场发射扫描电子显微镜S-4800操作规程

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。

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EV AC键，当EV AC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A.B.C.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。

5.对中调整改变加速电压和电流时，或图像在高倍聚焦发生漂移时，需要进行对中调整，方法如下：(1)选取样品上一个具有明显特征的位置放在视场中心。

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。

场发射扫描电子显微镜（S-4800）操作规程开机1. 检查真空、循环水状态。

2. 开启“Display”电源。

3. 根据提示输入用户名和密码，启动电镜程序。

样品放置、撤出、交换1. 严格按照高度规定高样品台，制样，固定。

2. 按交换舱上“Air”键放气，蜂鸣器响后将样品台放入，旋转样品杆至“Lock”位，合上交换舱，按“Evac”键抽气，蜂鸣器响后按“Open”键打开样品舱门，推入样品台，旋转样品杆至“Unlock”位后抽出，按“Close”键。

观察与拍照1. 根据样品特性与观察要求，在操作面板上选择合适的加速电压与束流，按“On”键加高压。

2. 用滚轮将样品台定位至观察点，拧Z轴旋钮（3轴马达台）。

3. 选择合适的放大倍数，点击“Align”键，调节旋钮盘，逐步调整电子束位置、物镜光阑对中、消像散基准。

4. 在“TV”或“Fast”扫描模式下定位观察区域，在“Red”扫描模式下聚焦、消像散，在“Slow”或“Cssc”扫描模式下拍照。

5. 选择合适的图像大小与拍摄方法，按“Capture”拍照。

6. 根据要求选择照片注释内容，保存照片。

关机1. 将样品台高度调回80mm。

2. 按“Home”键使样品台回到初始状态。

3. “Home”指示灯停止闪烁后，撤出样品台，合上样品舱。

4. 退出程序，关闭“Display”电源。

注意1. 每天第一次加高压后，进行灯丝Flashing去除污染。

2. 冷场发射电镜一般不断电，如遇特殊情况需要大关机时，依次关闭主机正面的“Stage”电源、“Evac”电源，半小时后关闭离子泵开关和显示单元背面的三个空气开关，关闭循环水。

