FEI Quanta FEG 650 User's Operation Manual
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FEI Quanta FEG 650 User's Operation Manual

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The Quanta FEG
250 / 450 / 650
User Operation Manual
th
5
Edition
20 August, 2010
Copyright © 2010
FEI Company
All rights reserved

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  • Page 1 The Quanta FEG 250 / 450 / 650 User Operation Manual Edition 20 August, 2010 Copyright © 2010 FEI Company All rights reserved...
  • Page 2 Trademark Acknowledgments FrameMaker™ is a trademark of Adobe Systems Incorporated. Microsoft® is a registered trademark of Microsoft Corporation. Windows XP™ is a trademark of Microsoft Corporation. Production Acknowledgments This manual was produced using FrameMaker™ document publishing software Technical Authors Martin Dufek...

  • Page 3: Table Of Contents

    TABLE OF CONTENTS Chapter 1 Preface User Manuals ..........1-1 The User Safety Manual .
  • Page 4 Control possibilities ........4-38 FEI Account Administrators ....... . . 4-38 Account Logging .
  • Page 5 Stages Types and Accessories ....... 7-2 Quanta FEG 250 – 50 mm Stage ......7-2 Quanta FEG 450 / 650 –...
  • Page 6 Replacing the Aperture Module ....... 8-8 Replacing the Aperture rod ........8-8 Gaseous Detectors .
  • Page 7 Cooling Stages Basic Operations ......9-30 Water Cooled Temperature Stage Operation Termination ..9-32 Wet STEM .
  • Page 8 C-vi...

  • Page 9: Chapter 1 Preface

    PREFACE User Manuals THE USER SAFETY MANUAL provides important information required during an operation and a maintenance for a product and personal safety. Be sure to read this document (which is delivered as the PDF file and in the printed form also) at least.

  • Page 10: How To Use This Manual

    Preface: How to Use this Manual How to Use this Manual This manual is available in two forms, the electronic PDF file and the printed form (option). It is recommended to read this manual before operating any of the microscope function. Most importantly, you should locate the topics necessary to operate the microscope in the proper way to safely achieve the best results.

  • Page 11: Chapter 2 System Overview

    SYSTEM OVERVIEW The Quanta FEG Scanning Electron Microscope (SEM) produces enlarged images of a variety of specimens, achieving magnifications of over 100 000× providing high resolution imaging in a digital format. This important and widely used analytical tool provides exceptional field of view, minimal specimen preparation, and the ability to combine the technique with X-ray microanalysis.

  • Page 12: Vacuum System

    System Overview: How Quanta FEG SEM Works FIGURE 2-1 SEM SCHEMATIC OVERVIEW FILAMENT PINS ELECTRON GUN SUPPRESSOR EMITTER LENS SYSTEM CONDENSER LENS(ES) SCAN UNIT DEFLECTION SCAN GENERATOR SYSTEM FINAL LENS DETECTION UNIT SPECIMEN VACUUM SYSTEM The entire electron path from gun to specimen must be under vacuum so that the electrons do not collide with air molecules.

  • Page 13: Image Viewing And Capture

    POSITIONING OF THE STAGE A choice of computer-controlled high-accuracy multi-axis stages offers precision specimen manipulation and automation for overall spatial orientation on highly repetitive or extremely irregular samples. FIGURE 2-2 QUANTA FEG 250...

  • Page 14: System Layout Of Quanta Feg

    System Overview: System Layout of Quanta FEG System Layout of Quanta FEG The standard layout of the Quanta FEG 250 / 450 / 650 system is based around a dedicated microscope controller. The user interface devices are peripherals to the microscope controller, either software or hardware.
  • Page 15 System Overview: System Layout of Quanta FEG System Control Panel The console / system power is activated by pressing the front panel / green power button located on the microscope console. This switches the sub-systems on and allows the interface and communication with the microscope controller.
  • Page 16 System Overview: System Layout of Quanta FEG Final Lens Aperture Strip The strip is made from a Mo coated Si. Either manual (numbered click-stop mechanism positions) or Automatic Aperture System (AAS) motorized software-control (option - see Chapter 9) enables to choose the aperture most applicable to your imaging needs (see Chapter 5).

  • Page 17: Quanta Feg Options

    System Overview: Quanta FEG Options Quanta FEG Options A range of hardware and software is available as options for the system. Contact your FEI sales representative for more up-to-date information on system options. • The Support PC connects your work space to the network and can hold some other software utilities.
  • Page 18 System Overview: Quanta FEG Options • The small diameter, low voltage Back-Scatter Electron Detector (BSED) • The low-voltage, High-contrast Detector (vCD) • The Gaseous Analytical Detector (GAD) is the low voltage BSED with an additional X-ray cone with a 500 µm Pressure Limiting Aperture which seals to the objective pole piece.

  • Page 19: Chapter 3 System Operation

    SYSTEM OPERATION This chapter describes: • The Quanta FEG vacuum system – Vacuum status and relevant actions (Pump, Vent) – Vacuum modes and relevant actions (HiVac, LoVac, ESEM) • Quanta FEG System States – Start up procedure generally – Shut down procedure generally –...

  • Page 20: Quanta Feg Vacuum System

    System Operation: Quanta FEG Vacuum System Quanta FEG Vacuum System Within the system there are three main vacuum sections: • • Column • Specimen Chamber Both Column and Specimen Chamber sections are vented for a sample exchange. In operation the Gun and Column sections are always under the high vacuum.

  • Page 21: Vacuum Statuses

    System Operation: Vacuum Statuses Vacuum Statuses The vacuum status controls are in the Vacuum module. The Pump button starts pumping for the operating pressure and the Vent button starts venting for a sample or detector exchange. In the Status module at the bottom of any page the actual vacuum status is represented by the colored icon, which may have three possible colors with the following meaning: •...

  • Page 22: Vacuum Modes

    System Operation: Vacuum Modes Vacuum Modes The vacuum mode radio buttons in the Vacuum module / Mode area are used to select the instrument target operating mode when a Pump sequence is initiated. The vacuum system recognizes High Vacuum, Low Vacuum and ESEM modes. HIGH VACUUM (HiVac) MODE The high vacuum condition is common throughout the column and specimen chamber.
  • Page 23 System Operation: Vacuum Modes Clicking the OK button after selecting an appropriate pole piece radio button (cone or a detector with an integrated PLA) informs the system that it is mounted on the lens insert. The system starts pumping to the LoVac mode.
  • Page 24 System Operation: Vacuum Modes Purging During this procedure the specimen chamber is automatically pumped down to a lower pressure to remove the old gas, then it is flooded with the new one (selected in the Vacuum / Mode module) to a higher pressure.

  • Page 25: Quanta Feg System States

    Note: Once you have your FEI Microscope user (or Supervisor) account set up via FEI User management software by FEI Account Administrator (see Chapter 4), you can use your name and password to access both Windows xP system and the xT microscope Control software.
  • Page 26 All valves are closed, and the electron column and specimen chamber areas are vented. This should only be carried out by a FEI service engineer. Normally it is used for a system transportation or for service actions, like repair to essential systems (electrical and air supplies).

  • Page 27: Power Off

    System Operation: Quanta FEG System States POWER OFF Take sufficient measures to avoid power failures as much as possible. If it occurs while the instrument is completely operational, the microscope comes down to a safe state and the following happens: •...
  • Page 28 System Operation: Quanta FEG System States 3-10...

  • Page 29: Chapter 4 Software Control

    This chapter gives an overview of the xT microscope Control (referred to as UI or sometimes xTUI in dialogue boxes), xT microscope Server and FEI User Management software, and describes the functionality of each part of the user interface. It takes you from the first main window and menu bar through each item on the pull-down menus.

  • Page 30: Software Interface Elements

    Software Control: Software Interface Elements Software Interface Elements ICONS Icons are small symbols indicating a specific software application. Double-click the icon to activate the program. There are also functional icons in the toolbar for selecting some software functions quickly. Clicking causes it to press in and activate, clicking it again or clicking another one (depending on a particular case) causes it to spring out and deactivate.

  • Page 31: Command Buttons

    Software Control: Software Interface Elements COMMAND BUTTONS carry out or cancel functions. They press in when clicked and some change color to show the corresponding function activity. Command buttons have labels that describe the actions performed by clicking them. The most common ones, which are typically used in dialogues are: •...

  • Page 32: Adjusters

    Software Control: Software Interface Elements ADJUSTERS allow to change parameters, such as contrast, brightness, gamma etc. in a continuous way by pressing and dragging the middle adjuster or clicking in the grey bar. They always have a label in the upper left and right corners for readout information.

  • Page 33: 2D Controls

    Software Control: Software Interface Elements 2D CONTROLS are represented by an X-Y box. The position of the crosshair corresponds to the actual parameter value with respect to its full range being represented by the perimeter of the box. Pressing anywhere inside the box changes the active quad cursor to the four-ended arrow and positions it to the screen point corresponding to the actual control value (minimum in the middle of the screen and maximum at the edges).

