f actor i s t he g rain s ize, w hich i s u sually 5-‐20 nm d epending o n t he c onditions o f s puttering.Also c arbon c oating c an b e u sed t o m ake s amples c onductive. I t i s a nappealing m ethod, w hen d oing X -‐ray a nalysis. I t c reates a v ery u niform l ayer without n oticeable grains.Figure. A lign t op o f stub w ith t he g roove on t he s ample holder.Basic m icroscope o perationBasic c onceptsWorking d istance a nd Z v alueWorking d istance (WD) v alue s ets t he e ffective f ocal l ength o f t he o bjective lens.Z h eight v alue s ets t he d istance o f t he (supposed) s urface l evel o f t he s ample from t he o bjective l ens.These t wo v alues a re e qual, w hen t op o f s ample i s a ligned w ith t he t op o f the h older (ie. 25 m m h igh f rom t able l evel, s ee f igure). W D > Z, i f y our sample i s l ower t han t he c orrect l evel a nd v ice v ersa. I f W D < Z y ou n eed t o set t he S ample O ffset v alue a ccordingly.Sample o ffsetThe h eight o f t he t op l evel o f t he s ample m easured f rom t able t op l evel should b e e xactly 25 m m. T he s ample c an b e s et a lso 0-‐4 m m h igher t han t he nominal l evel, b ut t hen t he S ample O ffset v alue h as t o b e s et a fter i nserting sample. I t i s l ocated a t t he b ottom o f t he s ample h older s elect w indow, w hich pops u p a utomatically a fter h older i nsert.Acceleration v oltage, e mission c urrent, p robe c urrent…The f irst t hing t o t hink a bout w hen s tarting i maging i s t he s election o f acceleration v oltage. T he c hoice d epends o n t he t ype o f t he s ample. S ee table b elow f or s ome e xamples.Sample Observation c ondition NotesGold p articles o n conductive s urface 5-‐30 k V, p robe c urrent a t c a. 10, working d istance 1.5-‐8 m mCoated p orous polymer 1-‐5 k V, p robe c urrent 6-‐10, w orking distance 4.5-‐8 m mUncoated p olymer 0.5-‐1 k V, p robe c urrent < 8, g entlebeam m ode, w orking d istance c a. 8mmCoated b iological sample 1-‐5 k V, p robe c urrent c a. 10, w orking distance 4.5-‐25 m m d epending o n feature s izeUncoated p aper 1-‐2 k V, g entle b eam (GB-‐L) m ode,working d istance 4.5 m m, p robecurrent 6-‐10.Coated p aper 5 k V, w orking d istance 4.5-‐25 m m,probe c urrent c a. 10X-‐ray a nalysis o f conductive s ample 15-‐30 k V, w orking d istance e xactly 8mm, h igh p robe c urrentRetractable B EIdetector i nsertedX-‐ray a nalysis o f poorly c onductive sample 5 k V, w orking d istance e xactly 8 m m,probe c urrent a s h igh a s p ossibleRetractable B EIdetector i nsertedThe e mission c urrent i s t he c urrent d rawn f rom t he e mitter. S et i t a lways t o 10 μA. Figure. S ample height s hould b e exactly 25 m m measured f rom t able top l evel.Probe c urrent i s t he c urrent d irected a t t he s ample. H igher v alues g ive better s ignal t o n oise r atio, b ut c ause m ore c harging a rtefacts i n p oorly conducting s amples. V alue o f 8-‐10 i s u sually a g ood c hoice.AligningUsually t he m icroscope i s a ligned w ell e nough f or m icrometer s cale operation. I n t his c ase, o nly f ocusing i s n ecessary. F or h igher m agnification work, t he e lectron b eam n eeds t o b e a ligned a nd a stigmatism o f t he o bjective lens h as t o b e c orrected.FocusThe f irst l evel o f a ligning i s a lways f ocusing. F ocusing i s d one u sing t he FOCUS k nob o n t he o peration c onsole. C lockwise r otation i s u nder f ocus (weaker l ens) a nd c ounterclockwise i s o ver f ocus (stronger l ens).If p ossible s elect s ome f eature, w hich y ou c an u se i n t he m agnification r ange from c a. 1000 t o 20000.Start f rom a l ow m agnification a nd w hen y ou g et g ood e nough i mage m ove on t o h igher m agnification f or f ocusing. I t t he a lignments a re r eally o ff, y ou might n ot g et a c lear i mage a t a ll.Beam a lignBeam a lign i s a lways d one a t p robe c urrent 8. S elect t he c orrect p robe current v alue f rom t he s oftware.Press A LIGN o n o peration c onsole. T he i mage s tarts t o m ove o n t he s creen. Use t he X a nd Y k nobs t o m inimize t he m ovement. P ress A LIGN O FF (STIG) button w hen i mage h as s topped. R epeat f or m agnifications u p t o c a. 20000. Focus t he i mage w henever n ecessary.Astigmatism c orrectionTo c orrect t he o bjective l ens a stigmatism p ress t he S TIG b utton o n t he operation c onsole (it i s u sually a lready s elected a t t his p oint). M ove o n t o a spherical f eature, w hich y ou a re a ble t o o bserve a t m agnification 10000 o r more.Move t he F OCUS k nob s o t hat y ou g o f rom u nderfocus t o o verfocus a nd b ack several t imes. W hen y ou h ave a stigmatism, t he i mage g ets e longated i n diagonal d irections w hen m oving a round t he f ocal p oint. S elect t he f ocal point w here n o e longation o ccurs.Adjust t he X a nd Y k nobs s o t hat y ou g et t he c learest i mage p ossible. F ocus whenever n ecessary.Other c orrectionsThere a re a lso o ther a lignments, s uch a s s ource a lign, c ondenser l ens astigmator, l ow m agnification c enter, a nd s tigmator c enter c orrections. These v alues s hould n ot u sually b e c hanged a nd t heir u se i s n ot d escribed here.Problems a nd t roubleshootingAnswers t o c ommon p roblemsI w ant t o u se U SB s tick t o t ransfer m y f iles!You c an t ransfer y our f iles t o a U SB s tick f rom t he s mall c omputer a t t he b ack wall. Y ou’ll f ind y our f iles u nder t he n etwork d rive H arley.Help! T here i s n o i mage.Follow t he c hecklist t o f ind t he c ause:1.Are y our Z a nd W D v alues t he s ame? I f n ot p ress W D t o s et c orrectdistance.2.What d etector a re y ou u sing? I f W D<8 m m y ou u sually d o n ot g etimage w ith L EI d etector; a nd i f W D>8 m m S EI g ives o nly s tatic n oise.LM m ode s hould w ork f ine i n t his c ase.3.What i s y our p robe c urrent v alue? I f i t i s l ow, t ry i ncreasing i t.4.If n one o f t he a bove i s t rue, t ry r esetting a lignment. G o t o A lignmentpanel a nd c lick R eset A ll.a.In a r eally b ad c ase t he s ource a lignment h as g one b ad.Contact a n a dministrator t o a lign i t.If t here i s n o i mage w hen s tarting o perationFirst, p ress A CB (auto c ontrast & b rightness). I f y ou e ven s ee s ome s tatic noise, y ou o nly n eed t o f ind t he c orrect f ocal p oint. S ee p revious s ection.In c ase y ou h ave c ompletely b lack s creen w hen y ou s tart i maging, f ollow t he list u ntil y ou h ave i mage.1.Restart o f S EM s oftware:a.File-‐>Exit t o g o t o l ogin s creen.b.Close l ogin s creen f rom E xit b utton.c.Wait o ne m inute.d.Start S EM_Monitor s oftware.e.Log i n a s G uest.2.Restart c omputer:a.Close S EM s oftware.b.Save E xcel l og b ook a nd e xit.c.Restart W indows.d.Start S EM s oftware a nd E xcel