开机时顺序相反。

3. 每半个月旋开空压机底阀放水一次。

4. 待测样品需烘干处理，不能带有强磁性，不能采用铁磁性材料做衬底制样。

5．实验室温度限定在25±5℃，相对湿度小于70% 。

仪器维护1. 每月进行电镜离子泵及灯丝镜筒烘烤。

2. 每半年进行一次机械泵油维护或更新。

Operating Procedure for Hitachi S-4800 Scanning Electron MicroscopeCFN Laboratory1L-32C.Black/G.WrightOperation of the Hitachi S-4800 Scanning Electron Microscope (SEM) requires specific user training and authorization. This operating procedure is meant as a general overview of tool operation and is NOT A SUBSTITUTE for obtaining proper training and authorization.Users should have reserved tool access via the FOM calendar.NIRTRILE GLOVES ARE TO BE WORN AT ALL TIMES when handling sample specimens, sample stages, and any parts to be introduced into the tool vacuum chamber. Suitable gloves are located on the workbench to the left of the Hitachi SEM.Sample PreparationSuitable samples for imaging will be mounted on solid flat substrates such as silicon or glass.Sample specimens must be mounted on a sample holder for insertion into the tool. Several different sample holder sizes are available. Sample holders are located on the workbench.Mount sample on sample holder. Specimens should be mounted using either double-sided sticky tape or clips. Silver paint is to be used only if absolutely necessary.Samples may be blown free of dust and debris using the can of compressed air located onthe laboratory workbench.Clean and organize sample preparation area when finished.Microscope PreparationObserve that microscope is energized and ready for operation. If any warning lights indicate a problem then STOP and contact a staff member.Log into the FOM and activate your reserved session to turn on the Hitachi computer.Loading a sampleAfter mounting sample on a sample holder, adjust the specimen height using the specimen height gauge located on the workbench. To adjust the height, loosen the lock screw and adjust the specimen height so that the height of the highest point of the specimen is the same as the bottom of the height gauge. Then tighten the lock screw by holding the fixed upper part of the holder..Move to the SEM console. Verify that there is no sample stage already loaded in the chamber by looking at the small camera monitor showing a view inside the chamber.Click the EXC button on the control panel. The stage inside the SEM will move to the specimen exchange position. Once this occurs the indicator beside the button will turn green. (Normally the stage will be left in the exchange position.)Press the AIR button on the specimen exchange chamber. After 15 sec. a buzzer will sound indicating that the chamber has been vented.Open the exchange chamber door. Be SURE to use the handle to open the chamber door and DO NOT USE THE SAMPLE LOAD ARM. Pulling on the arm in this way can damage the sample lock vacuum. The exchange chamber door is interlocked and will not open unless all vacuum conditions are satisfied.Confirm that the specimen exchange rod is in the UNLOCKED position by turning clockwise until the UNLOCK mark faces upwardsInsert the two spring pins at the end of the rod into holes of the specimen holder.While holding the specimen holder, turn the knob of the specimen exchange rod counterclockwise until the LOCK mark comes upwards. The sample holder is now lockedonto the load arm.Pull out the sample exchange rod completely and close the exchange chamber door.Press the EVAC button on the specimen exchange chamber. This will pump out the loadlock. Press the OPEN button to open the gate valve to the chamber, which will happen when a suitable low pressure has been achieved.After the gate valve opens, slide the specimen exchange rod all the way into the chamber WHILE LOOKING INTO THE CHAMBER on the small microscope screen toensure that the specimen holder inserts into the guide rails.Turn the specimen rod knob to the UNLOCKED position.Pull out the specimen exchange rod completely while VISUALLY WATCHING that the rod disengages from the sample holder.Press the CLOSE button on the specimen exchange chamber to close the gate valve. The sample is now loaded into the chamber.Applying the SEM high voltageClick the ON button on the control panel at the left of the HV DISPLAY area. You will be asked to verify the size (diameter and height) of the sample holder you are using. If the one displayed is in fact the one you are using, click OK. If not, clickCANCEL. Set the size of the sample holder you are using in the STAGE menu. If you are using the cross- section stage then you should select a stage size of 4 inches.High voltage can be applied only if the HV DISPLAY area on the control panel is blinking in yellow and blue. If the indicator is solid blue then the SEM conditions are not appropriate for high voltage application. Once the high voltage has been applied the indicator will display (nonblinking) yellow.Use the HV CONTROL dialog window to set SEM accelerating voltage and emission current.To set the accelerating voltage, select a voltage from the Vacc list box.To set an emission current, set a current in the SET Ie to list box. Hitachi recommends 10uA emission current for normal SEM operation.Click the ON button on the control panel at the left of the HV DISPLAY area. The SEM will automatically turn on the accelerating voltage, the extracting voltage, and the emission current. These values are displayed in the HV DISPLAY