S-4800扫描电镜操作步骤

HITACHI H-7650 透射电镜操作规程编号: QW148 HITACHI S4800扫描电子显微镜操作规程样品准备及要求:1.含水样品测试前必须干燥，样品要尽量的小，多孔样品做之前一般要烘两到三天;2.粉末样品测试时尽量用最少量的样品，否则容易使电镜污染;3.严禁观察磁性样品;4.样品须处于样品台中央位置，样品表面平坦，样品厚度不可太大。

操作步骤:一、开机顺序1. 开墙上主机电源的开关，开启冷却循环水;2. 将仪器后面板处的主电源开关(Main Power) 打开，之后按下Reset键;3.启动Evac Power，等待TMP指示正常后顺序打开IP1、IP2 和IP3的电源开关:4.达到真空度要求后，开启操作台电源，PC机自动启动进入Windows操作系统，并自动运行S-4800操作程序，此时点击OK (没有密码)后自动进入S 4800操作软件。

二、样品安装1.在实验台上事先粘好样品，并用高度规检测其高度;2.装样品前确认工轴、WD,x,y以及Rotation是否复位(Z轴=8，WD=8，x=25，y=25，Rotation=0)，如未复位，将其复位;3.点击样品交换室的Air键，当听到笛的一声后轻轻的拉开样品交换室;4.将样品杆手柄处于Unlock位置，把样品机座装于样杆的香蕉头处并转动手柄到Lock位置;5.轻轻推住样品交换室，点击Evac键，抽好真空后点市Open键，样品交换室与样品室间的闸门自动打开;5. 轻轻的推动样品杆的手柄将样品送至于样品台上，旋转手柄至Unlock, 拉出样品杆，最后点击Close关闭阀门，安装样品结束。

三、图像观察1.加高压后即可进行调试观察;2.首先在TV1模式下找到所要观察的区域;3.在高倍下用coarse键粗聚焦，然后用fine键细调聚焦，直到图像清楚;4.放回到观察倍数，用ABC或手动调到适合的对比度:5. 在SLOW模式下观察调试后的图像，不合适重新执行步骤2，3，若合适即可拍照。

S扫描电镜操作步骤集团标准化工作小组 [Q8QX9QT-X8QQB8Q8-NQ8QJ8-M8QMN]扫描电镜S-4800操作规程一、日常开机打开Display开关，电脑自动开机进入s-4800用户界面，PC_SEM程序自运行，点击确认进入软件界面。

二、装样品1.将样品台装在样品座上，根据标尺调整高度及确认样品位置后旋紧。

2.按下AIR键，当AIR灯变绿时拉开样品交换室，水平向前推出交换杆，把样品座插在交换杆上，逆时针旋转交换杆（即按照杆上的标示转至LOCK）锁定样品座后，将交换杆水平向后拉回原处。

3.关闭交换室，按下EVAC键，当EVAC绿灯亮时，按OPEN键至绿灯亮样品室阀门自动打开。

4.水平插入交换杆，直至样品座被卡紧为止，顺时针旋转交换杆（即按照杆上的标示转至UNLOCK）后水平向后拉回原处，点CLOSE键至绿灯亮样品室阀门自动关闭。

三、图像观察1.加高压点击屏幕左上方的高压控制窗口，弹出HV Control对话窗。

选择合适的观察电压和电流，点击ON，弹出提示样品高度的对话框，点击确定出现HV ON提示条，待图像出现后，关闭HV Control对话窗。

2.在低倍、TV模式下，找到所要观察的样品，点击H/L按钮切换到高倍模式，通过调节样品位置，找到所要观察的视场。

3.聚焦、消像散选好视场后，放大到合适的倍数聚焦消像散。

先调节聚焦粗调和细调旋钮，使图像达到最佳状态，若图像有拉长现象，则需进行消像散。

调节STIGMATOR/ALIGNMENT X使图像在水平方向的拉长消失，再调节STIGMATOR/ALIGNMENT Y使图像在垂直方向的拉长消失。

4.图像采集及保存用键或BRIGHTNISS/CONTRAST旋钮自动或手动调节图像的对比度和亮度，扫描速度变为慢扫，点击抓拍按钮进行采集。

采集后暂时存放在窗口下侧，选中要保存的图像，点击Save，弹出Image Save对话框，输入文件名，选好存储位置保存即可。

冷场发射扫描电子显微镜S4800操作说明（普通用户）燕山大学材料学院材料管A104（场发射，钨灯丝）编写人：李月晴吕益飞普通用户在熟练操作1个月后，如无不良记录，可申请高级用户培训。

