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（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。

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。

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。

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.。

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。