area. The electron gun airlock valve will automatically open upon completion of gun turn-on.Once the high voltage is applied the ON button will change to SET, allowing the user to set the emission current during high voltage operation. The OFF button turns off the high voltage. Note that during SEM operation the current will drop gradually over time. You can reset to the specified emission current (typically 10uA) by pressing SET.After high voltage turn-on a message will appear saying: “Stage is at specimen exchange position. Move to Home position?” Selecting YES will move the stage to the Home position such that the center of the sample holder will be directly underneath the electron beam.Obtaining a sample imageThere are many possible imaging variations for using the Hitachi S-4800 tool and these depend on the type of sample being imaged. We include here a summarized list of many commonly- used possibilities but do not provide detailed descriptions or an exhaustive list. The user is directed to the tool operating manual (located on the workbench to the left of the Hitachi SEM) for a complete discussion.Imaging mode:Selecting a Magnification Mode: The SEM has two magnification modes, HIGH MAG and LOW MAG. Most common applications will utilize the HIGH MAG mode.Within HIGH MAG magnification mode, user specifies:Probe current mode: NORMAL of HIGH. Most applications will utilizeNORMALFocus mode: UHR or HR. UHR mode allows full range of working distances.Working distance (WD). Shorter WD means higher resolution. Longer WDallows greater depth of focus and more sample tilting.Focus depth: Best resolution attainable with this value set to 1.0Specimen bias voltage: Specimen can be voltage-biased during imaging tominimize sample charging effects.Magnetic sample: Use this mode for observation of ferromagnetic samplesDegauss operation:Setting ABCC link: Automatically adjusts brightness and contrast during sample imaging.Column Alignment Operation: Obtaining the highest resolution image will involve aligning the electron optical column. This operation is done entirely through an electromagnetic alignment (i.e., using the computer interface) without need for touching any knobs on the SEM column. Alignment conditions are saved for each accelerating voltage and probe current setting such that only minimal alignment adjustment should be necessary.Press TV1 to obtain an image on the screen.Typically the beam can be tuned up using only an APERTURE ALIGNMENT. The procedure is as follows:Set the magnification to about 5,000 and position a point of interest in the center of the display.Focus the image and correct astigmatism.Click APERTURE ALIGN in the ALIGNMENT dialog box and make adjustments such that the wobbling motion of the image is minimized.Turn off the APERTURE ALIGN mode by clicking the OFF button.Sample imagingDetector selection: The SEM has two secondary electron detectors, the UPPER and the LOWER detectors. User can select either detector or alternatively image using a mixture of the two signals. Select a detector on the SIGNAL SELECT block of the OPERATION panel.Image Magnification: Select image magnification by dragging the mouse in the MAGNIFICATION INDICATION area on the CONTROL PANEL. The magnification can also be set by rotating the MAGNIFICATION knob on the control box.Focus and astigmatism correction: Iteratively adjust focus and astigmatism using the knobs on the SEM control box.Brightness and Contrast: Adjust brightness and contrast either manually by using BRIGHTNESS and CONTRAST knobs on SEM control panel or by pressing ABCC button for automatic control.The recorded images are stored in a memory buffer and displayed across the screen bottom. At the end of the session you will need to save them in the appropriate folder.Unloading sampleRemember to wear gloves when unloading samples.When finished imaging, turn off the high voltage by clicking OFF on the HV DISPLAY area. Move the sample stage to the exchange position by clicking the EXC button on the control panel. Once this occurs the indicator beside the button will turn green.Press the OPEN button on the specimen exchange chamber to open the gate valveTurn the knob on the specimen exchange rod clockwise so that the UNLOCK mark is facing upwards.Insert the specimen exchange rod straight into the chamber and fit the two spring pins into the holes at the end of the specimen holderTurn the knob counterclockwise so the LOCK mark comes upwards to hook on the sample holder.VISUALLY INSPECT that the sample holder comes out with the rod as you pull the rod all the way out of the chamber.Press the CLOSE button on the specimen exchange chamber to close the gate valve. Press AIR to vent the loadlock.Open the exchange door (by its handle) and turn knob clockwise to UNLOCK position. The sample holder can now be disengaged from the sample rod.Close specimen exchange chamber door and press EVAC to pump the loadlock back down.CleanupLog into the FOM computer and end your session. This will turn off the Hitachi computer.Unmount your samples from the sample holder.Return sample stage to appropriate stage storage box located near the workbench at the rear of the laboratory.Clean workbench area and properly dispose of any materials used during sample preparation.TURN OFF laboratory lights when leaving the room。