  • Page 34: Xt Microscope Server Software

    Software Control: xT microscope Server Software xT microscope Server Software The xT microscope Server application starts and stops the software service controlling basic microscope functions and also the user interface (UI) software xT microscope Control. Run the xT microscope Server (from the Windows Start menu or double-click the icon) –...

  • Page 35: Xt Microscope Control Software

    Software Control: xT microscope Control Software xT microscope Control Software xT microscope Control – also called User Interface (xTUI or UI) – is made up of several elements which compose the main window, displaying status and control features. FIGURE 4-2 THE MAIN WINDOW 4 - Quad 1 4 - Quad 2 4 - Quad 3...

  • Page 36: The Title Bar

    Software Control: xT microscope Control Software THE TITLE BAR displays the application icon and name plus the standard Windows buttons: Minimize and Close, which are enabled. FIGURE 4-3 THE TITLE BAR The Close button quits the xT microscope Control software (accelerating and detectors voltages are switched off for the security reasons).
  • Page 37 Software Control: xT microscope Control Software FIGURE 4-5 SAVE AS… DIALOGUE The dialogue displays, by default, the location and the name last used to save / open a file in the actual quad. You can choose different location, name base or suffix, select different image format (Save as type), and also choose whether to Save the image with / without Databar and with / without overlaid graphics by ticking / clearing an appropriate check box.
  • Page 38 • An 3rd party video signal can be selected, which is indicated as “External” in the databar. Contact a FEI service person about a connection details. • The CCD camera reflects the inner space of the specimen chamber.
  • Page 39 Software Control: xT microscope Control Software The Scan Menu (Alt + C) opens the scanning control functions: Pause (F6) pauses the image. This function is used automatically with Snapshot and Photo functions. Select Pause or press F6 or click the Pause icon once / twice to stop scanning at the end of the actual frame / immediately.
  • Page 40 Software Control: xT microscope Control Software Full Frame (Ctrl + M) is the default scanning mode, typical for navigation and imaging. Spot (Ctrl + K) In this mode, the image pauses and the scanning is switched off. The actual beam position is represented by a green cross in all paused electron images.
  • Page 41 Software Control: xT microscope Control Software Note: When two above mentioned functions are active, it is represented in the toolbar scan speed spiner with the letters LI / SI. Live is the default imaging mode, leaving the image unfiltered for collecting raw direct images - one frame follows another.
  • Page 42 Software Control: xT microscope Control Software settings. Only one is active at any time, but can be operated independently for each quad. Degauss (F8) triggers the procedure which puts all actually used electron lenses to a normalized state by removing their hysteresis effects. For a few seconds while the procedure is running all live images disappear or turn fuzzy, and then return back.
  • Page 43 Software Control: xT microscope Control Software Auto Beam Shift Zero automatically resets the beam shift each time it reaches the maximal value during the Get function (the point-to-point stage movement) and corrects the image position with a stage movement. Home Stage (Shift + F3) starts procedure which moves all motorized axes to their hardware limits and ensures that the physical stage position agrees with the coordinates readout.
  • Page 44 Software Control: xT microscope Control Software Sample Navigation toggles on / off function that enables to navigate live electron images (scan field) towards desired places on a specimen using either paused or loaded image of that specimen (usually taken at much lower magnification).
  • Page 45 The Lab Notes can be used to open, edit and save any text file without the necessity to hide the xT UI. FEI Movie Creator… provides a dialogue over the quad 4 for setting up a collection of sequenced TIF images, and lining them up into an AVI movie (see Chapter 5).
  • Page 46 Software Control: xT microscope Control Software The Window Menu (Alt + W) opens the Window menu functions: Center Cross (Shift + F5) places a cross in the center of all electron image quads. This function is automatically used in Alignment procedures to aid the centering of features and can be used to align a sample against a stored image in another quad.
  • Page 47 Software Control: xT microscope Control Software Remote Display Mode When using the Remote Imaging (option) this feature enables correct UI imaging at the remote site. It is also used for a remote service. Use of this function decelerates slightly a UI performace and it is displayed in the bottom left quad corner.

  • Page 48: The Toolbar

    Software Control: xT microscope Control Software THE TOOLBAR displayed below the Menu bar is made up of functional icons linked to the most frequently used system controls. It also contains group of icons for quick switching between UI Pages. The toolbar can be a bit different in content or style (see the Preferences…...

  • Page 49: Image Windows

    Software Control: xT microscope Control Software IMAGE WINDOWS The xT microscope Control software images via 4 independent windows called quads. All quads can contain live imaging from any detector (including External and CCD), paused imaging or images loaded from a file. Additionally, quad 3 can display a mix of images from quads 1 and 2, and quad 4 can display a mix of images from quad 1, 2 and 3.

  • Page 50: Pages And Modules

    Software Control: xT microscope Control Software PAGES AND MODULES The software controls on the right side of the screen are organized into Pages, which are divided into Modules holding specific functions. The required page can be selected by pressing the corresponding icon button or with the use of short-cuts (see below).
  • Page 51 Software Control: xT microscope Control Software 2. The Column Module contains controls for setting the electron beam conditions: The Beam On Button switches the accelerating voltage on / off. When activated / deactivated, the button changes from gray to yellow / yellow to grey. The High Voltage Preset / Continuous Adjuster enables to adjust the overall electron beam acceleration voltage (from 200 V to 30 kV in 100 V steps) either continuously or using the pre-set...
  • Page 52 Software Control: xT microscope Control Software Note: Right-clicking over the 2D box opens the menu with following particular choices: • The Reset sets the Beam Shift value to zero and moves the stage to compensate the resulting image shift (same as the Stage menu / Beam Shift Reset function).
  • Page 53 Software Control: xT microscope Control Software 7. The Status Module can be found at the base of all pages, displaying following information (some of them as a tool tip): • The Chamber Pressure: shows the specimen chamber pressure. • The Gun Pressure: shows the electron source space pressure. •...
  • Page 54 Software Control: xT microscope Control Software 8. The Stage Module consists of the tabbed sections (see Chapter 7). • The Map tab displays the stage positions location in a visual map form and as a list for selection. • The Coordinates tab displays numerical values of a particular position.
  • Page 55 Software Control: xT microscope Control Software 9. Rotation Module controls and displays the Scan Rotation value (see Chapter 7). 10. Detector settings Module enables to choose the selected quad detector and adjust its parameters. The Detector list box contains list of detectors actually available for the selected quad (the same as enabled items in the Detectors menu).
  • Page 56 Software Control: xT microscope Control Software 13. The Enhanced Image Module consists of four tabbed sections offering various digital image enhancements. In contrary to Detector module / Contrast and Brightness functions, these enhancements are applied only to the active quad independently. In case the user changes the default settings of LUT / Color / Process tab, its background color changes to green.

  • Page 57: Preferences

    Software Control: xT microscope Control Software PREFERENCES… DIALOGUE This dialogue can be opened by selecting Preferences… (Ctrl + O) from the pull-down menus: Scan and Tools. The opened menu from which it is chosen dictates the tab opened on entry. Once the Preferences dialogue is opened, any of the tabs can be chosen.
  • Page 58 Software Control: xT microscope Control Software The Databar Tab specifies content of the databar displayed at the base of all quads. The Databar configuration and available items differ according to the beam. Actual content of the Databar Preferences dialogue corresponds to the actually active quad. For all electron imaging quads the Databar configuration is identical, except of the Label which can be set independently for each quad.
  • Page 59 Software Control: xT microscope Control Software The Scanning Tab allows the user to change the dwell-times (scanning speeds) table and to set-up the Slow scan / Fast scan / Snapshot / Photo function. FIGURE 4-17 SCANNING PREFERENCES On the left side of the module there is a dwell-time preset list with the fixed number of entries.
  • Page 60 Software Control: xT microscope Control Software Slow (tortoise / large green sector) / Fast (hare / small green sector) preset icon indicates the matching dwell-time value. To change it move an icon up or down just by pressing it. Snapshot (F4) / Photo (F2) (different cameras) preset icon indicates the matching dwell-time value.
  • Page 61 Software Control: xT microscope Control Software The ESEM Tab enables to customize the specimen chamber purging, which is automatically initiated when the system pumps the vented chamber directly to the ESEM / Low Vacuum mode. FIGURE 4-19 ESEM PREFERENCES Purge Mode module radio buttons: •...
  • Page 62 Software Control: xT microscope Control Software The General Tab contains variety of user settings of both UI behaviour and microscope operation, which are of less importance and/or does not logically belong to other Preferences section. FIGURE 4-20 GENERAL PREFERENCES Each item of the General Preferences is represented by single line displayed in the property editor.
  • Page 63 Software Control: xT microscope Control Software • Spot Size Step (0.1 / 0.01 / 0.001) This enables to set the accuracy of the spot size setting. • Enhanced Contrast slider besides Contrast (Yes / No) enables to show the Enhanced contrast control next to the Contrast in the Detector module.
  • Page 64 Software Control: xT microscope Control Software • Switch off CCD automatically (No / 1 minute / 10 minutes / 30 minutes / 1 hour / 2 hours / 6 hours) Specifies if and when the CCD camera and infrared LEDs should be automatically switched off.
  • Page 65 Software Control: xT microscope Control Software Magnification Tab controls the imaging and stored / printed image databar magnification display. The constant imaging pixel size is set at the toolbar. When storing / printing an image (while in a Single or Quad imaging mode) the databar magnification display may not be correct.