l og b ook.3.Restart o peration c onsole:a.Read i nstructions b elow.If v acuum b reaks d uring s ample e xchangeVacuum u sually b reaks i f t he l ever i s p ushed o r t wisted d uring t he s ample insertion. T he c omputer w ill r aise a m aintenance w indow s howing e rror messages. T he m icroscope w ill a utomatically s hut d ownsome p arts a nd t he v acuum p umps h ave t o b e r estarted. B ring t he microscope b ack t o i ts n ormal c ondition b efore p roceeding. F or e xample, lift t he r od b ack t o i ts u pright p osition.1.Locate t he t wo V AC S W b uttons b elow t he t able. T here a re a lso M AINSW b uttons, b ut d o n ot t ouch t hem.2.Shut d own v acuum p umps b y p ressing V AC O FF (0=OFF, 1=ON)button. T he p umps s hould n ow s top, i f t hey w ere n ot s hut d ownalready.3.Wait a m oment a nd r estart p umps b y p ushing V AC O N b utton.a.There i s a 20 m in t imer f or s tarting t he p umps s o y ou w illhave t o w ait a t l east 20 m inutes b efore p roceeding.4.After a ll o f t he e rror m essages h ave d isappeared f rom t he d isplay,you c an c ontinue o perating.Turning o ff c omputer1.Log o ut f rom t he S EM s oftware (File-‐>Exit).2.Save t he E xcel l og b ook (File-‐>Save o r C trl-‐S).3.Close t he E xcel l og b ook.4.Select S hutdown f rom S tart m enu.Powering o n c omputer1.Start c omputer f rom t he p ower s witch.2.Log i n a s S EMUser (password: S EMUser).3.Start E xcel l og b ook b y d ouble c licking “SEM U sage L og” o n t he r ightmonitor d esktop.4.Start S EM s oftware b y d ouble c licking S EM_Monitor.5.Log i n a s G uest.Restarting o peration c onsole1.Turn o ff c omputer.2.Press O P S W O FF f rom b elow t he t able.3.Wait c a. 10 s econds.4.Press O P S W O N.5.Turn o f c omputer.6.Wait a c ouple o f m inutes b efore s tarting S EM_Monitor s oftware.。
FESEM 简介
6. 非导电性样品的观察
• 表面喷镀 • 使用低的加速电压 • 选用Mode 0、1 • 使用LDD
7. 关于Flash
自动设定：
NF：1次／15小时 SF ：1次／150小时
连续使用时推荐：NF：1次／4～5小时
Flash后等30～60分钟后再使用电镜
四. JSM-6700F的日常维护
• 机械泵油、油过滤器每1～2年更换一次 • 物镜光阑、噪声消除器光阑每1～2年更换一次 • 发射体寿命1年以上 • 冷却水3～6个月更换一次 • 氮气2～3个月1瓶
分辨率 ： 15KV 1KV
1.0nm 2.2nm
样品台 移动范围： X ：70 mm Y：50 mm Z: 1.5~25mm
R: 360°无限旋转 T: -5°~ 60°
3. 真空系统
4. 关于样品
可用的最大样品尺寸： Ⅰ： 直径 80 mm Ⅱ： 直径 160 mm Ⅲ： 直径 200 mm
样品与样品座最大高度差：3 mm
样品其它要求：
导电、固态、无磁、无挥发气体、干样品
5. 观察时的样品污染
• 现象：观察区域变黑
• 成因：样品表面残余有机气体分子在电子辐照下交联， 从而在表面形成聚合膜。
• 对策：减少有机气体分子
a. 用甲醇清洗样品 b. 200～300℃充分烘烤样品 c. 使用冷阱
一. 扫描电子显微镜基本原理 二. 场发射电子枪的特点 三. JSM-6700F的特点及应用 四. JSM-6700F的日常维护
一. 扫描电子显微镜的基本原理
1. 光波与电子波
光波 ：波长300～750 nm，分辨率极限0.2μm. 电子波Biblioteka 分辨能力与电子束入射锥角和波长有关
场发射扫描电镜技术标书
场发射扫描电镜技术标书附件：场发射扫描电镜技术标书一、设备用途扫描电镜是一种多功能的仪器，广泛地用于材料的微观组织观察、微区成分分析、材料的断口分析、材料的晶粒度分析、夹杂物分析及织构表征等，可对导电及不导电的固体材料进行表面形貌的观察及成分分析。
场发射电镜能够实现更高分辨率的形貌观察，可实现对超细晶材料尤其是纳米材料的表征。
基于相关附件，也可以对材料在温度及应力作用下的动态变化进行原位观察。
仪器包括电子光学系统、真空系统、样品室和样品台、探测器及成像系统、图像处理系统、应用软件及数据处理软件、X射线能谱分析仪（EDS）、背散射电子衍射分析仪（EBSD）、原位加热台。
二、技术参数1．运行环境1.1工作温度：可以在15~25环境温度工作1.2 相对湿度：湿度小于60%RH时正常工作1.3工作电压：在220V(±10%)、50Hz电压下，仪器可连续使用次电子探测器1个，高灵敏度低电压固体背散射探测器1个4.3相机：样品室红外高清CCD相机4.4检测器分辨率*4.4.1二次电子分辨率：30kV时小于1.0nm或20kV时小于1.3nm，1kV时优于3.0 nm*4.4.2背散射电子分辨率：30kV时小于2.5nm，1kV时优于3.0nm5．样品室和样品台5.1样品台：自动马达驱动5轴以上(X、Y、Z 、T 、R)*5.2移动范围：X≥100mm、Y≥ 100mm、Z≥50mm、T=-5~70°、R=360°连续旋转5.3移动精度：优于2μm5.4样品室尺寸：内径不小于300mm，高度不小于200mm，可容纳样品直径不小于200mm5.5样品室有EDS、EBSD接口*5.6可加配加热台和原位拉伸台，加热台运行时应保证成像系统和EBSD能够同步运行6．图像处理系统6.1存储分辨率：不低于30002000像素6.2活动窗口：多个活动窗口，可同时显示背散射及二次电子图像6.3图像格式：TIFF、BMP、JPEG等多种图像格式6.4图像帧数：不小于256帧，可降噪处理6.5能够进行数字动画记录6.6具有图像注释、测量等图像处理功能7．控制和数据处理系统7.1基于以太网架构的数据传输系统7.2软件平台适用于windows操作系统7.3显示器：24”LED显示器8．X射线能谱分析仪（EDS）8.1能量探测器：电制冷硅漂移探测器（SDD）*8.2有效采集面积：SDD晶体有效活区面积不小于30mm2，窗口有效面积不小于20mm2，可实现低电压或者小束流条件下的高质量、高效率分析*8.3探测器定位：探测器由马达控制精确定位，软件可控，能够实时监测和控制采集计数率，保证不同样品的数据重复性和测试条件重复性的目的*8.4能量分辨率：Mn Kα优于127eV，C Ka优于50eV，F Ka优于60eV8.5元素分析范围：至少为Be4~U92*8.6峰背比：优于20000:18.7谱峰稳定性：分辨率变化在1eV以内，48小时内峰位漂移小于1.5eV8.8计数率：输出最大计数率大于800,000CPS，可处理最大计数率大于1,500,000CPS8.9具有轻元素定量分析和修正功能，可对Be、B、C、N等进行浓度定量检测以及修正8.10采集界面：采用32位和64位双系统，采集界面方便简单，智能化设定参数，兼容原有EBSD数据，能实现能谱的采集与定量分析、线扫描及全息面扫描，包含常规面分布、定量面分布和快速面分布、快速智能面分布等*8.11定性分析：具备点、线、面扫描分析功能，可自动和手动进行全谱元素谱峰识别，并具有检验重叠峰剥离准确性以及合峰效应的有效方法，能够分析夹杂和偏析等微量元素和微量相8.12定量分析：采用最先进的修正技术和虚拟标样数据库，系统能够自动有效修正元素之间的相互吸收，可对抛光表面或粗糙表面进行点、线和面的分析，谱峰稳定，数据重现性好，不需要多元素校准峰位。
场发射扫描电子显微镜使用方法说明书
场发射扫描电子显微镜使用方法说明书一、引言场发射扫描电子显微镜（以下简称场发显微镜）是一种高分辨率的显微镜，利用电子束与样品相互作用产生的信号来获取样品表面的形貌和结构信息。
本说明书将详细介绍场发显微镜的使用方法，帮助用户正确操作和利用该仪器。
二、仪器准备在使用场发显微镜之前，需进行以下准备工作：1. 保证实验室环境在恒定的温度和湿度下，避免影响仪器性能。
2. 检查仪器电源和相关线缆的连接是否牢固，并确保电源供应稳定。
3. 准备待观察的样品，并确保样品表面干净、光滑。
三、开机及基本操作1. 打开仪器电源，待仪器完成自检后，进入操作界面。
2. 鼠标操作：使用鼠标控制光标移动至所需功能区域，并点击打开相应功能菜单。
3. 设置扫描参数：选择扫描模式、像素大小等参数，以适应不同样品的观察需求。
4. 样品安装：将待观察的样品安装到样品台上，并使用调节螺丝微调样品的位置，保证与电子束的最佳对准。
5. 自动对焦：使用自动对焦功能，校准焦距，确保样品图像清晰可见。
四、图像观察与分析1. 扫描图像获取：点击“扫描”按钮，开始获取样品表面的扫描图像。
图像会逐行扫描，根据设定参数生成图片。
2. 放大与缩小：使用鼠标左键点击图像区域，可进行图像的放大和缩小操作。
右键点击可还原图像原始大小。
3. 焦点平移：使用光标控制器或滚轮移动焦点位置，观察样品各个区域的细节。
4. 图像调节：根据需要调整图像的亮度、对比度等参数，以获得更清晰的图像。
5. 图像保存：观测到满意的图像后，点击“保存”按钮，将图像保存到指定路径，便于后续分析与报告撰写。
五、仪器维护与操作注意事项1. 仪器维护：固定时间段内对仪器进行清洁和维护，清除积尘，以保证仪器正常运行。
2. 样品处理：在安装样品之前，确保样品表面干净，避免影响观察效果。
避免使用尖锐物体接触样品，防止刮伤样品表面。
3. 仪器操作：在操作中避免突然断电，以免损坏仪器设备。
操作完毕后，及时关闭仪器电源。
场发射扫描电镜操作规程
21．按样品室操作面板上的“EVAC” 指示灯，使样品交换室保持真空状态。
22．选择菜单栏中的“File” 菜单下的“Exit”选项，退出扫描程序。
23．关闭电脑。
二、注意事项：
1．做完“Flash”30秒后，才可以进行扫描操作；先做“Normal Flash” 再做“Strong Flash” 且两次Flash 之间要间隔30秒以上。
点击工具栏中的tool按钮弹出maintenance窗口打开gunpmtvac标签查看真空室和过渡室的真空度是否在指定范围枪室真空度不能小于5108过渡室真空度不能小于5106打开instrumentflash标签点击normalflash选项清除枪表面吸附的气体等杂质
场发射扫描电镜操作规程
一、操作流程
13．调节操作面板上的放大倍数，焦距，亮度，对比度，像散等旋钮，获得清晰的图像。
14．按操作面板上的“Freeze”按钮，锁住图像。
15．点击“File”菜单下的“Image File Handling”选项，打开“Load/Save/Print Image”窗口。
16．点击“Export”或“Save”按钮，输入文件名及有关信息后，点击“Save”按钮，则样品的图像被存储在文件中。
4．确认工具栏中的加速电压按钮“HT”为兰色，选择“Stage”菜单下的“Exchange” （或点击工具栏中的“Speciman Exchange”按钮），打开“Sample Exchange”窗口，选择要使用的样品夹，点击“Exchange 1”。
5．旋转工作距离旋钮使WD为8mm，倾斜角为0o，当屏幕左下角指示的样品台的位置显示为“X=35.0, Y=25.0, R=0”且样品室操作面板上的“EVAC”和“EXCH POSN”指示灯亮时，按“VENT”指示灯，该灯闪烁，氮气进入样品交换室。
JEOL JSM-7900F 型 Schottky 场发射扫描电子显微镜 说明书