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。

S 4800场发射扫描电子显微镜测聚合物s-4800场发射扫描电子显微镜测聚合物用s-4800场发射扫描电子显微镜观察聚合物一、实验目的1.了解扫描电子显微镜的工作原理和仪器结构。

2.掌握仪器的操作方法及聚合物样品的制备和处理方法。

3.观察聚合物样品的表面形态、结构和聚集状态。

二、实验原理1.电子显微镜成像原理电子枪（场发射枪）发射一束电子，这就是电子源，其最少截面的直径对场发射枪而言大约为10～20nm，这个小束斑经3和5两级聚光镜进一步缩小几百倍，最后再经物镜缩小并聚焦在样品面上，这时束斑直径最小可到3～6nm（约小于扫描电镜的分辨本领），电子束打在样品上，就产生各种信号。

二次电子和背散射电子信号是最常用的两种信号，尤其是二次电子。

信号由接收器取出，经光电倍增器和电子放大器放大后，作为视频信号去调制高分辨显示器的亮度，因此显示器上这一点的亮度与电子束打在样品上那一点的二次电子发射强度相对应。

由于样品上各点形貌等各异，其二次电子发射强度不同，因此显示器屏上对应的点的亮度也不同。

用同一个扫描发生器产生帧扫和行扫信号，同时去控制显示的偏转器和镜筒中的电子束扫描偏转器，使电子束在样品表面上与显示器中电子束在荧光屏上同步进行帧扫和行扫，产生相似于电视机上的扫描光栅。

这两个光栅的尺寸比就是扫描电镜的放倍数。

在显示器屏幕光栅上的图像就是电子束在样品上所扫描区域的放大形貌像。

图像中亮点对应于样品表面上突起部分，暗点表示凹的部分或背向接收器的阴影部分。

由于显示器屏幕上扫描尺寸是固定的，如14in(1in=25.4mm）显示器的扫描面积是267×200mm2，在放大倍数为十万倍时样品面上的扫描面积为2.67×2μm2如放大倍数为20倍时，则为13.35×10mm2。

因此改变电子束扫描偏转器的电流大小，就可改变电子束在样品上的扫描尺寸，从而改变扫描电镜的放大倍数。

2.电子显微镜的分辨率特性扫描电镜的分辨本领一般指的是二次电子像的空间分辨本领，它是在高放大在多重模式下，人们可以从照片中分辨出两个相邻物体之间的最小距离。

场发射扫描电子显微镜实验操作扫描电子显微镜（SEM）是一种能够获得高分辨率表面形貌信息的重要工具。

在实验室中，我们经常会使用场发射扫描电子显微镜来观察样品的微观结构和形貌。

本文将介绍场发射扫描电子显微镜的实验操作步骤。

实验准备在进行场发射扫描电子显微镜实验之前，我们需要进行一些准备工作。

首先，确保实验室环境干净整洁，以避免样品受到污染。

其次，检查扫描电子显微镜设备，确保设备正常工作。

最后，准备好待观察的样品，并确保样品表面平整干净。

样品处理与加载处理样品是进行场发射扫描电子显微镜实验的关键步骤。

首先，将待观察的样品切割成适当大小，并利用相关方法处理表面以去除可能的杂质。

然后，将样品加载到扫描电子显微镜样品台上，并使用夹具固定样品。

参数设置在进行扫描电子显微镜实验前，需要设置合适的参数以获得清晰的显微结构图像。

首先，调整加速电压和工作距离，以适应待观察样品的性质和尺寸。

其次，设置扫描速度和倍率，以获得所需的图像分辨率。

最后，根据需要选择不同的检测模式和滤波器。

图像获取与分析当参数设置完成后，可以开始进行样品的图像获取。

通过扫描电子束对样品进行成像，获得样品表面的细微结构信息。

在获取图像后，可以利用相应软件对图像进行分析，包括测量尺寸、分析形貌等。

同时，可以记录图像和相应数据以备后续分析。

结束实验与维护实验结束后，及时关闭扫描电子显微镜设备，并对设备进行清洁和维护。

将样品从样品台取下，妥善保存或处理。

同时，整理实验记录和数据，保留有关信息以备后续参考。

通过以上步骤，我们可以完成一次成功的场发射扫描电子显微镜实验操作。

这不仅可以帮助我们深入了解材料的微观结构和形貌，还可以为科学研究和工程应用提供重要参考。

希望本文对您进行场发射扫描电子显微镜实验操作有所帮助。