JEM-2100透射电镜JSM-7600F场发射扫描电镜开放使用及

2100F高分辨电镜操作顺序--个人小结编辑整理：尊敬的读者朋友们：这里是精品文档编辑中心，本文档内容是由我和我的同事精心编辑整理后发布的，发布之前我们对文中内容进行仔细校对，但是难免会有疏漏的地方，但是任然希望（2100F高分辨电镜操作顺序--个人小结）的内容能够给您的工作和学习带来便利。

同时也真诚的希望收到您的建议和反馈，这将是我们进步的源泉，前进的动力。

本文可编辑可修改，如果觉得对您有帮助请收藏以便随时查阅，最后祝您生活愉快业绩进步，以下为2100F高分辨电镜操作顺序--个人小结的全部内容。

装好试样后,开始操作JEM—2100F的步骤：1、打开beam阀,在LOW MAG下，找到薄区所在的位置;2、在LOW MAG下将放大倍数调至500倍，然后切换至MAG1；3、找到一个薄区，将放大倍数调至2000倍,按下STD FOCUS，再进行调Z的步骤：1）方法一：将试样边沿移至屏幕中心，按下IMAGE WOBB X，试样呈抖动状态,再通过调节，使屏幕中心试样不在抖动为止;2）、方法二：找到试样薄区，逆时针旋转BRIGHTNESS，使电子束汇聚为一点，再通过调节，使各衍射斑点汇聚于同一点；4、将放大倍数调至100K倍（调节放大倍数时，需要同时旋转BRIGHTNESS和MAG/CAM L），并将无试样区域移至屏幕中心，逆时针旋转BRIGHTNESS至电子束呈合适大小内、外圆形；5、按下BRIGHT TILT按钮，并通过调节SHIFT X和SHIFT Y将电子束移至屏幕中心，再通过调节DEF/STIG X和DEF/STIG Y将电子束的内圆恰好移至外圆的中心(若电压对中过程中，平移与偏转相互影响,则联动比有问题,需要调最新的合轴文件）;6、再按下COND STIG按钮，通过调节DEF/STIG X和DEF/STIG Y将电子束的内圆内的图形调成“奔驰”车标形状；7、逆时针旋转BRIGHTNESS，使电子束的内圆和外圆重合，再在HIGH VOLTAGE CONTROL 界面中点击“ON”，按下F4，通过调节DEF/STIG X和DEF/STIG Y使内外圆同心缩放；8、检查电压对中和聚光镜消象散；9、顺时针旋转BRIGHTNESS，使电子束充满整个屏幕，套取一号聚光镜光阑，将电子束调至屏幕中心（机械对中）;10、再次合轴,将放大倍数调节至400K倍，再次检查电压对中和聚光镜消象散;11、将放大倍数调至100K倍,并将薄区边沿移至屏幕中心，通过调节OBJ FOCUS旋钮，将试样边沿调至为微欠焦(略显白色边沿），再将放大倍数调至400K倍，并将边沿区移至屏幕中心，按下F1，然后打开CCD,并调出傅里叶变换，按下OBJ STIG，通过调节DEF/STIG X和DEF/STIG Y和OBJ FOCUS旋钮（使傅里叶变换为一圆环)，得到清晰的高分辨像；12,关闭CCD，再按下F1，将放大倍数调至100K倍,找到感兴趣薄区，并将电子束汇聚于一点，按下SA DIFF按钮，并将相机常数调至60CM，手动将菊池线的交点移至电子束中心；至此，已完成电镜合轴、消象散、踩带轴的步骤，接下来便可进行选区电子衍射、明场像、暗场像和高分辨像的操作.一、选区电子衍射步骤:1、合轴完成后，在TEM、MAG1模式下，将感兴趣区移至屏幕中心；2、通过感兴趣大、小来套取合适的选区光阑；3、按下SA DIFF按钮转为衍射模式，获得相应的电子衍射花样，并通过调节MAG/CAM L 获得合适的相机常数（20-30CM）-—-不同相机常数的意义；4、通过顺时针旋转BRIGHTNESS和调节DIF FOCUS获得足够暗、圆锐的衍射斑点。

