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Zeiss Crossbeam 350, Instruction Manual

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Zeiss Crossbeam 350 Instruction Manual Download Page 126

Carl Zeiss Microscopy GmbH

Carl-Zeiss-Promenade 10
07745 Jena
Germany

phone: +49 1803 33 63 34
fax: +49 3641 64 3439

[email protected]
www.zeiss.com/microscopy

Instruction Manual ZEISS Crossbeam 350 | en-US | Rev. 3

Modifications reserved. | Printed in Germany

Summary of Contents for Crossbeam 350

Page 1: ...Instruction Manual ZEISS Crossbeam 350 Focused Ion Beam Scanning Electron Microscope FIB SEM ...

Page 2: ...s for archiving purposes shall remain unaffected thereby Any viola tions may be prosecuted as copyright infringements The use of general descriptive names registered names trademarks etc in this document does not imply that such names are exempt from the relevant intellectual property laws and regulations and therefore free for general use This shall also apply if this is not specifically referred...

Page 3: ...ressure Hazards 15 2 3 6 Magnetic Field Hazards 15 2 3 7 Mechanical Hazards 16 2 3 8 Radiation Hazards 16 2 3 9 Suffocation Hazards 16 2 4 Safety Equipment 17 2 4 1 Protective Cover Panels 17 2 4 2 Main Switch 18 2 4 3 Emergency Off EMO Option 18 2 4 4 Locking Devices 19 2 4 5 Lockout Tagout Equipment 20 2 4 6 Safety Labels 20 3 Product and Functional Description 24 3 1 System Overview 24 3 2 Main...

Page 4: ...de 74 6 3 2 Measuring the Probe Current 75 6 3 3 Changing the Extractor Voltage 76 6 4 Working with Different Aperture Configurations and Beam Modes 76 6 4 1 Determining the Installed Aperture Configuration Gemini I Column 76 6 4 2 Selecting the Aperture 77 6 4 3 Selecting the Column Mode 77 6 5 Finding Appropriate Detector Settings 78 6 5 1 Selecting a Detector 78 6 5 2 Setting up the InLens SE D...

Page 5: ...cking the Position of the Circuit Breakers 103 8 6 Detectors 103 8 6 1 Lubricating the Rod 103 8 7 Focused Ion Beam 104 8 7 1 Checking the Lifetime of the Ion Source 104 8 7 2 Regenerating the Ion Source by Heating 105 8 7 3 Manually Finding a New Extractor Value 105 9 Shutdown and Disposal 107 9 1 Putting the Microscope out of Operation 107 9 2 Transport and Storage 107 9 3 Disposal 109 9 3 1 Dis...

Page 6: ...e is almost no loss in beam brightness even at low acceleration voltages Sec ondly the beam booster technique en hances protection against external stray fields BSD Backscattered Electron Detector BSE Backscattered Electron CL Cathodoluminescence Condenser Device that collects and focuses the elec tron beam onto the specimen EBSD Electron Backscatter Diffraction EDS Energy Dispersive X ray Spectro...

Page 7: ...lectron beam becomes rotationally symmetrical Suppressor Electrode anode that suppresses un wanted thermionic emission from the shank of the Schottky field emitter U Voltage VP Variable Pressure Instruction Manual ZEISS Crossbeam 350 en US Rev 3 349500 8111 000Instruction Manual 7 ...

Page 8: ...microscope and its main hardware components Software Description Provides an overview of the user interface Installation Refers to the ZEISS service representatives Operation Contains information about starting the microscope and the software obtaining a first image adjusting important parameters and power ing down the microscope also in emergency Maintenance and Repair Informs you about preventiv...

Page 9: ...ss com corporate int home html Link to a website on the internet Tab 2 Link types 1 2 Explanation on Warnings and Additional Information DANGER WARNING CAUTION and NOTICE are standard signal words used to determine the lev els of hazards and risks of personal injury and property damage Not only the safety instructions and warnings in the Safety chapter are to be considered but also the safety inst...