  • Page 66: Fei User Management Software

    (set user group). FEI ACCOUNT ADMINISTRATORS As the highest account level, FEI Account Administrators have rights that allow them to create and delete users and change their properties over the following user groups (in order of significance): •...
  • Page 67 Remove (Del): click to remove an existing user. The user must be highlighted first. If an FEI Microscope User has user data, the account administrator is warned that user data will be removed also. If any additional user is to be removed, that additional user’s data is removed without warnings.

  • Page 68: Account Logging

    • Legend: clicking provides an explanation of icons used in the tree. • About: displays the FEI User Management software version and copyright. ACCOUNT LOGGING This accounting utility monitors user, log on / off actions, session time, filament lifetime and the UI status.

  • Page 69: Entering Commands In Summary

    Software Control: Entering Commands in Summary Entering Commands in Summary USING THE MOUSE TABLE 4-3 MOUSE BUTTON FUNCTIONS Key + Button Function Click Control Areas: makes selection in control areas (single arrow cursor). On Screen: press and drag a selected area to zoom in magnification to fill the imaging area with the selection (selectable in Preferences).

  • Page 70: Using The Keyboard

    Software Control: Entering Commands in Summary USING THE KEYBOARD TABLE 4-4 WINDOWS SYSTEM KEYS Key (+ Key) Function Enter Equivalent to OK in a dialogue box. 1. Equivalent to the Cancel button. 2. Cancels the click and drag function. 3. Stops the stage motion at that point. Note: During some procedures (Home Stage for instance) use the software Cancel or Stop button!
  • Page 71 Software Control: Entering Commands in Summary TABLE 4-5 FUNCTION AND SPECIFIC KEY SHORT-CUTS Key (+ Key) Function Displays On-Line Documentation Shift + F1 Opens Image Properties dialogue (Shift +) F2 Starts Photo (from all quads at once) Ctrl + (Shift +) F2 Starts / Stops Active Preset Snapshot (from all quads at once) Toggles Videoscope On / Off Shift + F3...
  • Page 72 Software Control: Entering Commands in Summary TABLE 4-5 FUNCTION AND SPECIFIC KEY SHORT-CUTS Key (+ Key) Function Ctrl + (Shift +) , Set one step slower (slow) scanning Ctrl + (Shift +) . Set one step faster (fast) scanning Ctrl + (Shift+) Tab (Backward) steps between quads Ctrl + Page Up / Down Left / Right steps between pages...

  • Page 73: Chapter 5 Operating Procedures

    OPERATING PROCEDURES This chapter describes how to use the Microscope system from an application point of view. The following subjects are covered: • Specimen Preparation and Handling • Obtaining an Image • Optimising an Image • Detector types and usage •...

  • Page 74: Specimen Preparation And Handling

    Operating Procedures: Specimen Preparation and Handling Specimen Preparation and Handling The specimen material for High Vacuum mode must be able to withstand a low pressure environment (without outgassing) and the bombardment by electrons. It must be clean and conductive. Oil and dust may contaminate the chamber environment, which could hinder or even prevent evacuation to the level needed for standard SEM operation.

  • Page 75: Mounting The Specimen To The Holder

    Store samples and sample holders in a dry and dust free environment. Dust on samples can get drawn into the electron column, degrading imaging and requiring an FEI Customer Service. INSERTING / EXCHANGING A SPECIMEN AND / OR A DETECTOR It is assumed, that the microscope is in the Full operation state (see Chapter 3).

  • Page 76: Obtaining An Image

    Operating Procedures: Obtaining an Image Obtaining an Image OPERATION PRE-CHECK To ensure correct operation in any Vacuum mode, check the following list before continuing. After obtaining a preliminary image, you can then experiment with your settings. It is also possible to use Set Default Parameters (Ctrl + D) function found at the Tools menu.

  • Page 77: Selecting Vacuum Mode

    Operating Procedures: Obtaining an Image SELECTING VACUUM MODE When a specimen and appropriate detector(s) are inserted correctly, close the specimen chamber door and continue the procedure (see above): 6. In Vacuum module, select the High Vacuum / Low Vacuum / ESEM radio button.

  • Page 78: Spot Size

    Operating Procedures: Obtaining an Image SPOT SIZE The electron beam diameter (usually represented as the Spot size) is considered to be close to ideal when its edges just touch the neighbouring spot. If it is too large, overlaps occur and the image appears out of focus.

  • Page 79: Obtaining An Image On Screen

    Operating Procedures: Optimising an Image OBTAINING AN IMAGE ON SCREEN The following assumes that the electron emission is on. Continue the procedure (see above): 10.Select an appropriate detector (see below) and release the active quad. 11.Click the Column module / Beam On button to ramp up the accelerating voltage.

  • Page 80: Scan Speed And Filtering

    Operating Procedures: Optimising an Image Alternatively Magnification could be expressed as the Horizontal Field Width (HFW), specifying dimension of the scanned area (see the Preferences… / General tab). The Quanta FEG supports two viewing sizes: Quad Image and Single Image modes. Magnification is always adjusted in the databar for the actual display, thus an image at 500×...

  • Page 81: Contrast And Brightness

    Operating Procedures: Optimising an Image CONTRAST AND BRIGHTNESS The contrast and brightness can be set manually either by adjusting the Detectors module controls (see Chapter 4) or using the MUI (option). Follow the procedure: 1. Select a medium speed scan in an active quad. 2.

  • Page 82: Focusing

    Operating Procedures: Optimising an Image FOCUSING Find a feature of interest with distinct edges on a specimen. Use a combination of contrast, brightness and magnification adjustments to maximize the image quality. To avoid scanning too long and contaminating or even damaging the sample, move away from a feature of interest with the stage, and focus until the image is sharp on an adjacent area.

  • Page 83: Pressure And Working Distance (Wd)

    Operating Procedures: Optimising an Image the cursor around the screen to achieve maximum sharpness. When you are satisfied, release the mouse button. 3. The MUI (optional): adjust image sharpness with the stigmator X and Y knobs until the best image is achieved. The computer beeps when the stigmator limits are reached.

  • Page 84: Digital Imaging Enhancement / Imaging Mixing / Coloring

    Operating Procedures: Optimising an Image DIGITAL IMAGING ENHANCEMENT / IMAGING MIXING / COLORING The Enhanced Image module offers various digital image enhancements. Note: When saving the image with the digital enhancements applied, be sure to choose the correct file format (see below). The LUT (Look-Up-Table) Tab enables to monitor and modify a grey level distribution (histogram).
  • Page 85 Operating Procedures: Optimising an Image new color spectrum before it is mixed with other image(s). Note: Color images (see below – the Color tab) are converted to greyscale ones before mixing. • The Invert check boxes inverts the corresponding source image spectrum.

  • Page 86: Detector Types And Usage

    Operating Procedures: Detector Types and Usage Detector Types and Usage The Detectors menu shows all detectors, a selected one has a tick mark next to its label. Availability of detectors (full color label) depends on the actual vacuum mode. The system remembers the last detector used for a particular vacuum mode and its Contrast &...

  • Page 87: Detector Connection

    Operating Procedures: Detector Types and Usage DETECTOR CONNECTION Detectors are connected to the feed-through connector panel. Connectors have engraved names and they are used to connect following detectors: • The STEM connector: STEM I (Scanning Transmitted Electron Microscopy, Wet STEM), STEM II (Annular STEM) •...
  • Page 88 Operating Procedures: Detector Types and Usage Either diode has an active area of approximately 125 mm per segment and is positioned directly above the sample to obtain maximum detector efficiency. Therefore it causes some limitation in the tilt range. Both detectors are connected to an SSD pre-amplifier input board. They can be used down to a high voltage about 1 kV and works best at a slow scan conditions.

  • Page 89: Large Field Detector (Lfd)

    Operating Procedures: Detector Types and Usage Obtaining Image in BSE Mode 1. Install one of the diodes and select the corresponding Detector. 2. Close the chamber door and pump down the chamber. When the BSED / GAD diode is installed, No Accessory / GAD cone must be selected in the PLA Configuration dialogue when this appears.

  • Page 90: Gaseous Secondary Electron Detector (Gsed)

    Operating Procedures: Detector Types and Usage GASEOUS SECONDARY ELECTRON DETECTOR (GSED) The GSED is integrated into a flexible printed circuit board and plugs into the signal connector behind the conical lens. It is used for general wet imaging and for high pressure imaging with auxiliary gases. FIGURE 5-6 GSED AND ITS CONFIGURATION The overall image consists of a very pure SE signal with very little BSE signal component, due to the detector design and chamber...