JEM-2100透射电子显微镜操作流程⏹冷阱、高压以及LENSE分两次加液氮，分两步升高压总计1h开LENSE，聚光镜光阑1档⏹安放样品使用样品杆前，请仔细检查样品杆是否完好、是否需要维护：销钉是否松动、高度感应端是否脱落）载物铜网正面朝上，压片压好载物铜网后轻轻旋紧螺钉洗耳球吹气确保样品杆关键部位没有杂物用样品杆中部轻击左手手掌，确保压片压好载物铜网⏹装样品杆预抽过程销钉对准卡槽，水平垂直推入样品杆（不得旋转）,开泵预抽（PUMP），听到噗的声音后松手，等样品杆旁边绿灯变亮后开始进杆；进杆紧握样品杆把手分两次向里均匀旋进（顺时针），直至样品杆进入样品室（该过程不得松手并有向外拉力、不得产生轴向力）拔杆确保关闭灯丝与CCD的前提下，用均匀的外力将样品杆向外拔（该过程较长），当样品杆受到阻力时，即可向外旋转（逆时针），旋转受到助力时，停止旋转，再用均匀力向外拔（该过程较短），当样品杆再次受到阻力时，即可向外旋转（逆时针），听到气门“噗”的声音时，停止拔杆。

手挡住样品杆尾部，放气（AIR）直至气门再次发出“噗”的声音时，将样品杆拔出样品室外。

测试步骤电压中心STD FOCUS低倍找样LOW MAG SPOTSIZE 1高倍照相MAG 1双中心调节聚光（BRIGHTNESS）看光斑是否在中心，不在中心采用电子束（SHIFT X Y）平移至中心粗聚焦利用IMAGE WOBB X Y、Z ⇑，Z ⇓调至样品不动为止1—5合轴在双中心的基础上（30 K），SPOTSIZE 5 光斑不在中心，采用电子束（SHIFT X Y）平移到中心，SPOTSIZE 1光斑不在中心，采用电子枪（F4+SHIFT X Y）平移到中心，调完点去F4，继调SPOTSIZE 1，反复多次，直至光斑中心不因SPOTSIZE的变化而偏移荧光屏中心注意：SPOTSIZE 5时不得采用F4键盘调像散100 K 将样品移开，用红线框选住碳膜，配合OBJ FOCUS 的FINE 或COARSE调出傅里叶椭球后，采用OBJ STIG+STIG X Y将椭球调节为圆形120 K 将样品移开，用红线框选住碳膜，先采用OBJ STIG+NTRL调出傅里叶椭球，再配合OBJ FOCUS 的FINE 或COARSE，采用OBJ STIG+STIG X Y将椭球调节为圆形。

JEM-2100F场发射透射电镜用双倾样品台非公开招标意见公示
粉末冶金研究院“JEM-2100F场发射透射电镜用双倾样品台”项目采用拟采用非公开招
标方式进行，该项目拟从捷欧迪拓姆（上海）贸易有限公司购买。

现将有关情况向潜在供应
商征求意见。

征求意见期限从2015年9月16日起至2015年9月23日止。

潜在供应商对公示内容有异议的，请于公示期满后两个工作日内以实名书面（包括联系人、地址、联系电话）形式将意见反馈至中南大学资产与实验室管理处（联系电话：88836825 联系人：肖老师）。

附：专家论证意见及专家姓名、工作单位、职称。

申请单位理由：
粉冶院的JEM-2100F场发射透射电镜配件双倾样品台、机械泵已使用7年，出现老化和
故障现象，已维修过多次，目前需要更换。

因双倾样品台、机械泵零部件是透射电镜不可缺
少的重要配件，而其他公司生产的零部件与JEM-2100F透射电镜均不兼容，只能向捷欧迪拓
姆贸易有限公司（日本电子在中国的代理公司）购买，故申请非公开招标采购。