高倍调清晰：局部放大(Red) →聚焦Focus→消像散一、日常开机1，开启冷却循环水电源。

2，按下Display开关至，PC自动开机进入用户界面并自动运行PC_SEM程序，以空口令登入。

3，打开信号采集开关，位置打到1，为打开。

4，打开电源插排的开关。

5，打开装有EDS软件的主机电源。

6，记录仪器运行参数(右下角Mainte)，即钨灯丝真空度。

如：IP1：0.0×10-8Pa；IP2：0.0×10-8Pa；IP3：9.6×10-7Pa。

PeG-1，<1×10-3；PeG-2，<1×10+2。

注意：PeG≤1×10-3Pa时才能加高压测量。

记录的参数：①点Flashing时会显示：In2(Ie)Flashing时电流最大值，如32.9μA；②加上高压后会显示，V ext=3.4kV。

二、轰击（点flashing，即在阴极加额外电压）目的：高温去除针尖表面吸附的气体1，最好在每天开始观察样品前一时做flashing；2，选择flashing intensity为2 ；3，若flashing运行时Ie小于20µA，则反复执行直至Ie值超过20µA且不再增加。

4，若flashing后超过8个小时仍继续使用，重新执行flshing 。

三、加液氮容积不要超过1L，能维持4~6h。

四、样品制备及装入样品制备简单，对样品要求较低，只要能放进样品室，都可进行观察。

1，化学上和物理上稳定的干燥固体，表面清洁，在真空中及在电子束轰击下不挥发或变形，无放射性和腐蚀性。

2，样品必须导电，非导电样品，可在表面喷镀金膜。

3，带有磁性的样品，由于物镜有强磁性，制样必须非常小心，防止在强磁场中样品被吸入物镜或分散在样品室中，工作距离(WD) 要大于8.0mm。

S-4800日立扫描电子显微镜（SEM）简易操作指南一、开机前准备1.1制备样品（带口罩与手套进行）SEM样品制备相对简单，原则上只要能放入样品室的样品，都可进行观察。