  • Page 91: Pla Cones

    Operating Procedures: Detector Types and Usage Removing the GSED CAUTION! DO NOT change the order of the following procedure! Otherwise you can damage the detector. 1. Remove the detector head from the lens insert first. Do this by catching a fingernail or thumbnail (of the gloved hand) on the FRONT of the yellow Torlon ring and pull down (there is a shoulder machined into the Torlon ring which is specifically designed for this purpose).

  • Page 92: Discharges Between The Gaseous Detectors And The Sample

    Operating Procedures: Detector Types and Usage DISCHARGES BETWEEN THE GASEOUS DETECTORS AND THE SAMPLE Excessive voltage may cause a “breakdown” between the detector and the sample, chamber, pole-piece etc. This could damage the sample (at ground) but does not damage the detector. This condition is indicated by white flashes or streaks across the image, and on some systems a large discharge could make the system unstable or cause the chamber to vent and switch off the HV.

  • Page 93: Capturing And Handling Single Image

    Operating Procedures: Capturing and Handling Single Image Capturing and Handling Single Image After obtaining a good image quality, the image could be paused and saved. It is possible to save an image using the File menu or using the Scandium database software (option) image saving function. Setup the file name label and harddrive destination for the image to be saved using the next available label / number prior to the capture session.

  • Page 94: Saving / Opening / Printing

    Operating Procedures: Capturing and Handling Single Image there is no reason to save an image with a higher bit and color depth than available in an original one. Over against saving an image with a lower bit and color depth than available leads to the loss of information.

  • Page 95: Recording Movies (Saving Multiple Images)

    Operating Procedures: Recording Movies (Saving Multiple Images) Recording Movies (Saving Multiple Images) This function captures dynamic experiments performed with the microscope and creates the digital video files (AVI). Up to 4 imaging quads (not the optical one) can be recorded simultaneously with a synchronized start.
  • Page 96 Operating Procedures: Recording Movies (Saving Multiple Images) Timer module The parameters in this section can be changed when the digital video is inactive, but are disabled during recording. The digital video is recorded asynchronously with the scanning. • The Movie check box – AVI (Digital Video) timer: After the Delay time, the image of each resumed quad is stored immediately (even in the middle of the frame) as a new frame in the video stream.

  • Page 97: Movie Procedure

    Operating Procedures: Recording Movies (Saving Multiple Images) MOVIE PROCEDURE The red dot button starts the recording of all live electron image quads at the same moment – no video / images are stored for paused quads. When a quad is paused during the video recording, the storing of the video frames is interrupted but the video streams keep synchronization for the next resuming.

  • Page 98: Fei Movie Creator

    Operating Procedures: Recording Movies (Saving Multiple Images) FEI MOVIE CREATOR This is a separate program that creates a movie from a sequence of TIF images. Click the Tools menu / FEI Movie Creator… to activate the tabbed dialogues. The following items are common for all tabs: •...
  • Page 99 Note: The Databar Preview does not show any item until you enter the File tab / Name Prefix field. FIGURE 5-11 FEI MOVIE CREATOR TAB: DATABAR • The Available / Displayed items: lists – all items that can be entered in the databar / are already present in the databar.

  • Page 100: Playing A Movie

    Once the movie is set-up, opening the Preview tab automatically displays the first image of the movie sequence. FIGURE 5-12 FEI MOVIE CREATOR TAB: PREVIEW • The Start / Pause / Stop button starts / pauses / stops the movie play back.

  • Page 101: Measurement And Annotation Functions

    Operating Procedures: Measurement and Annotation Functions Measurement and Annotation Functions The Processing page / Measurement / Annotation functions give the user many capabilities to measure distances, angles, diameters and areas as well as locating and labelling items that are of significant interest on the sample area.
  • Page 102 Operating Procedures: Measurement and Annotation Functions Shape Editing Once a Measurement or Annotation symbol has been drawn, it can be modified. Selected graphic is denoted by the addition of resizing handles to the graphic outline (use pointer cursor). Size and position the graphic correctly over the area of interest. A number of other choices are available in the Property editor for each graphics drawn.

  • Page 103: Chapter 6 Alignments

    ALIGNMENTS List of alignments accessible for a supervisor: • Final Lens Aperture Strip Alignment • 1 - Gun Alignment • 2 - Stigmator Alignment • 3 - Stage Rotation Center • 5 - Emitter Startup • 94 - CCD Camera Alignment •...

  • Page 104: Quanta Feg System Alignments

    Alignments: Quanta FEG System Alignments Quanta FEG System Alignments At the Alignments page select an alignment procedure available from the list box. Always follow the instructions given in the Instructions module. You can find some additional explanation in this chapter. COMMON RULES Alignments should be performed in the quad 1.

  • Page 105: Buttons And Control Elements

    Alignments: Quanta FEG System Alignments BUTTONS AND CONTROL ELEMENTS The following particular buttons and control elements have the same behaviours for all alignment procedures, when available: • The Start button starts the procedure and proceeds with following dialogues. • The End button moves the user to the last step (by clicking the Next button) to be able to finish the alignment procedure.

  • Page 106: Final Lens Aperture Strip Alignment

    Alignments: Final Lens Aperture Strip Alignment Final Lens Aperture Strip Alignment This mechanical alignment eliminates an image shift when focusing. The position of the final aperture should remain constant and should not be changed further during the alignment procedure. When the aperture is well aligned, the image does not rotate (at low magnification) or move (at high magnification) during focusing.

  • Page 107: Gun Alignment

    Alignments: 1 - Gun Alignment 1 - Gun Alignment After finishing the procedure there should be no image shift, no out of focus and no brightness change during microscope operation.
  • Page 108 Alignments: 1 - Gun Alignment...

  • Page 109: Stigmator Alignment

    Alignments: 2 - Stigmator Alignment 2 - Stigmator Alignment Particular Control Elements • The Modulator button starts automatic stigmator oscillation to facilitate the process. • The Clear Memory button resets the stigmator settings.

  • Page 110: Stage Rotation Centre

    Alignments: 3 - Stage Rotation Centre 3 - Stage Rotation Centre The stage rotation has a mechanical center and it can be controlled by changing the Stage module / Coordinates tab / R value. This moves the stage around its mechanical center. In some circumstances this is not desired because a rotation around the field of view center would be more useful.

  • Page 111: Emitter Startup

    Alignments: 5 - Emitter Startup 5 - Emitter Startup This procedure enables electron source switching On / Off. In cases of emergency shut down or the microscope mains switch off the Ion Getter Pumps (IGP) keep pumping the FEG source area backed up by the Battery Supply Unit (BSU).
  • Page 112 Alignments: 5 - Emitter Startup 1. Check the Gun vacuum page: if it is IGP ON click the Next button. If it is OFF click the IGP On button to automatically start the ion pump. This procedure takes a few minutes. If the ion pump start is not successful, call service.

  • Page 113: 94 - Ccd Camera Alignment

    Alignments: 94 - CCD Camera Alignment 94 - CCD Camera Alignment This procedure optimizes the CCD camera imaging performance. 6-11...

  • Page 114: 154 - Water Bottle Venting

    Alignments: 154 - Water Bottle Venting 154 - Water Bottle Venting 6-12...

  • Page 115: Chapter 7 Stages

    Control software. The scopes covered in this Chapter are the following: • Stages types and accessories: Quanta FEG 250, 50 mm 4 axes motorised Quanta FEG 450, 100 mm 5 axes motorised Quanta FEG 650, 150 mm 5 axes motorised •...

  • Page 116: Stages Types And Accessories

    Quanta FEG 250 Standard Sample holder The single stub holder and the multiple holder are provided with the Quanta FEG 250. The single holder has a spring clip fitting and a secure-fitting screw. The multiple holder is a 7-stub holding disc with a spring clip fitting only.

  • Page 117: Quanta Feg 450 / 650 - 100 / 150 Mm Stage

    Stages: Stages Types and Accessories QUANTA FEG 450 / 650 – 100 / 150 mm STAGE The stage has the X, Y, Z, Rotation and Tilt movements motorised, all with a manual override. All movements are read out on the screen, under the software control.

  • Page 118: Eucentric Position

    Stages: Stages Types and Accessories EUCENTRIC POSITION This should be adjusted after loading any new sample (other than wafer) or for the greatest accuracy, as the sample loading procedure clears all position informations. At the eucentric position, one can use various system components (such as the EDX) in a safe and optimal way.
  • Page 119 Stages: Stages Types and Accessories Sample Top Surface Positioning The distance between the observed sample and the stage rotation head surfaces must be properly set to bring the stage to the eucentric position. This procedure also prevents the specimen to touch the lens pole when moving the stage in the Z-axis direction.