Page 10: ...re for imaging and hardware con trol refer to the SmartSEM software manual SmartFIB Software Manual For detailed information on how to use the SmartFIB software for ion beam exposure refer to the SmartFIB software manual Instruction Manual for Options For detailed information regarding optional accessories refer to the respective instruction manual in your document folder Product Specification and...

Page 11: ...439 Email info microscopy de zeiss com Service Germany Phone 49 7364 20 3800 Fax 49 7364 20 3226 Email service microscopy de zeiss com Courses and training Email courses microscopy de zeiss com ZEISS Sales Service Partner You can find a ZEISS Sales Service Partner in your area under https www zeiss de mikroskopie website forms sales and service contacts html Instruction Manual ZEISS Crossbeam 350 ...

Page 12: ...on beam SEM Imaging or a focused ion beam FIB Imaging that is scanned across the speci men This application allows for the analysis of surface structures and near surface structures of ap propriate specimens Milling Milling comprises all applications that include material removal from the specimen surface by a focused ion beam In combination with a gas injection system option the microscope has be...

Page 13: ...all protective cover panels are installed Always follow the instructions given on the safety labels Inspect and clean the product safety labels to maintain good legibility 2 2 2 Requirements for Personnel Deviating from the instructions given in this manual and on the safety labels can be hazardous or can lead to property damage Do not operate the microscope until you have completely read and unde...

Page 14: ...ions and instructions may result in personal injury and property damage 2 3 1 Biological Hazards Danger to life Biological substances Biological substances may pose a threat to the health of humans and other living organisms Keep a logbook of the biological substances loaded into the microscope and show it to the ZEISS service representatives before they perform any work on the microscope 2 3 2 Bu...

Page 15: ... ment Only authorized ZEISS service representatives are allowed to service the microscope Do not try to service the microscope yourself Danger to life High leakage currents High leakage currents are present in the microscope Contact may cause burn or electrical shock Ensure proper grounding For more information refer to the Installation Requirements docu ment Do not operate the microscope without ...

Page 16: ...ion devices which under regular oper ating conditions ensure that the microscope operates in accordance with the German X ray pro tection regulation RöV the German radiation protection regulation StrSchV as well as with the EC Directive 2013 59 EURATOM In the EU the operation of the microscope is permission free as the following requirements are fulfilled The acceleration voltage is limited to 30 ...

Page 17: ...ick Download 2 4 Safety Equipment In order to prevent hazards to human health or property damage the microscope is equipped with several safety features 2 4 1 Protective Cover Panels Due to hazardous voltages and X rays inside the microscope the microscope is equipped with protective cover panels 1 2 3 Fig 1 Protective cover panels 1 Electron optical column protective cover panels 2 Specimen chamb...

Page 18: ...ergency Off EMO Option With the Emergency Off EMO option the microscope is equipped with the following additional safety equipment Microscopes with SEMI certification must be equipped with the Emergency Off EMO option Emergency Off EMO Button The EMO button is located on the plinth adjacent to the specimen chamber The EMO button must be pressed in an emergency to cut off mains power from the micro...

Page 19: ... side of the specimen chamber When this locking device is activated i e no electrical contact EHT Vac ready no is indi cated in the SmartSEM user interface EHT and SE detector voltages are blocked 2 4 4 2 Vacuum Locking Device The vacuum locking device ensures that gun vacuum and system vacuum are better than the re quired thresholds 2 4 4 3 Interlock System of Optional Airlock The interlock funct...

Page 20: ...he connections to the corresponding media when needed must be lockable in their off position in order to prevent accidental re activation The customer is responsible for having a working knowledge of the LOTO specification purchasing distributing and installing appropriate LOTO equipment auditing and enforcing compliance with LOTO procedures to all authorized personnel providing instructions on ho...

Page 21: ... of the Microscope 4 Labels Attached to the Rear Side of the Plinth 5 6 7 The safety labels always need to be attached to the correct spots at the microscope If a safety la bel is lost or unreadable it needs to be reordered via the following reorder numbers Instruction Manual ZEISS Crossbeam 350 en US Rev 3 349500 8111 000 21 ...