但需注意以下事项：a)样品在物理上和化学上必须要保持稳定，在真空中和电子束轰击下不挥发或变形，没有腐蚀性和放射性。

（通常是干燥固体。

）b)由于光源是电子，样品必须导电，非导电样品可喷镀金膜。

金膜在一定程度上会影响样品原有形貌。

（若样品本身导电，衬底不导电，如蓝宝石上的ZnO，只需用导电胶把样品表面连到样品台。

）c)由于物镜有强磁性，带有磁性的样品制样必须非常小心，防止在强磁场中样品被吸入物镜或分散在样品室中。

通常磁性样品必须退磁，且工作距离（WD）须大于8mm。

具体操作过程：(1) 按待测样品数量选择样品台，（支持直径d=5mm,15mm,1 inch,2 inch等规格，若要观测截面可选择带角度的样品台）。

(2) 剪一小段导电胶，粘到样品台上。

若样品为粉末，则把粉末撒到导电胶上，用吸耳球或高压氮气吹扫掉导电胶上未粘紧的粉末；若是块状样品，则把样品牢牢粘到导电胶上，用手轻轻推，样品不会左右晃动。

（为观测时方便定位，将样品排列成行（或列），并在行下方（或列左侧）标上数字编号。

）(3) 样品粘贴完成后，用吸耳球或高压氮气吹扫掉样品台上的粉末、灰尘、水珠、唾沫等（会影响照片质量，甚至使真空度下降而无法加高压，推荐认真执行。

）1.2查看真空度打开前面板盖，点击MODE按钮直至IP1指示灯闪，在登记表记下MULT INDICATOR数码显示管的读数，同理读取IP2，IP3并记录。

确认IP1<2E-7，IP2<2E-6，IP3<5E-5。

（通常情况都是IP1显示0E-8，IP2显示0E-8，IP3显示0E-8或aE-7,1<a<9。

）如图1所示：图1 按MODE读取IP1-IP3二、开机操作2.1开机a)开启冷却循环水电源，循环水温度显示应在15-20℃，水位应浸没金属线圈。

P r o c e d u r e f o r FIRST USER ofFIRST USER of day1.Turn on CPU power (inside lower cabinet)2.Turn on Computer Monitor3.Login to Windows (no password)4.Login to S-4800 software by clicking icon PC-SEM to open control panel (nopassword)5.Click box (Vacc, Ie) upper left of Toolbar (if dialog box w/FLASHING button isnot open)6.Click Flashing.7.“Flashing Execute ok?” Click Execute (Intensity 2 is normally ok).8.Repeat steps 5 & 6; Ie will transiently register current – should be between 20 and40 µA.9.Check Evacuation Control Panel for ion pump readings (IP1, 2, 3). Values are in10-3 Pa (For Lab Manager Only)ALL USERSU s e r S e t-u p f o r ALL1.For sample exchange, be sure that the sample stage settings – Rotation (R) = 0.0,Tilt (T) = 0.0, X = 25.0, Y = 25.0 and Z = 8.0 are all set to these positions asindicated on the front of the microscope.2.Click AIR button on right side of microscope – after a few seconds, air isadmitted to the Sample Exchange Chamber (SEC). There is a beep when the SEC is at atmospheric pressure.3.Pull open and turn black knob CW to UNLOCK position and remove sampleholder.4.While wearing gloves and at workbench, not on stage, install new sample onsample holder and adjust the height using the fixture console. See pictures taped to wall for details. This will give a working distance of 8 mm when the sample is inserted into the sample stage.5.Insert sample holder aligning to dual bayonet connectors in the SEC; rotate blackknob CCW to LOCK position. Then pull SEC and rod out to guide endpoint.(Check that rod is pulled out to endpoint). CLOSE SEC door.6.Press EVAC button – air is pumped out of the SEC. A beep sounds when vacuumis attained.7.Press OPEN to open the chamber door – a beep sounds when the chamber door isopen. Visually examine to check that stage is in chamber.8.Push rod all the way in until the sample holder fully engages the sample stage;rotate black knob CW to UNLOCK position.9.Grasp black knob and pull back to end of guides. Then make sure that the sampleholder remains on the stage.10.Press CLOSE to close the chamber door. Beep sounds when the door is closedand the vacuum is ready.11.To turn HV ON. Click ON (left of gray box on Toolbar) – for normal operation,V acc=15 kV and I e=10 µA. I e will drop during the first ~30 minutes of usage due to formation of a monolayer of absorbed gas on the tungsten emitter tip. To set Accl Voltage (VAcc) click large black arrow and set KV at .5 to 30. The lower the KV the more surface detail imaged and greater the KV will increase imaging the interior structure/views. Periodically click SET (right side of Toolbar) to re-set the emission to ~10 µA (this will increase V ext).12.Scan rate is selectable on the toolbar – TV1, Slow1 and Slow3.13.H/L button on toolbar selects low magnification (30 X – 2 KX) or highmagnification (800X – 500KX) modes. The magnification can be adjusted with the knob on the control box.14.ABC button on toolbar is Auto Brightness / Contrast. These can also be adjustedusing the Brightness and Contrast knobs on the control box.15.At the beginning of a session, it is important to check the alignment of theelectron beam. Click H/L and set magnification at ~5000X. While increasing magnification Beep will occur at 2000X. The beep is a reminder to click on H/L to reset mag to high. Click ALIGN on the toolbar. A menu box will appear.Click on BEAM ALIGN and center the beam using X and Y knobs(stigma/alignment) on the control box. Click STIGIMATION X, and stopmovement of image using X and Y knobs on control box. Click STIGIMATION Y and stop image movement using X and Y knobs. Click APERTURE ALIGN and stop movement of image using X and Y knobs on control box.Click OFF in ALIGN menu box.16.Adjust coarse focus until WD is ~ 5mm. It may be required to click on “resetfocus condition” in popup dialogue box.17.To obtain the best image