Ultimate Analytical tool1J S M-7900FSince the development of the first commercial SEM in 1966, JEOL has continued to be atthe forefront of technology innovation and has continually contributed to the advancement ofscience through its SEM technology.The JSM-7900F is a flagship model of a field emission scanning electron microscope (FE-SEM),which aims to facilitate research and technological breakthroughs for future generations. TheJSM-7900F successfully combines ultrahigh-resolution imaging, ultrahigh spatial-resolutionanalysis and higher operability, as well as multi-purpose functions. This new-generation SEMprovides the best data fidelity with the utmost ease of operation.2J S M-7900FUltrahigh spatial resolution ❖ In-lens Schottky Plus FEGThe in-lens Schottky Plus field emissionto the combination of the electron gunelectron gun can be efficiently focused, enabling probe currents on the order of a few pA to several tens of nA even at low accelerating voltages. High-resolution observation is easy, with no need to exchange the objective aperture for tasks from fast elemental mapping to EBSD, CL or WDS analysis.Conventional Schottky FEG Electron gun ❖ Super Hybrid Lens (SHL)The JSM-7900F comes with JEOL’Hybrid Lens (SHL)”. This powerful lens enables observation and analysis of any specimens at ultrahigh spatial-resolution, including magnetic and insulating materials.❖ GBSH-S（GENTLEBEAM Super High resolution）GBSH enhances resolution atvoltages.A newly developed GBSH-Svoltage up to 5 kV to be appliedstage.❖ Detector systemSimultaneous signal acquisitiondetectors is enabled.The JSM-7900F comes with LEDdetector) and UED (upper electronin-lens detector). In addition,(upper secondary electron detector)High spatial resolution observationSpecimen: Nano rod of TiO*Specimen courtesy: Shanghai Jiao Tong UniversityProfessor Shunai CheAcc. Vol.: 0.3 kV (GBSH)Signal: Secondary electronsDetector: UEDMagnification: ×120,000, ×300,000＊Reference： S. Liu, L Han, Y. Duan, S. Asahina, O. Terasaki, Y. Cao, B. Liu, L. Ma, J. Zhang, S. Che*, " Synthesis of Chiral TiO Nano fiber with Electron Transition-Based Optical Activity” Nature communications, 3, Article number 1215, 2012Specimen: Ag nanoparticlesSpecimen courtesy: Yamagata University Prof. M. Kurihara and Assistant Prof. T. Togashi Acc. Vol.: 5 kV (GBSH)Signal: Backscattered electronsDetector: RBEDMagnification: ×100,000, ×350,000Oxide nanomaterials Metal nanoparticles10 nm100 nm100 nm10 nm 5J S M-7900F1 μmSpecimen: Cross section of stainless steelinterconnect milled by CPAcc. Vol.: 7 kV (GBSH)Signal: Low angle backscattered electrons Detector: RBEDMagnification: ×120,000, ×200,000Specimen: Solder of Ag, Sn and Cu Acc. Vol.: 5 kV Energy filter: -0.5 kV Signal:High angle backscattered electrons (with UED)Secondary and backscattered electrons (with LED)Detector: UED, LED Magnification: ×7,000Simultaneous signal acquisitionSteel materials1 μm100 nm100 nm Signal differentiation–Applications obtained by a variety of detectors–Compositional and crystalline information Topographic informationMetal materials6J S M -7900FJSM-7900FUltimate Analytical Tool of Next-generationHigh vacuum （10-5 Pa）10 μmThe low vacuum function easily suppresses charging of an insulating specimen.Mg KC K3 μm3 μm3 μmSpecimen: Fractured surfaceof coffee beanAcc. Vol.: 5 kV Vacuum: 150 Pa Magnification: ×500Low vacuum functionLow vacuum (150 Pa)10 μm【EDS analytical conditions】Acc. Vol.: 5 kV, Vacuum: 150 Pa, Magnification: ×900, JED 100 mmEDS detector used7J S M -7900FLow vacuum function–Observation at high magnification–The JSM-7900F provides high spatial resolution even in low vacuum. These images demonstrate that inorganic fillers contained in an organic film on a glass are clearly observed.1 μm1 μmGlass100 nmSpecimen: Fractured surface of organic film on glass Acc. Vol.: 5 kV Vacuum: 150 PaSignal: Backscattered electrons Detector: LVBEDMagnification: ×7,000, ×10,000, ×100,000Magnification: ×7,000Magnification: ×10,000Magnification: ×100,000OrganicfilmGlass8J S M -7900FJSM-7900FUltimate Analytical Tool of Next-generationFilter set: +0.3 kVFilter set: -0.1 kV Filter set: -1 kV 3 μmOperability–Extended automatic functions–Soft materials❖ Neo EngineThe JSM-7900F is equipped with a new electron-optical control system, “Neo Engine/New Electron Optical Engine”, which accumulates JEOL’s superb electron optical technologies. Neo Engine achieves further ease of operations of automatic functions.❖ New platformNew exterior design, with no operation console, dramatically reduces the instrument footprint. Thus, the JSM-7900F accommodates a variety of installation environments.❖ New specimen exchange systemA newly designed specimen exchange system (load lock) is adopted for simple specimen exchange, higher throughput, and higher durability.❖ SMILENAVISMILENAVI is an operation navigation system, which is developed for beginners to grasp basic SEM operations efficiently.Improved operability Specimen: Name card, Acc. Vol.: 15 kV, Detector: UED, Magnification: ×3,500Seamless energy selection using a new energy filterOperability–Extended automatic functions–Specimen: Cross section of mineral (resin-embedded) milled by CP, Acc. Vol.: 5 kV, Detector: RBED, Magnification: ×100,000Automatic functions, with greatly improved precision, allow for beginners to easily acquire a high-magnification image.100 nm100 nmSecondary electronsBackscattered electrons9J S M -7900FOperability–New specimen exchange system–Operability–SEM Supporter for image acquisition support–A new specimen exchange system is adopted. The new system achieves simpler and smoother specimen transfer via guided operations. This capability enables fast specimen exchange for beginners to experts.The SEM Supporter of SYSTEM IN FRONTIER INC. enables automatic line width measurement (metrology) utilizing the contrast of SEM images.【SEM observation】Specimen: Specimen for metrology (MRS5)Acc. Vol.: 10 kVMagnification: ×50,000100 nmSpecimen exchange rodSpecimen exchange chamberOperability– SMILENAVI –SMILENAVIGUI screenSMILENAVI is an assistant tool designed for beginners to allow smooth SEM basic operations. When the operator clicks an icon button according to the SMILENAVI flowchart, the SEM GUI screen is linked to the click operation for guiding the operations.ClickAssistInterlock10J S M -7900FJSM-7900FUltimate Analytical Tool of Next-generationUnit ：mm3000 or morePower1000 or more2800 o r m o r e＊Specifications subject to change without notice.No. 1301G755C Printed in Japan, Kp。
Thermo Fisher EVOS M7000 荧光显微镜说明书
EVOS ™ M7000 Imaging SystemFor fluorescence and transmitted light applicationsCatalog Number AMF7000Pub. No. MAN0018380 Doc. Part No. 710246 Rev. A.0Note: For safety and biohazard guidelines, see the “Safety” appendix in the EVOS ™ M7000 User Guide (Pub. No. MAN0018326). Read the Safety Data Sheets (SDSs) and follow the handling instructions. Wear appropriate protective eyewear, clothing, and gloves.This document is intended as a benchtop reference for the users of the EVOS ™ M7000 Imaging System (Cat. No. AMF7000). See the EVOS ™ M7000 User Guide for detailed instructions and troubleshooting. The user guide is provided on the USB flash drive and is also available for download at .Capture imagesa. Turn the instrument power switch located in back of the instrument base to the ON position.b. Turn the computer and monitor ON.c. When the computer shows the Windows ™ desktop and the X-Y stage of the instrument has stopped moving, click the M7000 icon to start the EVOS ™ M7000 software.d. When the Capture tab is displayed, the EVOS ™M7000 Imaging System is ready to use.1Turn onthe EVOS ™M7000Imaging System a. Place the vessel containing your sample on the stage using the appropriate vessel holder. b. On the Capture tab, click the Vessel button to open the Vessel Selection dialog.c. Select the Vessel category that corresponds to your sample vessel,then select the Holder and Vessel type from the dropdown menus.d. Click Done to complete your selection and close the dialog.The Vessel map on the Capture tab displays your selected vessel.2Selectsample vessel a. Click the desired Objective button to select the corresponding magnification. b. Select the desired Light source for which you wish to adjust brightness and set focus.3Select objective andlight sourceb. For Mode, select Simple or Actual.