Page 22: ...e operating this product Reorder no 347800 0033 000 01en 4 At the rear of the electron optical column Contact may cause burn or electric shock Only authorised service Staff is allowed to service the equipment Disconnect power before opening Hazardous voltage inside WARNING 347800 0033 000 03en Hazardous voltage inside Contact may cause burn or electric shock Only authorized service Staff is allowe...

Page 23: ...freeze burns or severe frostbite Wear face eye and skin protection For relevant options Liquid nitrogen Contact with liquid or cold vapors can cause freeze burns or severe frostbite Wear face eye and skin protection Reorder no 347800 0033 000 09en Underneath the cover panels of the microscope there are some more safety labels which are ad dressed to authorized ZEISS service representatives These s...

Page 24: ...ctron optical column Refer to Electron Optical Column Gemini I 30 2 Ion getter pumps IGPs for FIB 3 FIB column optional Refer to Ion sculptor Focused Ion Beam FIB Column Optional 32 4 Specimen chamber with door handle 5 Plinth with ON STANDBY OFF buttons 6 Monitor 7 Work desk 8 Dual joystick Refer to Dual Joystick 40 9 Personal Computer PC 24 Instruction Manual ZEISS Crossbeam 350 en US Rev 3 3495...

Page 25: ... to instruction manual Flood Gun 5 Single needle GIS for high angle specimen access Refer to instruction manual UniGIS 6 Micro manipulator for specimen modification and probing 7 aBSD detector for high efficiency BSE detection and angle selective material characteriza tion Refer to aBSD Detector 44 8 EsB detector for finest z resolution without topographic artifacts and unique material contrast Re...

Page 26: ...Ablation Upgrade Refer to instruction manual Rapid Laser Ablation Upgrade Time of flight secondary ion mass spectrometer TOF SIMS Refer to instruction manual TOF SIMS Further options on request 3 2 Main Components 3 2 1 Vacuum System Purpose For operation of the microscope the gun head the column and the specimen chamber have to be evacuated The vacuum is essential to operate the gun and to preven...

Page 27: ... gauge 14 Vent valve 15 Roughing backing valve RBV 16 Pre vacuum pump The microscope can be operated in different vacuum modes High vacuum HV mode Variable pressure VP mode optional HV mode characteristics Pressure regions HV mode is the standard mode of the micro scope HV mode offers the possibility of analyz ing and mapping conducting specimens In HV mode the pressure in the specimen chamber is ...

Page 28: ... chamber from the column System Vacuum in VP Mode The pre vacuum pump 16 directly evacuates the specimen chamber 6 The roughing back ing valve RBV 15 opens the connection between pre vacuum pump and specimen chamber The Turbo isolation valve TIV 8 is closed so that the turbo pump 9 is separated from the specimen chamber The turbo pump evacuates the lower part of the column via bypass 5 The needle ...

Page 29: ... column chamber valve closes and gaseous nitrogen flows into the specimen chamber via the vent valve 14 As soon as the pressure equilibrium is obtained the chamber door can be opened to change the specimen Evacuating In order to continue operation the Pump command makes the pre vacuum pump and the turbo pump evacuate the specimen chamber As soon as the vacuum in the specimen chamber is ready for o...

Page 30: ...Sup UB 2 1 3 4 5 6 7 8 9 Fig 9 Schematics of the electron optics 1 Gun 2 Extractor Positive electrode that extracts electrons from the filament 3 Anode aperture 4 Multihole aperture aperture changer 5 Condenser 6 InLens SE detector EsB detector 7 Objective lens Focuses the electron beam on to the specimen surface 8 Scanning coils Deflect the beam across the specimen surface in what is usually refe...