  • Page 120: Stage Movement Limits

    Stages: Stages Types and Accessories STAGE MOVEMENT LIMITS The motorised movements of the stage can be operated under software control for more advanced location mapping. This includes Shift, Get, Track and the Stage module functionality. A live image can be repositioned either by the stage movement (manual or software) or by the Beam Shift.

  • Page 121: Software Stage Functions

    Stages: Software Stage Functions Software Stage Functions The Navigation page / Stage module controls the stage movements that locate the position of the specimen by reference to coordinate points. It consists of Map / Coordinates / Tilt / Navigation tabs. MAP TAB In the map area the stage schema is represented displaying all stored locatable positions, which are listed in the Location list box for...
  • Page 122 Stages: Software Stage Functions Radar view The small circle in the stage schema top right corner conveys the stage rotation at any time by the black triangle and perpendicular lines position. To rotate the stage, press over the circle perimeter triangle, move it round and release the mouse button at the desired position –...

  • Page 123: Coordinates Tab

    Stages: Software Stage Functions • Clicking the Remove selected position item deletes the selected location(s) from the map and from the Location list. The Coordinates tab / Remove button has the same functionality. • Clicking the Magnification item provides menu allowing the Map area magnification factor (5) to be selected.

  • Page 124: Tilt Tab

    Stages: Software Stage Functions When the Compucentric Rotation check box is ticked, the R coordinates operates as the Compucentric Rotation function. Note: The R coordinate is permanently locked and its homing is disabled when the heating or cooling stage is plugged in. TILT TAB When the appropriate check box is ticked, the function becomes active.

  • Page 125: Stage Related Functions

    Stages: Stage Related Functions Stage Related Functions STAGE MOVEMENTS Track This function allows continuous directional stage movements at a variable speed. Press and hold the mouse wheel over an active electron image window – the yellow dot appears onscreen at the mouse cursor point. Move the mouse to the direction intended for an observation –...
  • Page 126 Stages: Stage Related Functions This function brings an image point of interest to the screen center. Double-click over an image point. The object is mechanically centred onscreen by moving the stage, which is suitable for lower magnifications. When working at higher magnifications, beam shift could be also employed (see the Preferences…...
  • Page 127 Stages: Stage Related Functions Compucentric Rotation (F12) Clicking the Stage menu / Compucentric Rotation places a green circle in the image window. The green triangle on its perimeter denotes, by its position, the sample rotation relative to its original position when mounted on the stage. Initially, this is in the 12 o’clock position.

  • Page 128: Specimen Alignment

    Stages: Stage Related Functions SPECIMEN ALIGNMENT xT Align Feature This utility is designed specifically for long features, extending off the screen at the magnification required for an observation. It applies the mapping process bringing the long feature either to the horizontal or vertical axis to make the navigation easier.
  • Page 129 Stages: Stage Related Functions 4. Drag any point to change its position, if needed. Click the Finish button to orientate the feature either Horizontal or Vertical, as selected previously. Click the Cancel button any time to cancel the function. User Units Clicking the Stage menu / User Units activates user defined units as the basis of the stage coordination system.
  • Page 130 Stages: Stage Related Functions 1. Select a sample surface feature and view it at an appropriate magnification to check its relation to other structures. 2. Click the Stage menu / Define User Units… A Start dialogue appears. Click the Define New User Units radio button. Redefine User Units –...
  • Page 131 Stages: Stage Related Functions 6. Check the Details if needed or Finish the procedure. Using 1-, 2- or 3- Point Alignments TABLE 7-4 ALIGNMENT TYPE DIFFERENCES 1-Point Alignment 2-Point Alignment 3-Point Alignment Major Use Aligning to new point Aligning the stage axes with Transforming to nonstandard directly offset from the specimen X-Y orientation...

  • Page 132: Scan Rotation (Shift + F12)

    Stages: Stage Related Functions SCAN ROTATION (SHIFT + F12) This function activates the onscreen tool to rotate the scan and align the image. Because it is solely a scan coil function, it has no effect on the stage movements. It is used to orient the image relative to mechanical rotation and detector direction.

  • Page 133: Chapter 8 Maintenance And Troubleshooting

    MAINTENANCE AND TROUBLESHOOTING This section describes necessary microscope maintenance procedures that can be carried out by the FEI Supervisor User / FEI Microscope User. The user maintenance is at a minimum due to gun and column design providing the long uptime. Therefore a complicated maintenance is normally a part of a service contract to be performed by a qualified service engineer.

  • Page 134: Cleaning Procedures Overview

    Maintenance and Troubleshooting: Cleaning Procedures Overview Cleaning Procedures Overview Frequency of cleaning is, in most cases, determined by necessity due to poor image quality or gross astigmatism level. Recommended cleaning procedures are given below for parts which operate in vacuum and which are subject to possible contamination. LIST OF APPLIED CLEANERS •...

  • Page 135: Materials And Technique

    Maintenance and Troubleshooting: Cleaning Procedures Overview C a u t i o n ! Gold plated parts should not be polished with abrasive. MATERIALS AND TECHNIQUE To polish components, place a lint-free cloth on a flat surface (a glass block is ideal) and apply a small amount of Soft Scrub or CIF and distilled water to the cloth.

  • Page 136: The Standard Insert

    Maintenance and Troubleshooting: The Standard Insert The Standard Insert The following tools and procedures are used to install and remove the standard insert from the lens pole and to assemble Pressure Limiting Apertures and the Insert body. REMOVING AND DISASSEMBLING The following instructions describe how to remove and disassemble the standard insert assembly.

  • Page 137: Housing Cleaning

    Maintenance and Troubleshooting: The Standard Insert FIGURE 8-3 REMOVING AND DISASSEMBLING THE INSERT Aperture Positioning Tool Housing Final Aperture + c-clip 3. Inspect the o-ring at the bottom of the insert. If the o-ring looks deformed or damaged, replace it. This is a critical seal between EC1 and EC2 (which is under very low pressure).

  • Page 138: Platinum Apertures Installing

    Maintenance and Troubleshooting: The Standard Insert Polishing scratches the soft material and makes the aperture unusable for high resolution. All apertures must be cleaned and must not have scratches at the center hole. The top aperture should not have any scratches or defects. PLATINUM APERTURES INSTALLING 1.

  • Page 139: Aperture Strip Module

    Maintenance and Troubleshooting: Aperture Strip Module • Installing the c-clip into the insert is done using both the aperture tool and the injector/plunger tool. Use tweezers to insert the c-clip into the injector tool, then use the injector tool to install the c-clip into the aperture insert.

  • Page 140: Replacing The Aperture Module

    Maintenance and Troubleshooting: Aperture Strip Module REPLACING THE APERTURE MODULE The new Aperture Module comes in a container, has been cleaned and is ready to be fitted to the rod. 1. Unscrew the Titanium screw holding the old module onto the rod. Keep the screw in the hole of the rod and let the module fall away.

  • Page 141: Gaseous Detectors

    Maintenance and Troubleshooting: Gaseous Detectors Gaseous Detectors CLEANING THE GSED / LFD FIGURE 8-6 REMOVING THE GSED ASSEMBLY 1. Vent the chamber. 2. Pull the end of the GSED detector head down to remove it from the standard insert. The insert will remain inside of the pole-piece. 3.

  • Page 142: Stage Maintenance

    Maintenance and Troubleshooting: Stage maintenance Stage maintenance STAGE MECHANICS Checking the condition of the stage should be a weekly exercise as many different samples may be exchanged in this time period. Some samples may be powders or composite materials that inadvertently drop particles on or in the stage.

  • Page 143: Refilling The Water Bottle

    Maintenance and Troubleshooting: Refilling the Water Bottle Refilling the Water Bottle The water bottle in the instrument typically needs to be filled about once a month if the instrument is used on a regular basis at a high pressure. The water reservoir is located in the rear of the column console, beneath the frame.

  • Page 144: Pre-Vacuum Pump Maintenance

    Maintenance and Troubleshooting: Pre-Vacuum Pump Maintenance Pre-Vacuum Pump Maintenance The Rotary pump supplied with the system is used to directly pump parts of the vacuum system (such as the specimen chamber after a sample exchange) and for backing the main pumping system – Turbo Mechanical Pump (TMP).

  • Page 145: Troubleshooting

    Maintenance and Troubleshooting: Troubleshooting Troubleshooting TABLE 8-2 POSSIBLE PROBLEMS AND CORRECTIVE ACTIONS Problem Possible solution Not possible to switch the microscope • Check the mains switch and the mains unit circuit or the PC on breakers placed at the microscope back. •...
  • Page 146 Maintenance and Troubleshooting: Troubleshooting TABLE 8-2 POSSIBLE PROBLEMS AND CORRECTIVE ACTIONS Poor ETD image • Select the ETD. Open the Detectors menu / Detector Settings. Select the Mode: Custom. Change the Grid Voltage from maximum to minimum (see Chapter 5). •...