• Simple mode allows you to control Brightness as a single parameter.• Actual mode allows you to adjust Light (i.e., LED intensity), Exposure, and Gain individually.c. For Camera, select Mono (monochrome) or Color.• Mono is used for image capture in fluorescence and transmitted light (brightfield) channels• Color is used for image capture in the brightfield channel onlyd. Optional: Choose Phase options.Note: Phase options are available only for the transmitted light (brightfield) channel; they are not availablefor fluorescence channels.e. Click the Brightness and camera settings button again to collapse the controls.and cameraoptionsa. Click the Light button to turn on the excitation light for the selected light source and enterthe instrument in the Live mode.b. Adjust brightness using the Brightness controls.Note: For best results, optimize the brightness parameters as follows:• When searching for sample: Increase Gain for a brighter signal and decrease Exposure for faster framerate during navigation around the vessel.• When capturing image: Decrease Gain to reduce background noise and increase Exposure to regainsignal intensity, as needed.• For brighter signal: Increase Light intensity for brighter illumination. If needed, follow by increasingGain.• For time lapse imaging: Increase Gain and Exposure, and decrease Light intensity to reducephotobleaching and phototoxicity.a. Choose the channels you wish display in the Viewing Area by selecting the appropriate channel checkboxon the corresponding Light source button.You can select multiple channels to display in the Viewing Area. In the following example, DAPI, RFP, andtransmitted light (brightfield) channels have been selected.b. Click the Image Display settings button to expand the image display controls for the selected channels.c.Adjust the Brightness , Contrast , and Gamma settings for each of the selected channels usingthe corresponding sliders.d.Optional: To remove a channel from displaying in the Viewing Area, unselect the corresponding Displaycheckbox.To display an available channel not shown in the Viewing Area, re-select the checkbox.e.Click the Image color display button to display the sample pseudo-colored in the default emissioncolor of the selected channels. By default, color display option is on.f.Click the Image Display settings button again to collapse the controls.Note: Adjustments made to Image display settings only affect how the image is displayed in the ViewingArea; they do not change how the image is captured.5AdjustbrightnessBrightness controls in Simple mode Brightness controls in Actual mode6Set imagedisplayoptionsa. Click Autofocus to run the autofocus procedure to find the best focal plane for thecurrent channel and sample.Alternatively, use the Coarse and Fine focus sliders to manually find the best focal position.b. To choose a different autofocus method, click Advanced focus settings button, then select from theAutoFocus Method dropdown.Available options for AutoFocus Method are:• Small Structure: Choose this option for samples with many fine, hair-like structures (e.g., filaments or structural stains).• Large Structure: Choose this option when your sample contains large structures (e.g., whole cell stains).• Small Bright Objects: Choose this option when capturing samples with localized staining (e.g., nuclei).Z-Offsets allow you to specify the optimal focus position in each channel relative to the focus position in other channels.a. Verify that the Lock Z-Offsets option is checked in the Advanced focus settings window, then click theAdvanced focus settings button again to close the window.b. Select the Objective and the Light source (i.e., channel) you wish to capture.c. Click the Light button to enter the Live mode, and focus on the sample manually using the Coarse and Finefocus sliders or automatically by clicking the AutoFocus button.d. After you have found the optimal focus position in the first channel, click the A dvanced focus settingsbutton, then uncheck the Lock Z-Offsets option.e. Without changing the objective, select the next Light source (i.e., channel) you wish to capture.f. If the light is off, click the Light button to turn it on, then focus on the sample manually using the Coarseand Fine focus sliders or automatically by clicking AutoFocus.g. Repeat this procedure for every channel you wish to capture.h. When you have found the optimal focus position in all the additional channels you wish to capture, clickthe Advanced focus settings button, then check the Lock Z-Offsets option.When you have completed this procedure, the focus position in each selected channel will be offset relative to each other.7 8Focus on the sample Optional: SetZ-Offsetsa. While in Field View , click the Light button and enter the instrument in the Live mode.b. To go to a specific location on the sample vessel, click and dragthe crosshair to the corresponding location on the virtual vessel.If needed, click on the Zoom button to open a larger view of the Vessel map for easier navigation to the desired location.Click the Zoom button again to close the zoom window.c. While in the Live mode, use the Jog Control to move the stage at an intermediate pace to thedesired location as you view the sample until you find the field of view you wish to capture.Alternatively, click on the navigation arrows (up, down, left, right) on the Viewing area to move in the corresponding direction exactly one field of view. You can also click and drag the field of view itself to move around the sample vessel.d. Click the Lightbutton again to exit the Live mode in Field View.9Find theregion ofinterest inthe Livemode 10Select fieldand capture images a. In Area View , position the capture crosshair over the region of interest and click to select the field you wish to capture. Alternatively, find the field you wish to capture in the Live mode.b. Click Capture to acquire an image of the selected field using the current capture settings.A thumbnail of the captured image is displayed above the Light source button for the specific channel in which the image was captured (in this example, DAPI).The Viewing are displays the captured image at the