Page 31: ...ter Probe current Typical application 40 μm 5 pA to 20 nA High resolution 100 nA high current configuration Anode aperture diameter Probe current Typical application 90 μm 12 pA to 100 nA Combined high resolution and analytical investigations The multihole aperture is the final beam limiting aperture It is decisive for the probe current The standard is the 30 μm aperture hole that is the central a...

Page 32: ...d Improved depth of field when combined with small apertures 60 µm Minimum Probe Current Smallest possible probe currents for low dose applications Fisheye Very large field of view at an EHT of 100 V Larger working distances are suggested Widefield Large field of view with the InLens detector Requires the SmartSEM software license Field Mode 3 2 3 Ion sculptor Focused Ion Beam FIB Column Optional ...

Page 33: ... be continuously adjusted in the range between 1 pA and 100 nA Objective Lens The objective lens is designed as an electrostatic Einzel lens system It focuses the beam onto the specimen surface 3 2 3 1 Imaging Modes Purpose With the FIB option different imaging modes are available to operate the microscope 1 2 3 Fig 11 Imaging modes available with the FIB option Imaging Mode FIB Mode Characteristi...

Page 34: ...ecially suitable where the working distance is large Surface detail as the effect of lateral illumination emphasizes the topography of the specimen Backscattered Electrons BSEs Backscattered electrons BSEs emerge from below the surface of the specimen up to an order of µm The number of electrons emitted at the point of impact is highly dependent on the mean atomic number of the specimen material T...

Page 35: ...r 36 SE1 Surface structure SE Detector 37 SE2 Topography Optional Detectors Detected Signals Typical Application VPSE Detector 41 SE2 Topography in VP mode SESI Detector 42 SE2 Ions Channeling contrast crystal orientation Compositional contrast EsB Detector 43 SE1 BSE Surface structure Material contrast aBSD Detector 44 BSE Angular resolved BSE imag ing Compositional contrast aSTEM Detector 47 Tra...

Page 36: ...ive lens by the electrostatic lens This electrostatic field acts as acceleration field for the SEs generated on the specimen surface At the InLens SE detector the electrons hit a scintillator This generates a flash of light that is led out of the beam path and onto a photomultiplier by means of a lightguide The photomultiplier converts the light information into an electronic signal which can be d...

Page 37: ...d directed to the scintillator The electrons gain energy from the scintillator and thus are able to interact with a phosphor layer which generates photons light The light travels up a light pipe to a photomulti plier The photomultiplier multiplies the flashes of light and outputs a signal that can be used for imaging The collector voltage can be varied in the range between 250 V and 400 V A positi...

Page 38: ...e chamber CCD camera has two illumination modes The chamber can be illuminated either with white light or with infrared light Infrared light gives a grayscale image whereas white light gives a color image In standard settings the mode is automatically selected depending on the imaging mode and the selected detectors White light limits the performance of most detectors Therefore infrared illuminati...

Page 39: ...moving a tilted stage in X Y direction no displacement moving out of focus occurs When a pre tilted specimen holder is used X Y movements require an adjustment of the Z position to stay in focus The stage can be operated using the Dual Joystick 40 or using the SmartSEM software Axis Description Movement X X axis Movement towards or away from the cham ber door horizontal movement in the image Y Y a...

Page 40: ...k push button Stops the stage in an emergency 3 M push buttons Controls a second Z axis M on super eucentric stages to set the eucentric point of the specimen tilt on these stages 4 X Y R joystick Controls the X and Y axes and the stage rotation by turning Operating Principle All axes are deflection compensated When the joystick is moved only slightly the respective axis moves slowly Larger moveme...

Page 41: ... 3 4 5 Fig 18 Schematics of the VPSE detector 1 Preamplifier 2 Photomultiplier 3 Objective lens 4 Light guide with collector electrode 5 Specimen Operating Principle The collector electrode mounted on the light guide 4 is held on a positive potential forming a collecting field for SEs Thus SEs move towards the detector In VP mode gas molecules are present in the specimen chamber The accelerated SE...