  • Page 147: Diagnostics Auto Report

    To run this procedure the xT Microscope Server can be stopped or running. 1. Run the system Start / Programs / FEI Company / User Tools / Diagnostics Auto Report. Click the Start button. 2. Write down how to reproduce the problem and choose a problem class (when prompted by the tool).

  • Page 148: Simple Tad

    Maintenance and Troubleshooting: Troubleshooting SIMPLE TAD If the xT Microscope Server is running, the Simple TAD automatically performs all the tests (communication, optics, supplies etc.). If it is exited, only the communication tests proceed. 1. Run the file located in C:\TAD\Simpletad_collector.exe. Click the Start button.

  • Page 149: Chapter 9 System Options

    X-ray Analysis for Different Vacuum Modes • Temperature Stages • CryoCleanerEC • Plasma Cleaner • Quanta Morphologi • Remote Imaging • Beam Deceleration • Specimen Holder Kit option • Quick Loader For further information on any of these items please contact your local FEI representative.

  • Page 150: Manual User Interface

    System Options: Manual User Interface Manual User Interface The Manual User Interface (MUI) provides knobs to perform functions that can also be performed with the software. It is connected to the USB connector located on the microscope controller. FIGURE 9-1 MUI The MUI offers additional flexibility for controlling magnification, beam shift, focus, astigmatism, contrast and brightness.

  • Page 151: Automatic Aperture System

    System Options: Automatic Aperture System Automatic Aperture System The Automatic aperture system (AAS) option enables a motorized final lens strip aperture exchange. Aperture The Beam menu / Aperture selection list (see Chapter 2 and 5) enables to choose the Final Lens Aperture. Home Apertures This feature moves the Final Lens Aperture aperture mechanism to its home position.
  • Page 152 System Options: Automatic Aperture System...

  • Page 153: Nav-Cam

    System Options: Nav-Cam Nav-Cam On contrary to Navigation Montage feature, which navigates across the sample surface, this functionality represents a possibility to navigate across the range of the stage movement area. This is convenient when investigating large area samples or several samples with the use of any multi sample holder.

  • Page 154: 401 - Nav-Cam Autobrightness

    System Options: Nav-Cam 401 - NAV-CAM AUTOBRIGHTNESS...

  • Page 155: Optional Detectors

    System Options: Optional Detectors Optional Detectors GASEOUS BACK SCATTERED ELECTRON DETECTOR (GBSD) The GBSD is used in place of the standard Gaseous SE (GSED) detector and Large Field Detector (LFD). It was specifically designed to image at pressures above 4 Torr (534 Pa) (predominantly in the range of 6 to 9 Torr (800 to 1200 Pa)).

  • Page 156: In Column Detector (Icd)

    System Options: Optional Detectors BSE converter plate. A zero voltage potential is applied to the SE collection grid. When the electrons strike a gas molecule with enough energy, they ionize it. The two electrons are further accelerated, causing more collisions. The SE signal is “amplified” in the gas with gains up to a few thousand resulting in BSE image.

  • Page 157: Scanning Transmission Electrons Microscopy Detector (Stem I)

    System Options: Optional Detectors SCANNING TRANSMISSION ELECTRONS MICROSCOPY DETECTOR (STEM I) The STEM I is a two segment solid-state diode mounted underneath the STEM I holder. It can be used at any available working distance (preferably close to the lens for high resolution) or at the eucentric position for simultaneous use of the EDX.
  • Page 158 System Options: Optional Detectors Loading samples Materials or hard samples should be prepared as for the TEM by appropriate thinning technique. The STEM I holder (which is a part of the detector assembly) can either be loaded with samples while outside the microscope chamber (which is more convenient) or when it is mounted and fixed to the stage.

  • Page 159: Annular Scanning Transmission Electrons Microscopy

    System Options: Optional Detectors ANNULAR SCANNING TRANSMISSION ELECTRONS MICROSCOPY DETECTOR (STEM II) This is a 14 segments solid-state diode mounted on a retractable arm. It must be used only with a special sample holder, oriented in an exact position monitored by a software (see below). It works best at a slow scan conditions.
  • Page 160 System Options: Optional Detectors Load In Row Holder 1. Place the row holder to the load base (the load base pin is beneath the position you want to load in / out). Tighten it by the screw knob, the pin lifts up the spring. If the pin does not lift up the spring enough to put the sample in, adjust the lifting height by turning the screw.

  • Page 161: Detector (Stem Ii)

    System Options: Optional Detectors Settings for STEM II Detector 1. Position the desired sample grid in the field of view using the ETD. Focus and link Z coordinate to FWD. 2. Select the Detector Settings module / Detector list box / STEM II detector.

  • Page 162: Low-Voltage High-Contrast Detector Lens Mounted / Retractable (Vcd)

    System Options: Optional Detectors LOW-VOLTAGE HIGH-CONTRAST DETECTOR LENS MOUNTED / RETRACTABLE (vCD) This is a solid State detector ideal for low accelerating voltages down to about 200 V. The diode has an active area of approximately 100 mm and it is positioned directly above the sample (optimum WD should be from 3.5 to 7 mm) to achieve maximum detection efficiency.

  • Page 163: Directional Backscattered Detector - Concentric Backscattered Detector (Cbs)

    System Options: Optional Detectors DIRECTIONAL BACKSCATTERED DETECTOR – CONCENTRIC BACKSCATTERED DETECTOR (CBS) The CBS uses concentric segmentation of the detector diode to distinguish between BS electrons scattered close to the beam axis – inner segment (preferentially compositional contrast) and electrons scattered far from the beam axis –...

  • Page 164: Esem & Gaseous Analytical Detector

    System Options: Optional Detectors ESEM & GASEOUS ANALYTICAL DETECTOR This detector has both GAD and GSED functionality. The GAD diode is combined with the needle shaped gaseous SE detector, which could be used at pressures above 200 Pa. FIGURE 9-10 ESEM & GAD DETECTOR QUAD BACKSCATTERED ELECTRONS DETECTOR (QUAD BSED) These are four-segment low voltage silicon diode.

  • Page 165: Photo Multiplier Tube / Backscattered Electron Detector Autrata, Centaurus (Pmt-Bse)

    System Options: Optional Detectors The Quad BSED is mounted close to the (optional) X-ray detector collimator, which must not be touched when changing detectors. It is advisable to retract the EDX collimator when mounting / removing the detector on / from the objective pole piece. Detector Settings Select the Quad BSED from the Detector Settings module / Detector list box.

  • Page 166: Energy Dispersive X-Ray (Edx) Analysis

    System Options: Energy Dispersive X-ray (EDX) Analysis Energy Dispersive X-ray (EDX) Analysis The EDX (sometimes referred to also as EDS analysis) is a technique used for identifying the elemental composition of the specimen, or an area of interest thereof. It works as an integrated feature of a scanning electron microscope (SEM), and cannot operate on its own without the latter.

  • Page 167: Lfd Edx Analysis

    System Options: Energy Dispersive X-ray (EDX) Analysis LFD EDX ANALYSIS EDX analysis should be performed at the lowest possible gas pressure, so it should be done with the LFD. Normally, X-ray analysis is performed with a relatively high beam current so that there is enough signal for a good LFD image even at very low gas pressure.

  • Page 168: Gad Edx Analysis

    System Options: Energy Dispersive X-ray (EDX) Analysis GAD EDX ANALYSIS Maximum detector response is around the 8.5 mm WD, providing an atomic number contrast, when the resolving power is better than 0.1 (in the Atomic number range around 20). FIGURE 9-17 X-RAY GAD CONFIGURATION IN ESEM MODE STEM EDX ANALYSIS Set the sample surface to 10 mm WD.

  • Page 169: Cooling Stage / Waterless Cooling Stage

    ± 20 °C around the ambient, uppermost from - 25 °C to +55 °C and to observe it with the use of FEI electron microscope. In conjunction with a specimen chamber water vapour pressure it can be used to create a water condensation on the sample surface to keep it wet.
  • Page 170 System Options: Cooling Stage / Waterless Cooling Stage FIGURE 9-19 COOLING STAGE ASSEMBLY • The mounting adapter enables to attach the Cooling stage to the microscope stage. • The Cooling stage base holds the thermoelectric module and the specimen holder with the use of a thermal grease. Water hoses and the inner cable are connected permanently to the base.
  • Page 171 System Options: Cooling Stage / Waterless Cooling Stage FIGURE 9-20 COOLING STAGE ASSEMBLY MOUNTING ADAPTER WITH MOUNTING SCREW The Chamber feed-through Plate provides feed-through connectors for the cables and water hoses. FIGURE 9-21 CHAMBER FEED-THROUGH PLATE INSIDE / OUTSIDE Heating Stage connector Water hoses flanges (blue color) Cooling Stage connector...