2015年9月16日
JEM-2100F场发射透射电镜用双倾样品台
非公开招标采购专家论证意见表
2015年9月16日。

JEM－2100f透射电镜测角台的维护与故障处理刘小青;邓志刚;罗婷婷;谢峻林【摘要】简述了JEM －2100f透射电镜测角台结构及样品杆进样、取样工作原理，分析了引起测角台故障的原因，阐述了测角台故障处理方法及日常维护技巧。

%In this paper ,the goniometer structure and working principle ofinserting/removing speci‐men holder of JEM‐2100f transmission electron microscope were briefly introduced ,the goniometer failure causes were analyzed ,the fault handling methods and daily maintenance skills of goniometer were described.【期刊名称】《分析仪器》【年(卷),期】2015(000)002【总页数】3页(P96-98)【关键词】透射电镜;测角台;维护;故障处理【作者】刘小青;邓志刚;罗婷婷;谢峻林【作者单位】武汉理工大学材料研究与测试中心，武汉 430070;武汉理工大学材料研究与测试中心，武汉 430070;武汉理工大学材料研究与测试中心，武汉430070;武汉理工大学材料研究与测试中心，武汉 430070【正文语种】中文JEM-2100f透射电镜测角台(以下简称测角台)是透射电镜成像系统的重要组成部分，是JEM-2100f透射电镜能够在纳米及原子尺度进行物质微观形貌观测和晶体结构研究的关键部件之一。

测角台一旦出现故障势必导致透射电镜无法正常工作，熟悉测角台结构及其工作原理，掌握测角台的维护与故障处理技巧由此显得非常重要。

透射电镜维护与故障处理专业性很强 [1-8]。

对测角台而言，如果不是机器老化或测角台本身质量问题，测角台故障主要与样品杆前处理不够，以及进样、取样操作不当有关。

JEM-2100F/2200FS操作说明制作：北京东方捷欧技术服务站马宁一，开机（此步只能由实验室管理员操作）。

1. 合上配电柜中电镜主机的单相电源，同时合上循环水的三相电源。

2. 合上主机的稳压电源开关。

3. 合上主机电源柜上的电源开关。

4. 确认电子枪的模式转换器在COND模式（见图一）。

（图一）5. 按压主机控制台上的I 键2、3秒钟后松开，RP开始动作，主机启动。

6. 打开TEM控制PC，首先等待PC显示器右下角的图标由未建立通讯状态转变为已建立通讯状态，这通常要等待5分钟，再等操作控制台上按键指示灯变亮后双击桌面上图标打开TEM控制软件，确认Status Monitor-System中各项显示都为Running状态（如图二）。

（图二）未建立通讯状态（图三）：如果发生这种情况，关闭软件确认通信建立后再打开。

如果还不行，关闭计算机，然后再VME RESET，等1分钟再将PC打开，通信建立后打开软件。

（图三）7. 确认电源柜上的60L，20LSIP真空档位选择器在X10-6Pa的位置，并且指针基本上是在左端基本到底的位置，如指针指示超过0.5X10-6Pa,请立即通知服务中心。

（图四）8. 确认真空符合要求后加高压（在COND模式，从100KV起加，参照长假期处理）备注：如无法正常开机，请检查下列各项：1，检查电源，包括电源柜中的主闸及电镜分开关是否正常，稳压电源是否在开启状态，以及主机电源柜的空开是否在开启状态。

2，打开Status Monitor-Alarm，察看是否有变红的报警提示(一般会自动弹出此报警窗口，如图五)，如有请与服务中心联系。

（图五）3，打开TEMCON软件后弹出下列窗口（图六）是由于过早打开软件造成，关闭软件后再次开启此问题就会解决（图六）二，插拔样品杆1，放入样品杆前，如当时EMSN 是ON 的状态不要关掉灯丝（热场的灯丝一般总保持在发射状态，所以无须关灯丝，这是与普通电镜的区别之处），同时更换不同的样品杆要在计算机里选择相应的型号。