location of its capture when the zoom level is greaterthan one field of view.c. To capture the same field in another channel, select the desired channel using the corresponding Lightsource button.d. Readjust the brightness and focus (if needed), then click Capture.A thumbnail of the captured image is displayed above the Light source button for the new channel in whichthe image was captured.The Viewing area displays a multicolor overlay of the images at the location of their capture.e. To capture another field, position the capture crosshair over the new region of interest, then click to selectthe new field.f. Readjust the brightness and focus (if needed), then click Capture.g. To capture a field using a different magnification, select the desired Objective, then repeat the captureprocedure with the new magnification as described.h. To capture a selected field in multiple channels simultaneously, select the channels you wish to capture bychecking the small circular checkboxes on the the corresponding light source buttons.In the following example, DAPI, RFP, and transmitted light (brightfield) channels have been selected.i.Readjust the brightness and focus (if needed), then click Capture Channels.The instrument captures an image of the selected field in each of the selected channels using the current capture settings. After capture, the Viewing area displays a multicolor overlay of the captured images at the location of their capture.Save captured imagesa. When finished capturing images, click Save… to open the Save widialogndow.b. Select the captured fields you wish save. Available options are:• Currently selected field: Saves images only from the currently selected field.• All newly captured fields: Saves images that have been captured and stored in the image cache, but notyet saved. This option is available only if you have previously saved images from the same session.• All captured fields: Saves images from all captured fields that are held in the image cache.This is typically all of the images that you captured during an imaging session.a. Click Browse , navigate to the desired folder, then click Select .To create a save new folder, navigate to the desired location, click New , type in the name of the newly creat-ed folder, then click Select .Note: We recommend that you save your captured images to an external hard drive.b. If desired, type the prefix you wish to use for your save images in the File name prefix textbox.a. Select File types to save by checking the corresponding checkboxes. You can choose multiple file types foryour captured images. Available options for file type are Raw images and Displayed images .• Raw images: Saves images captured in different channels individually as 16-bit raw images.This is the recommended format for image analysis.Available raw image options are:–Single field, individual channels: Saves images capturedin each field and each channel individually.–Z stack planes, individual channels: Saves the z-stackprojection and each z-stack plane for each field and each channel as a separate image.Available File format for raw images are: TIF , PNG , C01, and DIB .• Displayed images: Saves images in a format that can be viewed in most image display applications.Available displayed image options are:–Single field, individual channels: Saves imagescaptured in each field and each channel individually.–Merged image: Saves the images of a field captured indifferent channels as a multi-channel overlay.–Tiled image, merged channels: Merges the imagescaptured in each channel, then aligns them close together into a tiled format.Available sizes for tiled images are Small (2000 × 2000 pixels), Medium (4000 × 4000 pixels), Large (10,000 × 10,000 pixels),or Maximum (26,000 × 26,000 pixels)Available Color options for displayed images are:–Grayscale: 16-bit–Pseudocolor:24-bit RGB (8-bit per RGB channel).123Select captured fieldto saveSelect savelocation Select file types to saveAvailable Brightness options for displayed images are:–High: Limits pixel depth and reduces exposure time and dynamic range.–Full: Provides more detail for quantitative imaging.Available File format for displayed images are: TIF, PNG, and JPEG.Note: While pseudocolors help differentiate the channels used in multi-channel overlays, grayscale images usually show more detail.24-bit images (8-bit per RGB channel) are NOT recommended for image analysis as not all channels will display in many image analysis applications.b. If desired, check the Include Grid option and select the grid size.When checked, this option superimposes a grid on the displayed images.You have the following options for the grid size (in pixels): Auto, 10 × 10, 50 × 50, 100 × 100, 200 × 200, and 500 × 500.c. To see more file type options in a table format, click More options…Full menu of save options are displayed in a convenient table format, allowing you to save your captured images in a number of formats simultaneously.d. After you selected save options for your captured images, click Save.The instrument will save the images in the designated folder based on your specifications.Documentation and supportTechnical supportFor the latest services and support information for all locations, go to /support.At the website, you can:• Access worldwide telephone and fax numbers to contact Technical Support and Sales facilities• Search through frequently asked questions (FAQs)• Submit a question directly to Technical Support (/support)• Search for user documents, SDSs, vector maps and sequences, application notes, formulations, handbooks, certificates of analysis, citations, and other product support documents• Obtain information about customer training• Download software updates and patchesSDSSafety Data Sheets (SDSs) are available at /support.Limited Product WarrantyLife Technologies Corporation and/or its affiliate(s) warrant their products as set forth in the Life Technologies’ General Terms and Conditions of Sale found on Life Technologies’ website at /us/en/home/global/terms-and-conditions.html. If you have any questions, please contact Life Technologies at /support.For Research Use Only. Not for use in diagnostic procedures.The information in this guide is subject to change without notice.DisclaimerTO THE EXTENT ALLOWED BY LAW, LIFE TECHNOLOGIES AND/OR ITS AFFILIATE(S) WILL NOT BE LIABLE FOR SPECIAL, INCIDENTAL, INDIRECT, PUNITIVE, MULTIPLE OR CONSEQUENTIAL DAMAGES IN CONNECTION WITH OR ARISING FROM THIS DOCUMENT, INCLUDING YOUR USE OF IT.Revision history: Pub. No. MAN0018380Important Licensing InformationThese products may be covered by one or more Limited Use Label Licenses. By use of these products, you accept the terms and conditions of all applicable Limited Use Label Licenses.Manufacturer: Life Technologies Corporation | 22025 20th Ave SE St #100 | Bothell, WA 98021All trademarks are the property of Thermo Fisher Scientific and its subsidiaries, unless otherwise specified.©2018 Thermo Fisher Scientific Inc. All rights reserved.。