resolution, carefully adjust coarse, fine focus, x-stigmation and y-stigmation KNOBS at a high magnification. Adjust brightness and contrast, and observe image in Slow2 mode (button on toolbar). N.B., set Working Distance (WD) only in Hi Mag mode to ~ 5mm by using the Z adjust knob18.Set magnification at ~ 1000X. Then lower Z by turning Z knob on scope.19.Find field of interest by moving X/Y stage. Set to required magnification.20. Before Image captur, be sure to set slow scan mode for best image quality.21.To capture an image, click the 1280 button on the toolbar to the right of the H/Lbutton. This will capture a 1280 x 960 image. The resolution can be changed using the pull-down arrow.22.When the image is captured, it is displayed in the lower left, highlighted inyellow.23.Click the PCI button in the lower left to export the image to QuartzPCI imageanalysis software.24.In QuartzPCI, click File – can SAVE or EXPORT image (e.g. to a JPEG file).Clicking SAVE will actually create 3 files of which one is PCI format. EXPORT, which creates 1 file, is more efficient choice.25.Back in S-4800 software, click RUN on toolbar to resume scanning.S h u t D o w n P r o c e d u r e1.Turn off beam2.Return stage to proper settings.3.Press OPEN4.Insert rod at unlocked position5.Turn rod to locked position6.Pull rod and sample out to endpoint.7.Press CLOSE8.Press AIR, wait for beep9.Slide open SEC10.Turn black knob to UNLOCK and remove sample11.If done, close SEC and press evacuate to pump down chamber12.Turn off monitorCommon Abbreviations and DefinitionsVext (Extracting voltage) Voltage that is applied between the cathode and first anode.Electrons are emitted from the cathode.Vacc (Accelerating voltage) electrons are accelerated by an accelerating voltage.Flashing- cleansing of the cathode (FE tip) by turning on the flashing power supply in order to remove absorbed gas on the surface of the cathode. This is to be done,before usage, first thing in the morning or the evening.Ie (emission current) is generally set to 10 μA for normal operation.HV (high voltage) Applies HV to the electron gun and controls the extracting voltage to obtain the emission current.Beam monitor (adjustment of the reference voltage) is provided to reduce tip noise, which is a low frequency noise caused by fluctuations of the emission current.Dividing the image signal by a reference signal that is proportional to probe current can stabilize it. It is recommended to keep the beam monitor on for normaloperations.Beam indicator (box with cross hairs) to reset image shift to the center, click theindicator areaUnder signal selection box, L.A is low angle. When BSE is selected, the amount of BSE signal is controlled by BSE ratio selection box. Low angle BSE will be detected with L.A0 to L.A100. With the larger number, the amount of SE is suppressed and results in a BSE richer image.HR is high resolution mode where the short working distance range is limited and it is easier to use at a longer working distance (>5mm).UHR is ultrahigh resolution mode where the full working distance range is availableUnder scan size…Small screen mode has faster frame speeds and in some cases results in better image quality.Dynamic focus allows you to focus the beam for the entire field of view.Condenser lens 1 setting to lower values (1-16 range) results in weaker excitation and larger Probe Current and larger “spot size” and vice versa. Recommended value is 5. Unclicking box will turn off lens and this condition is typically used for mechanical alignments.Focus depth is recommended to be set at 1.0 or larger to increase focus depth.Degauss button should be clicked after changing focus widely or before making the electron optical axis alignment (You can do this by hitting the F2 hotkey)To select many images, press and hold down the control keyLayout button opens the Report Generation window for printing the imageSC stands for the specimen chamberApt heat should be set at auto. If the objective aperture lens is contaminated, charging will degrade image quality and the image will drift because of micro discharge. Such problems are noticeable at low accelerating voltages. The aperture is heated to about 150C to remove contaminants to one tenth or less of what it would be at room temperature.The display switch is on when the line is depressed (a 1 or switch is up is on)For use at high magnifications or low accelerating voltages, the use of the anti-contamination trap is recommended to prevent specimen contamination by hydrocarbon build-up. Fill the trap with liquid nitrogen (LN2). The Dewar is usable for about 5 hours at room temperature. ** Before