Page 42: ... the polarity of the collector voltage either electrons or ions scattered from the specimen 5 are attracted by a collector grid 4 and accelerated to the converter In the converter both electrons and ions are converted into secondary electrons which are used to gen erate an image Detector Mode FIB Mode Detected Signals Typical Application SE mode typical collector voltage 300 V SEM FIB Secondary el...

Page 43: ...EsB detector right 1 EsB detector 2 Filtering grid 3 InLens SE detector Operating Principle A small amount of SEs pass through the hole of the InLens SE detector 3 and would be ob served by the EsB detector 1 To prevent detection of these SEs a filtering grid 2 is in stalled in front of the EsB detector By switching on the filtering grid voltage the SEs are rejected and only BSEs are detected Belo...

Page 44: ...t to Auto Detect then the TV illumination is automatically switched off when a diode detector is used The BSD detector has applications mainly in materials analysis and in the life sciences Material analysis Metallurgical sections Geological sections Complex materials Printed circuit boards Semiconductors Bond pads Life sciences Mineral deposits in plant structures Bone structures The BSD detector...

Page 45: ...a high enough energy can create electron hole pairs and can contribute to image generation Electrons that have a lower energy e g secondary electrons are not detected by the BSD detector The emission of backscattered electrons from a specimen is related to the atomic number of the involved material Elements with high atomic numbers generate more backscattered electrons i e the backscatter coeffici...

Page 46: ...t disturbing your image quality NOTICE Risk of property damage Short working distance When inserted the aBSD detector is positioned directly underneath the objective lens The lower edge of the detector is then located at a working distance of 1 5 mm If you move the specimen to a working distance below 1 5 mm then you damage the aBSD detector 4 Do not move the specimen to working distances below 2 ...

Page 47: ...the CCD Mode is set to Auto Detect then the TV illumination is automatically switched off when a diode detector is used Operating Principle The aSTEM detector is a pneumatically retractable multi mode detector with a 12 stub specimen holder for bright field and dark field detection The diodes of the aSTEM detector collect transmitted electrons below the ultrathin specimen A special arrangement of ...

Page 48: ...plays details concerning the diode status and the diode arrangement Each diode segment can have the following status On The signal is added to the total signal Inverted Inv The signal is inverted and then added to the total signal Off The signal is not used NOTICE Risk of property damage Motorized specimen stage Risk of damaging the detector when operating the motorized specimen stage 4 Retract th...

Page 49: ...eracting with the primary electron beam Differences in crystal structure or the presence of impurities in a cathodo luminescent material result in variations in the energy gap between the filled valence bands and the empty conduction bands and consequently a change in the CL emission The light photons emitted by the specimen is collected by the CL detector and converted into a signal for imaging T...

Page 50: ...umn axis 3 Scan Rotate Rotates the scanning pattern 360 continuously This turning knob has a push button function to deactivate the scan rotate function and reset the scan rotation to 0 4 Shift X Shift Y Shifts the scanned region of the specimen in the X and Y directions 5 Brightness Contrast Brightness Adjusts the image acquisition chain offset for the currently selected detector Each configured ...

Page 51: ...xchange Resume Exchange Starts the pre defined macro for specimen exchange with the airlock Resume Starts the pre defined macro to finish specimen exchange with the airlock 10 Camera Switches to chamber view 11 Focus Scan Speed Focus Changes the focal point of the column by adjusting the magnitude of the objective lens Scan Speed Increases or decreases the scan speed by doubling or halving the bea...

Page 52: ...creen layout of the user interface 1 Title Bar Displays the name of the user interface and the logged on user 2 Menu Bar Enables you to access to SmartSEM features via sub menus 3 AVI Toolbar Contains the controls to set up record and play back video sequences of scanned images 4 Toolbar Provides quick access to SmartSEM tools 5 Image Area with Data Zone Displays image information and acquisition ...

Page 53: ...ently used dialogs and to the recipe management 4 1 2 Graphical Control Elements The following graphical control elements are used in the SmartSEM GUI Screenshot Control El ement Function Tab Provides a group of graphical control elements Section Forms a group of control elements with related functions Button Enables you to start an action Checkbox Enables you to activate or deactivate a function ...