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.。

JEM-2100培训一、开机程序：1.检查各仪表的读数是否正常（一般一个月检查一次）。

a．离子泵（SIP）：开灯丝前应保证真空压力小于4*10-5Pa；b．高压箱：未开高压时，高压箱SF6（高压绝缘气体）气压表大于0.01MPa;电子枪SF6气压表0.28-0.32（主机左侧下方圆表），该压力值不能低于0.28，低于该值不能启动，当前指针在0.3左右；c．水阀压力：左侧Lens（0.06MPa），中间DP泵（0.06MPa），右侧Lens units(0.04MPa)，d．循环冷却水箱：温度在18（+/-0.5）度；e．空压机在启动状态：压力表位于主机左侧下方（上面方表），当黑色指针大于红色指针表示空压泵启动，红色指针当前位置为0.25左右；空压机一般一个月放一次。

f．主副系统通讯连接：若通信中断，操作面板右侧后方有重启开关。

g．一般情况下，Gun，Column，Specimen和camera的值Ready状态时为<35，但主要看电源柜上离子泵读书，RT值为54。

抽真空方式为：机械泵抽RT室（储气室）；DP泵抽照相室和样品室，DP泵抽到一定程度后SIP离子泵启动抽气，此时潘宁规工作显示真空度值。

2.加液氮：在冷阱中加入液氮，第一次加满后盖上盖子5min后液氮会喷出，再加一次。

一天工作中，隔4个小时要加一次（早上9点左右加满，晚上4点多关的话，中间可以不用再加液氮）。

一旦加了液氮，下班时必须烘烤冷阱。

3.升高压（慢点好）：a.点HT ON，高压自动升到120KV；b.程序升高压，Target HT 160KV，间隔0.1KV，1sec，约6.7min，点START；c.程序升高压，Target HT 180KV，间隔0.1KV，2sec，约13.4min，点START；d.程序升高压，Target HT 200KV，间隔0.1KV，3sec，约20.1min，点START；4.放样品：样品杆中放入待观察样品，单倾杆是铜网正面向上，双倾杆是铜网反面向上。

JEM-2100（HR）透射电子显微镜操作规程1检查仪器状态、实验室环境1.1离子泵真空度必须优于4×10-5Pa；1.2电子枪、镜筒、照相室、储气罐真空状态必须显示为READY；1.3冷却水箱的温度，包括进水口（左）、出水口（右）均必须在17.5℃~18.5℃之间；1.4电脑操作界面无警报提示；1.5室内温度在17℃~25℃之间，湿度在60%以下。

注意：出现以上任何一点异常均不得进行下一步操作，须立即告知仪器管理员。

2升电压每天做第一个实验前需升电压。

图1.2 图1.3 图1.4注意：升电压时必须注意Beam current 的稳定性，当每步完成时的Beam current 超过对应值（即高压箱放电）时，必须等Beam current 自我恢复到对应值并稳定一段时间才能进行下一步操作。

3 加液氮3.1加冷阱液氮每天第一次加冷阱液氮时必须分两次加，先加入少量（1/3瓶热水瓶）预冷，待冷阱温度稳定后再加满，此后每隔3~4个小时加一次液氮（直接加满）。

3.2加能谱仪液氮每隔1天加一次能谱仪液氮，此工作由电镜楼楼管负责，若能谱仪发出缺少液氮的警报声应立即告知楼管或仪器管理员。

注意：加液氮时观察屏的盖子一定要盖上，以防液氮腐蚀铅玻璃；操作面板也盖上塑料薄膜以防止液氮滴溅腐蚀按键。

4 装样、进样注意：任何通过该操作培训、考核的用户未经授权不得对其他用户进行培训，违者重罚。

5 加灯丝（发射电流） 点击Filament ON注意：加灯丝前须确保Beam current 在101μA 左右，离子泵真空度优于2×10-5Pa 。

冷阱能谱仪液氮罐6观察6.1普通形貌MAG1）,6.1.2 放大倍数调至40K6.1.3 , 至图象不晃动；法二：6.1.4 聚焦（OBJ FOCUS6.1.5 ，聚焦后冻结后打开）6.1.6 保存图像6.2高分辨像6.2.1 检查电压中心：将放大倍数调至400K，光斑散开，按HT WOBB检查电压中心是否对中（图像有无左右上下晃动，有晃动则电压中心没有对中）。