扫描电子显微镜
多模式和多功能：未来 的扫描电子显微镜将具 备多种模式和功能，例 如在观察形貌的同时进 行成分分析、晶体结构 分析等。此外，还将开 发出更多的附属功能， 如样品制备、图像处理 和分析等
扫描电子显微镜的发展趋势
自动化和智能化：随着 自动化和智能化技术的 不断发展，未来的扫描 电子显微镜将更加智能 化，具备自动调整参数 、自动聚焦、自动扫描 等功能。同时，还将引 入人工智能和机器学习 等技术，提高图像处理 和分析的自动化程度
高分辨率和高质量图像 ：随着透射电镜等其他 电子显微技术的发展， 扫描电子显微镜的分辨 率和图像质量也将得到 进一步提高。同时，新 的探测器和信号处理技 术也将被引入，以提高 图像的信噪比和对比度
高速扫描和实时成像： 为了更好地观察动态过 程和实时变化，扫描电 子显微镜的扫描速度将 得到提高，同时配备更 快的电子束扫描系统和 更灵敏的探测器，实现 高速扫描和实时成像
扫描电子显微镜的应用领域
总之，扫描电子显微镜作为 一种高分辨率的电子显微技 术，在各个领域都有着广泛 的应用前景
随着技术的不断发展和进步， 相信它的应用领域将会越来 越广泛
4
扫描电子显微镜的发展趋势
扫描电子显微镜的发展趋势
随着科技的不断发展，扫描电子显微镜也在不断发展和改进，未来将会呈现出以下发展趋 势
材料科学：材料科学领域 需要对金属、陶瓷、聚合 物等材料的结构和性能进 行研究。扫描电子显微镜 能够提供高分辨率和高对 比度的图像，帮助研究人 员了解材料的微观结构和 性能之间的关系
扫描电子显微镜的应用前景
总之，扫描电子显微镜作为一种高分辨率的电 子显微技术，在各个领域都有着广泛的应用前
景
随着技术的不断发展和进步，相信它的应用领 域将会越来越广泛，为科学研究和技术创新做
JSM-7800F_技术参数
JSM-7800F场发射扫描电子显微镜技术参数1 工作条件：1.2 电源220V（±10％），50Hz；单相1.3 环境20±5℃1.4 相对湿度＜80％1.5 连续工作时间 连续操作2 技术说明：2.1 场发射扫描电子显微镜JSM-7800F主要用于材料表面的微观形貌的高分辨观察，可配备X射线能谱仪等附件，可同时进行微区的成分分析，具有配备X射线能谱仪等的相应安装接口。
2.2 技术参数2.2.1 分辨率：二次电子图像：0.8nm (15kV), 1.2nm (1kV) 2.2.2 背散射电子像：1.5nm2.2.3 加速电压: 0.01 - 30KV 连续可调2.2.4 束流范围：1pA～200nA连续可调2.2.5 放大倍率25X – 1,000,000X ；放大倍数粗、细模式连续可调，具有随着工作距离或加速电压的变化自动精确校正、补偿、预设等功能2.3 真空系统2.3.1 真空度：电子枪室高真空 10-7Pa，提供离子泵专用的UPS，延时200小时以上样品室真空10-4Pa2.3.2 泵系统：磁悬浮涡轮分子泵、2台离子泵和1台机械泵2.3.3 污染防止：液氮冷阱和前置阱2.4 电子光学系统2.4.1 电子枪：高稳定性浸没式肖特基（Schottky）热场发射电子源，能自动合轴调整2.4.2 聚光镜：电磁透镜会聚系统，束流强度可连续可调；光阑角度控制透镜控制束斑尺寸20 nA下无需手动切换光阑2.4.3 物镜：超级混合型物镜设计，对样品没有局限性，任何种类的样品都可以得到超高分辨图片2.4.4 物镜光阑：4级可调、X/Y方向精细可调对中，20 nA下无需手动切换光阑2.4.5 消像散器：八级电磁系统，具有自动消像散功能2.4.6 扫描线圈：2级电磁系统，具有扫描图像旋转连续可调，并随工作距离能自动旋转补偿等功能2.4.7 电图像位移：±10 µm，可通过控制电子束移动实现2.4.8 自动调整功能：具有自动透镜控制、自动合轴、自动聚焦、消像散、反差、亮度调节功能，样品台导航控制等功能，并兼有手动调整功能2.5 样品室和样品台2.5.1 样品台：5轴马达驱动全对中样品台, 示意图在监视器上显示2.5.2 行程：X＝70mm, Y=50mm, Z=2 - 41mm 倾斜 -5° - +70°旋转 360°2.5.3 样品更换：快速气锁更换样品(最大尺寸100mm直径*40 mm高) 2.5.4 主机附件：红外CCD照相机2.6 探测器及成像系统2.6.1 高位和低位二次电子探测器：二次电子像2.6.2 背散射电子探测器：背散射电子像2.6.3 成像模式：同时得到二次电子像、背散射电子像2.7 扫描电镜计算机系统2.7.1 操作系统Windows® 7 Professional2.7.2 显示器 19英寸 LCD2.8 主动式减震系统: 标准配置2.9 自动离子溅射仪2.9.1 工作压力：好于20Pa2.9.2 溅射电流：10,20,30,40mA2.9.3 溅射靶：Pt2.9.4 样品台：直径64mm2.9.5 真空室：120mm(直径)x100mm(高)2.10。
扫描电镜SEM-JEOL7600F详细操作步骤
扫描电镜SEM-JEOL7600F详细操作步骤Operating procedure for JEOL 7600F High Resolution Analytical SEMI. Specimen preparationThere are several holders for different kinds of specimens and applications. During your initial training you should have received a general overview of these holders. Also, you should have received training on specimen mounting using the holder that best suits your specific application. Only use a holder for which you have received training by the tool instructor. If you wish to use a different holder, first contact the tool instructor.It is very important to know the kind of holder you are using and the way to mount specimens. For example, for the 12.5 and 26 mm holders, the correct way to mount your specimen is to flush its surface with the cylinder top face (see Fig. 1).FIG. 1. Specimen positioning on 12.5 and 26 mm holders. (Diagram taken from JEOL’s manual.)If your specimen needs to protrude above the cylinder’s top face (or the top face of another holder), you can still use this holder, but you need to estimate (with approx. 1 mm accuracy) the offset between the specimen and holder top surfaces. To make sure you are doing things correctly, use the sample height tool(see Fig. 2). Try to have the sample’s surface aligned with the zero offset line. If it needs to be above this line, read the offset in the meter scale. This offset value will be used when loading your sample in the SEM chamber.FIG. 2. Sample height tool. The right image shows a sample correctly flushed at the zero offset line.II. Loading a specimen1) Log on your session in the Facility Online Manager (FOM) software (icon on the desktop ofthe DATA computer). After a correct login, the SEM monitor should automatically turn on.If it does not, STOP YOUR WORK AND CONTACT A STAFF MEMBER. Never modify any physical connections or push any system buttons. Doing so is unsafe for you and the instrument.2) Confirm that the stage is in the exchange position by checking that the EXCH POSN light onthe airlock is ON. If not:a.Click the OFF button under Observation in the upper left section of the main window(see Fig. 3). The system diagram, located in the lower right corner of the main window, should show the beam stopped at the upper section of the SEM column. This means that the SEM column gate is closed, if not, please contact the tool instructor.b.Click the Observation button in the upper right section of the main window.c.Click the Exchange Position button in the SEM Monitor window.FIG. 3. Main window of Graphical User Interface (GUI).3) Before continuing with the next step, make sure that all the stage coordinates (X, Y, R and T)are “0.0”, except for Z, which should be “38.0”.4) Turn on a “live” image of the chamber using the infrared (IR) camera. To do this, click onthe “Windows” key in the SEM computer keyboard and select “IR Camera” icon.5) Ordinarily, the airlock chamber is under high vacuum and the airlock chamber isolation valveis open. Before loading, the lights in the airlock buttons should be: VENT-off / EVAC-on / EXCH POSN-on / HLDR-off.6) Press the VENT button for 2 seconds then release it. (The VENT light blinks; the isolationvalve closes; N2 gas vents into the airlock.)7) When the VENT light stops blinking, unlock the airlock chamber by releasing the clasp.Open the airlock door.8) Lock the specimen holder into the clamp on the end of the exchange rod. (The specimenheight above the top of the holder is limited to ~5 mm.) Make sure the flat side of the specimen holder lies perpendicular to the insertion direction (see figs. 4 and 5).FIG. 4. Locking the sample holder in place in the airlock chamber. a) Top view of specimen holder. b) and c) Identification of “flat side” with respect to dovetail channel at the base of holder. The flat side is perpendicular to the length of the dovetail channel. d) Correct way of locking specimen holder with the holder’s flat side perpendicular to the insertion direction. (Diagrams taken from JEOL’s manual.)FIG. 5. Sample locked in place in the airlock chamberIT IS VERY IMPORTANT TO CHECK THAT THERE ARE NO VERTICAL GAPS BETWEEN THE HOLDER AND THE CLIP MECHANISM. GENTLY PUSH DOWN ON THE HOLDER TO MAKE SURE IT SITS PROPERLY OVER THE CLIP.9) Before closing the airlock chamber, check that the door’s O-ring is free of dust and dirt andcorrectly positioned in the groove.10) Close and lock the airlock chamber and press the EVAC button. (The EVAC light blinks; theairlock is pumped to high vacuum; the isolation valve opens.)11) Wait until the EVAC light stops blinking. Now the lights in the airlock buttons should be:VENT-off /EVAC-on /EXCH POSN-on /HLDR-off. Also confirm that the system diagram (lower right of main window) indicates that the airlock chamber is under vacuum (gray color)and that the airlock isolation valve is open.12) Lower the specimen-exchange rod horizontally without pulling along its axis (see Fig. 6).Once it is completely horizontal, the low pressure in the chamber may suck the rod in. This is normal, it will stop by itself due to friction.FIG. 6. Lowering of specimen-exchange rod. (a) Initial vertical position. (b) Detail of location of the plastic stopper.