  • Page 172: Cooling Stage Installation

    System Options: Cooling Stage / Waterless Cooling Stage FIGURE 9-22 OUTER AND INNER CABLES Water Chiller, Flow Box and Cooling Water Hoses Note: In case the waterless Cooling stage is installed the following devices are not available. An external water chiller is provided to efficiently remove excess heat from the temperature stage.
  • Page 173 System Options: Cooling Stage / Waterless Cooling Stage 3. Place the mounting adapter on the stage rotation head and fix it through the centre using the mounting screw (finger tight). 4. Slacken off the mount locking screw on the stage body side using a metric 0.5 mm hex wrench, then place the stage on and over the mounting screw.
  • Page 174 System Options: Cooling Stage / Waterless Cooling Stage reason, which is indicated by an alarm sounds. The Start Flow button must be pressed and held again to re-establish flow through the system. CAUTION! Never pump the specimen chamber without checking for water leaks first.

  • Page 175: Software Control

    System Options: Cooling Stage / Waterless Cooling Stage SOFTWARE CONTROL Temperature Stage Control Module The cooling / heating stage is software controlled using the xT microscope Control software / Temperature Page (added when any temperature stage is installed) / Temperature Stage Control module. The Cooling / Heating button activates the Cooling / Heating stage software control.
  • Page 176 This application controls humidity of wet samples during ESEM microscope operations with the FEI Cooling Stage installed. It is possible to do so manually by the sample temperature and specimen chamber water vapour pressure control. User can set a desired sample humidity directly via the Humidity tab.
  • Page 177 System Options: Cooling Stage / Waterless Cooling Stage 9-29...

  • Page 178: Cooling Stages Basic Operations

    System Options: Cooling Stage / Waterless Cooling Stage COOLING STAGES BASIC OPERATIONS Condensation Point When determining the Cooling stage condensation point, use the flat sample holder. This positions the sample closer to the thermistor, thus giving a more accurate reading. Use carbon paint or carbon tape to hold samples onto the holder.
  • Page 179 System Options: Cooling Stage / Waterless Cooling Stage to this occurs when imaging an oil / water emulsion, in which case the oil always appears darker than water. CAUTION! When using shorter working distances, water from the sample can splash onto the GSED. To avoid this, start with a longer working distance until the sample has equilibrated, then move to a shorter working distance to optimize the image.

  • Page 180: Water Cooled Temperature Stage Operation Termination

    System Options: Cooling Stage / Waterless Cooling Stage WATER COOLED TEMPERATURE STAGE OPERATION TERMINATION 1. Let the stage cool to the room temperature. 2. Shut down the water chiller. 3. Disconnect one of the water hoses coming out the water flow box to the chamber.

  • Page 181: Wet Stem

    System Options: Wet STEM Wet STEM The Wet STEM is used to observe objects dispersed in thin liquid layer by transmitted electrons. The Wet STEM assembly consists of the following parts (in effect the Cooling Stage and the STEM I detector): •...

  • Page 182: Wet Stem Basic Operations

    System Options: Wet STEM WET STEM BASIC OPERATIONS The Wet STEM experiments are very dynamic and proper observation conditions can be stable for a few minutes only. Note: Precise control of sample humidity is essential in Wet STEM experiments. Therefore, it is highly recommended to execute the cooling stage calibration procedure (see above).

  • Page 183: Heating Stage 1000 °C / Heating Stage 1500 °C

    Heating Stage 1000 °C / Heating Stage 1500 °C The Heating stage (HS) is used to control the sample temperature up to 1000 °C, resp. 1500 °C and to observe sample with the use of FEI electron microscope. WA R NI NG ! Opening the microscope chamber does not switch off the heating.
  • Page 184 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C FIGURE 9-29 HEATING STAGE ASSEMBLY • The dovetail mounting adapter enables to attach the Heating stage to the microscope stage. • The Heating stage base (5) holds all components. •...
  • Page 185 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C Cables The Outer Cable is 4-ended cable connecting the outside of the chamber feed-through plate with the HS controller and SSB board. The greater / lesser spherical connector connects to the connector labeled Heating stage / Cooling stage (this is used in case your system enables both stages, to use only one cable).
  • Page 186 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C 2. Snap the wire hook on the printed circuit board onto the cap. 3. Plug the printed circuit board adapter into the connector on the chamber ceiling. 4. Press the cap onto the final lens aperture standard insert. 1000 °C Heating Stage variances Heat Shield is a small part sitting on the HS assembly top.
  • Page 187 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C arm is pushed away. Adjusting the Heat Shield If the heat shield touches the high temperature GSED or sits farther than 2 mm from it, the arm needs to be adjusted. It must be centred in the X / Y directions too (this may not typically need to be adjusted).

  • Page 188: Heating Stage Installation

    System Options: Heating Stage 1000 °C / Heating Stage 1500 °C HEATING STAGE INSTALLATION 1. Remove an actual (if any) sample holder adapter. 2. Install the dovetail included onto the stage rotation base (if it is not in place) parallel to the door opening direction. 3.

  • Page 189: Software Control

    System Options: Heating Stage 1000 °C / Heating Stage 1500 °C SOFTWARE CONTROL Temperature Stage Control Module The cooling / heating stage is software controlled using the xT microscope Control software / Temperature Page (added when any temperature stage is installed) / Temperature Stage Control module. The Cooling / Heating button activates the Cooling / Heating stage software control.
  • Page 190 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C The Advanced tab The Advanced tab is displayed only when the HS is connected to the feed-through plate connector. • The Auto Power check box is cleared, the Power slider becomes active and user can apply desired power directly to the heater.
  • Page 191 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C 150 - Heating Stage Settings This is the supervisor alignment procedure. • Step 1: the Temperature Ramping Limit could be set up to 300 K/min (default value is 50 K/min). Caution! Ramp speed higher than 100 K/min strongly decreases the heater lifetime and leads to regulation instability.

  • Page 192: Heating Stages Basic Operations

    The HS assemblies are factory calibrated with the standard ceramic crucible, at 400 Pa chamber pressure, under a water environment and with the ramp rate 10 K/min. At these conditions the temperature shift should be less than 50 K. In other case, contact your local FEI service representative. Note: Different pressure, environment and fast ramp speeds lead to a less accurate sample temperature readout and to incompatible results.
  • Page 193 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C FIGURE 9-37 TEMPERATURE PROFILE When the last cycle is finished, the controller holds at 600 °C (the last setpoint) indefinitely until further action is taken. Temperature Conductivity The sample crucible temperature matches the thermocouple reading. The actual sample temperature however varies, depending on the sample thermal conductivity and its thickness.
  • Page 194 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C Outgassing Samples Some types of samples may contain compounds which evaporates under high temperatures. This does not affect the pressure in the chamber. However, if large quantities of compounds are given off, they may condense and get on the aperture inside of the GSED assembly (PLA), and then astigmatism could result.
  • Page 195 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C done by simply rotating the detector so that one of the gaps in the ring faces the EDX detector. In the following photo, note that the bars on the collection ring are oriented so that the path from the EDX detector to the GSED is clear.

  • Page 196: Hs Maintenance

    System Options: Heating Stage 1000 °C / Heating Stage 1500 °C Water Cooled Temperature Stage Operation Termination Same as for the Cooling stage (see above). HS MAINTENANCE Cleaning The Heating stage could be polluted after a long term use or when using highly outgassing samples.
  • Page 197 System Options: Heating Stage 1000 °C / Heating Stage 1500 °C Consumables TABLE 9-3 HS 1000 / 1500 CONSUMABLE PARTS Item Part # HS 1000 Standard crucible (10 pcs) 4022 298 00681 Low crucible (10 pcs) 4022 298 00691 HS 1500 Standard crucible (10 pcs) 4022 298 00711 Low crucible (10 pcs)

  • Page 198: Cryocleanerec

    System Options: CryoCleanerEC CryoCleanerEC These equipments allow to decrease the contamination level in the system. The CryoCleanerEC can be efficient to approximately 24 hours (CryoCleaner – older version – has silver plated Dewar vessel and can be efficient about 10 hours). The kit consists of: •...

  • Page 199: Cryocleaner Operation

    System Options: CryoCleanerEC Flanges The Vacuum vessel has special flange enabling to mount it to different chamber ports with the use of interlink with a desired shape (depending on the port to be used and the vicinity). FIGURE 9-44 CRYOCLEANER FLANGES The interlink flanges can be mounted on by means of the 3 screw-hole fittings on the perimeter of the vacuum flange.
  • Page 200 System Options: CryoCleanerEC FIGURE 9-45 PLASTIC CAP FILLING POSITION PLASTIC CAP OPERATION POSITION Removing Nitrogen Vessel WA RN I N G ! Use the Safety pliers provided when handling the Nitrogen vessel. Removing the Nitrogen vessel depends on the level of contamination found in the specimen chamber.

  • Page 201: Maintenance

    System Options: CryoCleanerEC WA R NI NG ! When the LN2 is removed from the nitrogen vessel, the bottle still remains at a very low temperature. 5. Place the Nitrogen vessel onto the Stand ready for baking. Baking Nitrogen Vessel 1.