introducing air into the chamber, wait for a few hours until the LN2 Dewar has completely emptied so that the trap will not frost up and deteriorate the vacuum. The air introduction value does not have a protection link with the cold trap.WD (working distance) is the distance between the bottom face of the objective lens and the surface of the specimen. At a shorter working distance, higher resolution is obtainable. At a longer WD, a larger tilt angle and a greater depth of focus are obtainable. To change the WD, move the Z to a lower #, which moves the stage up. Short-Cut KeysCtrl O Open SEM Data ManagerCtrl P PrintCtrl C Copy ImageCtrl L Open Captured Image windowF1 Help can be openedF2 Activates Degauss functionF5 Runs or stops scanning alternatelyF4 Changes alignment mode to the next stepShift F4 Changes alignment mode to previous stepNotes for AdministratorPassword is “hitachi”To preset magnifications, open the Image Tab of the Setup dialog window and input desired values in the three Preset Magnification boxes. A PM mark is indicated in the Magnification indicator area when the preset magnification is set.Setting up logins: Option menu, login setting (must be logged in as S-4800) to create or change login names and passwords for each user. Can also change password setting under Option menu.TroubleshootingWhen operating at short working distances and experiencing uneven brightness at low magnifications, turn specimen bias voltage off.Magnetic samples such as iron can cause astigmatism correction to be difficult.The use of double-sided adhesive tape may cause specimen drift. Use the least amount possible to minimize out gassing.Perform beam and aperture alignment when you change HV value, accelerating voltage, probe current mode, or setting of Cond Lens1. For all alignments, either drag the mouse in the grid area of the Alignment dialog window or adjust theSigma/alignment X and Y knobs on the control panel. Set the magnification at 5, 000X for aperture alignment.The lowest magnification that can be obtained at a WD of 25mm or more is 20X.To maximize brightness and contrast, start B/C monitor mode by double clicking the MontiF button or operate menu, BC monitor. When the maximum and minimum values of the waveform are adjusted to fit within the upper and lower reference lines, appropriate brightness and contrast will be obtained. To terminate this mode, click the cancel button in the BC monitor mode message or one of the scanning speed buttons.To maximize focus, set magnification to 1,000X and start the focus monitor by clicking the Monitor button (MontiF) on the control panel and focus the image so that the waveform shows sharp peaks. To close the focus monitor, click the cancel button in the focus monitor mode or click one of the scanning speed buttons.Auto focus or auto stigma functions will not work correctly with little or no surface detail on the specimen or when the specimen is charging. These functions should also be performed at magnifications higher than 5,000X.For high magnification work, staging locking is recommended for better mechanical stability. The Z and T axes are locked or released by the Lock button on the specimen stage. ** If the Z or T axis is moved while the stage is locked, the stage mechanism may be damaged. X, Y, and R axes are free and movable when the stage is locked.Objective lens apertures are 50 μm for settings 2 or 3. The electron optical column of the HRSEM is designed to achieve highest resolution with a 50 μm aperture. Suggestions on getting better image quality:1.Higher spatial resolution can be obtained at higher accelerating voltages2.For uncoated, insulator specimens, accelerating voltages less than 1kV arerecommended for minimizing charging. In some cases, high accelerating voltages (20kV or higher) may produce a better image.3.Influence of contamination at lower voltages is more pronounced4.Disturbances by leakage magnetic field (wobbling or distortion of the image) aregreater at low accelerating voltages.5.Generally a soft-tone image is obtained at low accelerating voltages because moreSEs are detected than BSEs.6.Ion Pump readings should be this or better:IP1: 2 x 10^-7 PaIP2: 2 x 10^-6IP3: 5 x 10^-5SC: 2 x 10^-3Stereo ImagingPg 3-165BSE ImagingA mixed signal is available. When +BSE is selected, the amount of BSE signal is controlled by the BSE ratio selection box. Low angle BSE will be detected with LA0 to LA100. With a larger number, the amount of SE is suppressed and this will result in a BSE richer image. HA results in a high angle BSE image.Refer to sections 3.5.1 SE Detector and 3.5.1.2 Signal control。