(c) Lowering of rod without pulling along its axis. (d) Fully horizontal position. Rod is held extended due to friction in sliding metal parts. Note that plastic stopper is pushed down when rod is horizontal as shown in (e).13) Fully insert the specimen-exchange rod, keeping the holder horizontal, until you feel it cometo a firm stop. Look at the chamber live image to detect this event. Then apply more force to lock the holder in the SEM stage (see Fig. 7).FIG. 7. Lo cking holder in SEM stage. (a) Insertion of rod by pushing horizontally along rod’s axis. (b) Rod position when it first touches the SEM stage. (c) Rod position with holder locked in SEM stage.14) After confirming that the HLDR light has lit up, fully retract the exchange rod horizontallyuntil the plastic stopper snaps and comes up (see Fig. 8). Let the rod sit on the stopper and then tilt up the exchange rod without pulling along its axis. Now the lights in the airlock buttons should be: VENT-off / EVAC-on / EXCH POSN-on / HLDR-on.FIG. 8. Retracting exchange rod. (a) Fully retracted and resting on the plastic stopper. (b) Detail of rod resting on plastic stopper. C) Lifting of rod to its vertical position without using any force along rod’s axis.15) Click on the Specimen Offset button in the graphical user interface (GUI) and select fromthe list the holder you installed. If your sample has an offset (in mm) measured with the sample height tool (see Fig. 2), enter it in the specimen surface offset field of the specimen holder pop-up window (see Fig. 9).FIG. 9. Graphic user interface showing the specimen holder popup window.III. Obtaining an image1) Wait until the chamber vacuum is at 5x10-4 Pa or lower. Open the Gun Isolation Valve byclicking the ON button under Observation.3) Select the SEI detector and SEM mode, and click on the working distance (WD) in the imageinfo area of the GUI (see Fig. 10). VERY IMPORTANT: Only click on WD when in SEM (high mag mode), never do it in LM (low mag mode). Select 15 mm from the list and click “OK” in the window that pops up after clicking WD. This action will focus the beam toa WD of 15 mm and will bring the stage to Z=15.0+OFFSET. If the stage doesn’t move,check that the ZFC button is “on” (green). Keep an eye on the movement in the IR camera window.FIG. 10. Graphic user interface showing the position of the WD indicator/selector area.4) Unfreeze the image, if necessary, by clicking on the FREEZE button in the knobset panel(see Fig. 11).FIG. 11. Knobset panel, specimen stage control panel and trackball.5) Find a feature in your sample by moving the stage using the trackball (see Fig. 11). If needed,select LM mode and, once you find the feature of interest, switch back to SEM. Adjustcontrast and brightness using the autocontrast (ACB) button or the IMAGE CONTRAST and BRIGHTNESS knobs in the knobset panel (see Fig. 11). If the offset is correct, the image should be rather focused. Now, rotate the outer ring of the trackball until the image is in good focus. As you rotate the ring, the Z value changes. Make sure Z doesn’t change by more than ±2 mm from its initial value. If not sure about this step, please contact the tool instructor.6) Once the image is in focus, update the sample offset. For example, if your sample had aninitial offset of 3 mm (Z=15.0+3.0=18.0 mm), and after focusing with the outer ring, Z=17.5 mm, then the new offset should be OFFSET=17.5 - 15.0 = 2.5 mm. Click on the sample holder image (see Fig. 9) and enter the new offset in the corresponding field.7) Choose probe current setting. You may change the probe current by selecting the desiredlevel in the probe current section of the GUI (right under the WD info area, see Fig. 10):a.For most secondary electron (SE) imaging choose low current (LC) mode with levels 1-10 (6-7 typical). The objective lens (OL) aperture should be set to #4.b.For analytical work, especially when using wavelength dispersive spectroscopy (WDS),choose high current (HC) mode with levels 11 – 20 and with the OL aperture set to #1.CAUTION.-Do not attempt to change the OL aperture without having been trained on this specific procedure by the tool instructor.CAUTION.-If you change the current setting, repeat steps 5 and 6 to update thesample offset.8) Now, you are ready to navigate to the region of interest in your sample, and if necessary,change the beam parameters and the working distance./doc/46d9e41c941ea76e59fa0401.html e low magnification mode (LM) when necessary by pushing the LOW MAG button inthe knobset panel. Navigate to the area of interest using the trackball./doc/46d9e41c941ea76e59fa0401.html e SEM mode in high magnification when possible. This is selected when the light ofthe LOW MAG button is off.CAUTION.- If you move the stage by more than 1 mm, repeat steps 5 and 6 toupdate the sample offset.c.Set WD to 4-6 mm for best resolution secondary electron (SE) imaging using the inlensdetector (SEI), especially at low beam energies.d.Set WD≤8 mm for good resolution SE imaging using the low, in-the-chamber SEdetector (LEI).e.Set WD=8 mm for EDS, and WD=15 mm for WDS work.CAUTION.- If you desire to change to a shorter WD, repeat steps 5 and 6 to update the sample offset.CAUTION.-Unless you have been authorized by the tool instructor, the minimum WD you can use is 4.5 mm. Note that EDS work is done at WD=8 mm and WDS work is done at WD=15 mm. NOTE.