  • Page 202: Plasma Cleaner

    System Options: Plasma Cleaner Plasma Cleaner The Tools menu / Sample Cleaning… item starts the Sample Cleaning procedure, which is efficient process for removing very thin contamination layers, which are typically formed by hydrocarbons residues remaining on vacuum parts after conventional cleaning or could be transferred into the microscope chamber with a sample.

  • Page 203: Sample Cleaning Procedure

    System Options: Plasma Cleaner SAMPLE CLEANING PROCEDURE 1. Move the stage to the lowest Z-axis position. 2. Run the Tools menu / Sample Cleaning… procedure. When the procedure is entered from the vented state, the system pupms to the HiVac mode automatically. When the procedure is finished or aborted by the user, the system remains in the HiVac mode.

  • Page 204: 104 - Plasma Cleaning Alignment

    System Options: Plasma Cleaner 104 - PLASMA CLEANING ALIGNMENT When repeated Sample Cleaning… procedure is not efficient (see above), click the Start Chamber Cleaning button, (the procedure Duration is much longer). Warning! Do not use Chamber cleaning procedure when EDS / WDS / EBSD system is mounted! If you need to clean system with EDS detector mounted, use 1 mm collimator and do not exceed 30 minutes once a week at most.

  • Page 205: Quanta Morphologi

    System Options: Quanta Morphologi Quanta Morphologi Quanta Morphologi is a method for precise determination of size and shape of submicron particles dispersed in a dilution. It is a complex method which consists of sample preparation, image acquisition and image analysis. SAMPLE PREPARATION ITO slides Dilution with dispersed particles is deposited on the conductive side of...

  • Page 206: Image Acquisition

    System Options: Quanta Morphologi FIGURE 9-49 FILTER MEMBRANE IMAGE ACQUISITION All analyzed particles must fill certain number of pixels in the image for accurate size calculation. Therefore table of particle size classes that fulfill the pixel number requirements was defined. Use of the size classes for the image acquisition is recommended.

  • Page 207: Recommended Settings

    System Options: Quanta Morphologi FIGURE 9-50 SETUP OF CONTRAST USING VIDEOSCOPE AND USING COLOR TAB RECOMMENDED SETTINGS Several ways of image acquisition can be applied depending on the character of particles. General recommendations for settings are described below, but user tests must be done to found out the ideal settings for each type of sample.

  • Page 208: Symmetrical Low Vacuum Detector (Slvd)

    System Options: Quanta Morphologi Filter membranes Particles on filter membranes can be observed almost directly after sample preparation, but in the Low Vacuum mode only. Use: all types of conductive and nonconductive particles • pressure of 60 – 100 Pa •...

  • Page 209: Mapping Tool

    MAPPING TOOL It is located in Stage menu / Mapping tool or in Windows: Start / Programs / FEI Company / Applications / Mapping. Due to statistical reasons, a sufficient number of particles should be calculated. Therefore the Mapping tool is applied for the automatic acquisition of user-defined number of images.

  • Page 210: Image Analysis

    System Options: Image Analysis Image Analysis The Morphologi software is used for the image processing of saved images and calculation of morphological data of particles. The Morphologi SW is installed on the Support PC. Detailed description of the image processing and particle calculation can be found in the Morphologi user manual.
  • Page 211 System Options: Image Analysis FIGURE 9-53 IMAGE PROCESSING OF STANDARD SPHERES IMAGES Set the Analysis Settings and Filters according to the following pictures. FIGURE 9-54 ANALYSIS SETTINGS AND SIZE BANDS 9-63...
  • Page 212 System Options: Image Analysis FIGURE 9-55 FILTER SETTINGS: 300 nm and 1 µm SPHERES Save Image Processing to the .vsemsop file and run the measurement. After measurement, check calculated number of particles. It should be > 80. Then check the CE Diameter D[4,3] (µm). Limit is within range <0.285;...

  • Page 213: Remote Imaging

    System Options: Remote Imaging Remote Imaging The Remote Imaging enables to connect to the Microscope PC via network using the VNC application and to control the microscope operation remotely. For information how to install this functionality, see Installation Instructions available on the installation CD. For more details on the remote connection and its possibilities, see VNC documentation available on the installation CD.

  • Page 214: Microscope Pc's Desktop Sharing

    Microscope PC's screen over the network. 1. In FEI User Management application, create a non-active user account for the view only purpose. 2. Open the VNC Viewer application on the remote PC of the person who is intended to control the microscope and connect remotely to the Microscope PC as user/supervisor.

  • Page 215: Beam Deceleration

    System Options: Beam Deceleration Beam Deceleration The Beam Deceleration mode (BDM) method is based on a negative voltage Stage Bias (bias) applied to a stage (i.e. a sample). The electrical field between the sample and the nearest surface above (a column bottom or a detector) is formed, acting as the additional electrostatic lens.

  • Page 216: Stage Modification

    System Options: Beam Deceleration STAGE MODIFICATION When extending the system capabilities with the Beam Deceleration mode, it is necesary to make the stage modification by mounting the BD attachment on the stage head. For systems acquired with the Beam Deceleration this procedure is not carried out. 1.

  • Page 217: Beam Deceleration Applications

    System Options: Beam Deceleration BEAM DECELERATION APPLICATIONS • The BDM enables detection of the BSE when the electron energy is under the detection limit of the detector. • The BDM expands the electron energy range under the minimum HV limit. •...
  • Page 218 System Options: Beam Deceleration Beam Deceleration Mode Imaging Procedure 1. Put the sample into the chamber and pump to the HiVac. In the BDM a sample becomes the electrode. Its position, size, tilt and surface roughness influence an imaging quality. At optimal conditions the sample should be symmetrical, planar, have a size comparable with the detector size, and placed perpendicular to the column axis.

  • Page 219: Specimen Holder Kit Option

    System Options: Specimen Holder Kit Option Specimen Holder Kit Option The Specimen Holder Kit is Universal. The interfacing parts allow the fitting of all the common components to the Inspect S, Inspect F, Quanta and Quanta FEG. Major holders in the kit locate with a 2 pin system originating from the stage rotation head, through the interface piece, to the holder.

  • Page 220: Older Interface Adapter

    System Options: Specimen Holder Kit Option FIGURE 9-59 QUANTA 450 LOCATION POSITIONS Location slot Single holder threaded hole Location hole OLDER INTERFACE ADAPTER This adapter is used on pre-Quanta 50 mm stages that had no 2 pin locating holes. The old centre rotation head needs to be removed from the stage and this component should replace it.

  • Page 221: Multi-Holders

    System Options: Specimen Holder Kit Option FIGURE 9-61 INTERFACE PILLAR FOR MULTI-HOLDERS Analytical holder screw positions Location pins Location pins bottom MULTI-HOLDERS The Multi-Holders fit individually on the Interface pillar using the same pin location system. Numbers 1 and 2 have a captive centre screw for fixing to the Interface pillar, where as number 3 has two captive screws offset from the centre.

  • Page 222: Polished Mount Holders

    System Options: Specimen Holder Kit Option Analytical Holder (3) The Analytical Holder is use in conjunction with an EDX system. 2 polished 1inch mounts can be slotted from below into the retaining holes until they become flush to the top of the holder. Here they can be locked in place by screws in the holder side wall.

  • Page 223: Quick Loader

    System Options: Quick Loader Quick Loader The Quick Loader comprises of the following components: • Gate valve unit with system safety interlocking • Lead glass door and loading chamber • Sample sledges and Stage Adapter • sample stubs of diameters 12.5 mm, 25 mm and 32 mm •...
  • Page 224 System Options: Quick Loader Loading rod The loading rod has a pre-machined slot to move in to load or unload a sample. At each end there is a side slot. There are 2 side slots at the further end from the vacuum chamber. One is for loading and unloading the sample carrier in the loader chamber and the other is a parking position (prevents the rod to be sucked in by the vacuum).
  • Page 225 The Stage Adapter is connected to the rotation base of the FEI stage by 3 hexagonal headed screws. The base of the adapter has 3 highpoints for a firm 3-point contact to the rotation base to prevent vibration transmission.

  • Page 226: Installation

    System Options: Quick Loader INSTALLATION The Quick loader is pre-installed in FEI factory. No special adjustment is needed only the loading rod was uninstalled for transport. 1. Unpack the lead glass lid. 2. Remove four screws holding the cover of the loading rod feedthrough.

  • Page 227: Operations

    System Options: Quick Loader OPERATIONS Loading a sample 1. Mount the sample with fast drying adhesive medium onto the stub. Allow to dry. 2. Check the sample satisfies the sample limits imposed by placing the top of the mounting tool over the base mount. Caution! If the sample proves to be too large this has to be addressed before the sample and carrier should be allowed into the loader...
  • Page 228 System Options: Quick Loader Unloading a sample 1. If there is a sample carrier in the loader chamber attached to the bayonet, remove it (the chamber needs to be vented and the carrier removed). 2. Switch OFF the electron and ion beam accelerating voltage. Retract the GIS, Omniprobe or STEM modules (if present) to a safe state (can not be used in combination with loader).

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