一、介绍Hitachi S-4800场发射扫描电镜采用了新型ExB式探测器和电子束减速功能,提高了图象质量(15 kV下分辨率1 nm)，尤其是将低加速电压下的图象质量提高到了新的水平(1 kV下1.4 nm)；新型的透镜系统，提高了高分辨模式、高速流模式、大工作距离模式、磁性样品模式等多种工作模式，使其能够精确和清楚地捕捉最短暂的瞬间。

二、操作说明1．开机（1）日常开机：打开Display的开关，PC自动开机进入用户界面并自动运行PC_SEM程序，以空口令登入。

（2）完全关闭电源后开机：接通配电盘电源→拔上MAIN Swith 开关→按一下Reset按钮，→将MAIN控制面板上EVAC POWER按至ON，SC EVAC指示灯处于常绿状态后，等半小时→按下Display开关至ON, PC 自动开机进入用户界面并自动运行PC_SEM程序，以空口令登入。

2．图像观察（1）装入样品制样→把样品托装入样品座，并用标尺确定高度、旋紧→按AIR按钮→将样品座插在样品交换杆上，并锁紧→将交换杆拉至尽头卡紧，关闭交换室→按下EVAC按钮→按下OPEN 按钮打开MV-1后，推进交换杆，旋转样品杆UNLOCK位置后拉出交换杆→按下CLOSE 按钮。

（2）图像观察及保存SC真空恢复正常后（显示为L E-3）→选择适当的加速电压（Vacc）→加高压→在低倍、TV模式下将图像调节清楚→聚焦、消象散→Slow3确认图像质量→点击Capture按钮拍照→点击右下方Save按钮→选择保存位置、使用者及样品信息，保存。

（3）结束观察点击OFF按钮关闭加速高压→将放大倍率还原设至×1.00K→按操作界面上home使样品台回到初始位置→依照装入样品的方式反序取出样品。

3．关机（1）日常关机退出PC_SEM程序→退出Windows XP系统→关闭DISPLAY（2）完全关机短时间关机：退出PC_SEM程序→退出Windows XP系统→关闭DISPLAY→关闭EVAC→等待约35分钟后Multi Indicator区域显示“POFF”→关闭MAIN SWITCH→关闭电源总开关。

S4800型SEM操作指南S-4800具体操作过程1.日常开机按下DISPLAY开关至“━”，PC自动开机进入用户界面并自动运行PC_SEM程序，以空口令登入。

2．轰击（flashing）FE-SEM在作样之前，必须要进行轰击（作为电子源的FE尖端的清洁）。

在开始使用时，轰击频率为一次。

但是，电压外加时间累计超过8小时，发射电流开始不稳定，需要再次轰击。

轰击后可以立即观察图象。

但是在最初的1小时左右，有时会有图象干扰（图象中出现明暗的横线）。

进行高分辨率的观察时，最好在轰击完1小时以上之后进行观察。

执行过程：（1）点击控制面板上的加速电压显示区域，出现加速电压HV设定画面。

（2）点击“Flashing”键后，出现轰击执行窗口。

（3）确认轰击强度是否确实是“2”后，点击“执行”键。

HV的Ie（发射电流）显示器显示2秒钟轰击产生的发射电流，电流值大约为20uA-30uA，有时仅轰击一次，达不到所要求的值，这时需要连续轰击2-3次。

（为了保护FE灯丝，中间间隔30秒钟后，才可以进行下一次轰击。

）3．样品制备及装入3.1 样品制备相对简单，原则上只要能放入样品室的样品，都可进行观察。

高度保持在2cm以内，直径在4cm以内。

但是，样品在化学上和物理上必须要保持稳定，在真空中和电子束轰击下不挥发或变形，没有腐蚀性和放射性。

由于光源是电子，样品必须导电，非导电样品可喷镀金膜。

金膜在一定程度上会影响样品原有形貌。

带有磁性的样品，由于物镜有强磁性，制样必须非常小心，防止在强磁场中样品被吸入物镜或分散在样品室中。

操作过程：(1) 剪一小段导电胶，粘到样品台上。

（非导电样品可以用双面胶。

）(2) 把粉末撒到导电胶上，用吸耳球或高压氮气吹扫掉导电胶上未粘紧的粉末；若是块状样品，则把样品牢牢粘到导电胶上，用手轻轻推，样品不会左右晃动。

（3）样品若不导电，需要喷镀金膜。

3.2 样品装入：（1）把样品台装入样品座并调节样品表面与标尺在同一高度，旋紧。