- The shortest WD for 30 keV and 15 keV is 6.5 mm and 4.5 mm, respectively.For beam energies 2 keV, the shortest WD can be 2 mm, however, make sure you have authorization from the tool instructor before setting WDs below 4.5 mm.IV. Optimizing an image1) Align the beam.a.Set magnification to ~10,000x - 50,000x using the MAGNIFICATION knob in theknobset panel.b.Focus the image (FOCUS knob in knobset panel) and correct astigmatism if necessary(see IV.2)c.Turn the wobbler on (WOBB button in knobset panel). If the image shifts, adjust X and Yknobs to stop image shiftingd.Turn the wobbler off.2) Astigmatism correction.a.Find a feature that has approximately circular shape using medium to high magnification./doc/46d9e41c941ea76e59fa0401.html ing the FOCUS knob, check for astigmatism by going through over and under focuswhile looking for directionality of focus in the image (over and under focus directionality will be at right angles to each other).c.Stop focus at center of over and under focus (image may not be sharp but has nodirectionality of focus).d.Adjust the X and Y stigmation knobs (one at a time) and try to obtain an image as sharpas possible.e.Focus the image with the FOCUS knob and, if necessary, repeat steps b-e.f.If required, increase the magnification and repeat steps a-e.V. Unloading a specimen1)Click the OFF button under Observation in main window (see Fig. 12). The systemdiagram, located in the lower right corner of the main window, should show the beamstopped at the upper section of the SEM column.2)Click the Exchange Position button in the SEM Monitor window.FIG. 12. Main window of Graphical User Interface (GUI).4) Before continuing with the next step, make sure that all the stage coordinates (X, Y, R andT) are “0.0”, except for Z, which should be “38.0”.5) Turn on a “live” image of the chamber using the infrared (IR) camera. To do this, click onthe “Windows” key in the SEM computer keyboard and select “IR Camera” icon.6) Ordinarily, the airlock chamber is under high vacuum and the airlock chamber isolation valveis open. Before unloading, the lights in the airlock buttons should be: VENT-off / EVAC-on / EXCH POSN-on / HLDR-on.7) Fully insert the specimen exchange rod until it “grabs” the specimen holder on the SEMstage. You can check this event in the IR camera image. These steps are describe in steps II.12 and II.13. Confirm that the HLDR light remains on8) Fully retract the exchange rod as described in step II.14. Confirm that the HLDR light goesoff.9) Press the VENT button. (The VENT light blinks; the isolation valve closes; N2 gas vents intothe airlock.)10) When the VENT light stops blinking, unlock the airlock chamber by releasing the clasp.Open the airlock door.11) Remove the specimen. Close and lock the airlock chamber and press the EVAC button. (TheEVAC light blinks; the airlock is pumped to high vacuum; the isolation valve opens.) The lights in the airlock buttons should be: VENT-off I EVAC-on I EXCH POSN-on I HLDR-off.12) Close the IR camera window to increase the life of safe the life of the IR lamp.13) Log off your session in the Facility Online Management (FOM) software. The SEM monitorshould automatically turn off. If it does not, please contact the tool instructor.V. Notes on using the TED detector1)Make sure you have previously accurately determined the stage offset (see section III).2)Go to a WD between 6-8 mm.3)Verify that the vacuum level is in the mid 10-4 Pa range or better.4)Click the OFF button under Observation in main window (see Fig. 12). This will isolate thevacuum in the e-beam column.5)Insert the TED and wait until the vacuum level is back at 5x10-4 Pa or better. This will take afew minutes.6)Once the vacuum level is appropriate, click the ON button under Observation in mainwindow.VI. Policy for mounting powder samples (including magnetic powder samples)We need to be extra careful when mounting powder sample, especially magnetic.1)Before mounting ANY powder sample, YOU NEED TO SHOW IT TO THE TOOLMANGER TO RECEIVE GREEN LIGHT TO GO ON. Once it is determined that it is safe for the system, you can repeat the mounting method as many times as you want on your own.In the next section you can find some tips on mounting powder samples, including magnetic powder samples.2)The closest WD for magnetic powder samples is 8mm. You can't image these samples anycloser.3)Make sure you secure extremely tight any bulk magnetic sample to the sample holder toavoid any chance of having it fly onto the objective lens.VII. Tips for mounting powder samples (including magnetic powder samples)A good general procedure is to cover an aluminum or carbon stub with carbon paint or silver paint/cement and quickly deposit a very small amount of powder on to the stub before the paint dries. Once dry, blow off any loose particles with compressed air. Remember that YOU CAN’T DO THIS IN 1L32, you need to do it in an approved lab here on in your owninstitution.Nano sized magnetic particles .- If the particles are nano sized and are relatively small in number, mounting them on a carbon stub by drying an alcohol suspension is OK. The weak force will keep them stuck to the stub. They can also be mounted on lacey or holey carbon TEM grids the same way (this implies using the TEM sample holder). Mounting on TEM grid reduces considerably the interaction volume allowing higher resolution for elemental mapping.Imaging large size (> 1 µm) magnetic particles.- This size particles cannot be mounted as in the previous bullet, because the objective lens (OL) flux will pull them onto the lens. For imaging these large particles, to study rough particle morphology for example, you need toinsure that they are FIRMLY stuck down in carbon tape with all of the loosely adhering particles blown off with compressed air or nitrogen. (You have to do this in your own lab, or an in approved lab in the CFN, not in 1L32!) For safety of the microscope, only use low mag (LM) mode for imaging these particles. In LM mode, the OL flux field is turned off.EDS of large size magnetic particles.- Mount these particles in a 1” or 1 ” inch standard epoxy mount (see for example, /doc/46d9e41c941ea76e59fa0401.html/material_html/mat1.htm). Polish the mount to expose surfaces of particles and then coat with carbon. This will give the bestmicroanalysis conditions.VERY IMPORTANT! Mounting samples of the kind described in this section CANNOT be done in lab 1L32. Ask the tool manager to give you a holder for you to mount these samples in an appropriate lab in the CFN or in your own institution.。
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國立中央大學地球科學系
熱場發射掃描式電子顯微鏡J E O L J S M7000F
使用申請表
使用者：申請日期：
隸屬單位：聯絡電話：
E-mail：
研究計畫名稱：
計畫主持人或指導教授簽名：
申請事項F委託操作
F自行操作
F申請自行操作訓練
申請
使用之儀器Coating F Pt _________sec. F Carbon
F SEM（JEOL JSM-7000F）
F BSI
F EDS
F Standard ____________________________________
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請“詳述”試片製作方式、材料種類及特性
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經辦人：
申請人(簽名) 計畫主持人或指
導教授(簽名)
儀器負責人員
(簽名)
儀器負責教授
(簽名)
欲使用本設備者，請先至儀器介紹網頁詳讀【JEOL-7000F SEM管理辦法】，以明瞭本設備之功能與使用規範。
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詳細記錄儀器狀況。
3. 離室前請確實檢查實驗室門窗及儀器之水、電安全，並維持室內整潔。
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詳填使用者與試片資訊後，並以電話03-4227151ext. 65642或
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2. 申請人於預約時段前將試片送交儀器操作技術員。
3. 預約操作申請人於操作時須親自在現場共同進行實驗。
自行操作訓練與考核辦法
1.本實驗室提供SEM上機訓練課程，通過考核後，即可自行操作機台。
SEM上機訓練與
考核辦法見JEOL-7000F SEM管理辦法。
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