Page 54: ...nistrator User Access Level Description Novice Only the items assigned to the novice category are accessible These include most frequently used parameters Expert Items assigned to the novice and expert category are accessible These include parameters useful for advanced operators Service All items are accessible also including infrequently used items and cal ibrations Additional to the user access...

Page 55: ...which implements the internal communi cation between control software and microscope hardware plus several programs and utilities The main purpose of the SmartSEM Program Suite is to access all necessary microscopy parame ters and software features to capture SEM data and optimize image acquisition Access Windows start menu SmartSEM Program Description ChamberScope Enables you to display the chamb...

Page 56: ...presentatives only Gun Monitor Enables you to monitor important parameters of the microscope GUN Service Service activities for ZEISS service representatives only Piezo Configurator Service activities for ZEISS service representatives only Service Centre Provides an overview of the state of the microscope Smart Stage Map ping Service activities for ZEISS service representatives only SmartBackup To...

Page 57: ...g Area the following items are displayed Live Mode captured image and patterning elements Editing of patterning elements is possible only in Live Mode Sample Mode Virtual Sample and writing positions EPD Mode captured image and thickness map 4 Control Panel Contains tabs for controlling the FIB process The range of visible tabs depends on the se lected mode 5 Status Bar Left hand side informs you ...

Page 58: ...the desired value is set Readout Displays the status of a system entity Enables you to select an action or a value by opening a dialog with an input field Input field Enables you to enter the desired value Slider Enables you to adjust the corresponding function Expandable sec tion Enables you to expand or collapse the section as required 4 2 3 SmartFIB Program Suite The SmartFIB program suite comp...

Page 59: ...inly used for editing patterns and structures and creating recipes Sample Mode Mainly used for creating recurring automated workflows EPD Mode Used for thickness determination of a TEM lamella Designer Offline creation of layouts Arrangement of elements in the scan ning area Interaction with Sample Mode Used as a drawing tool for Sample Mode Instruction Manual ZEISS Crossbeam 350 en US Rev 3 34950...

Page 60: ...arried out by an authorized ZEISS service represen tative An excerpt of the installation requirements can be found under Installation Requirements 114 For more details refer to the document Installation Requirements 60 Instruction Manual ZEISS Crossbeam 350 en US Rev 3 349500 8111 000 ...

Page 61: ...e microscope has been de energized by turning the MAIN switch to the OFF position ü Alternatively the microscope has been de energized by pressing the Emergency Off EMO button 1 Verify that the main shut off valves for compressed air nitrogen and cooling water at the facility installation are operable Otherwise open and unlock the main shut off valves 2 If the Emergency Off EMO option is installed...

Page 62: ...oscope à The EM Server Log On dialog is displayed 3 Enter the user name and password 4 Click OK à The SmartSEM user interface opens and is ready to operate the microscope 6 1 3 1 Calling up the Help There are different ways to access topics in the Online Help Function Menu Shortcut Control Elements Startup page Help F1 Table of Contents Help Contents Ctrl F1 Context sensitive Shift F1 F1 on focus ...

Page 63: ...hift to zero SCROLL LOCK Toggles Freeze Unfreeze PAUSE Causes currently executing macro to continue Performs Find Image function CTRL 2 Loads Second Image Window from display CTRL A Switches Annotation panel ON CTRL B Display Toolbar View dialog CTRL D Toggle Data Zone ON OFF CTRL E Calls the Export TIFF dialog CTRL F Starts Auto Focus fine CTRL SHIFT F Starts Auto Focus coarse CTRL G Switches Cro...

Page 64: ...Performs Centre Point function 6 2 Obtaining a First Image Info Mobile phones in the microscope room can cause image quality infringements and in worst case workflow interruptions This section describes basic procedures to obtain an image using the SE detector To simplify the procedure the description uses the Crossbeam SEM Control panel and status bar functions in the SmartSEM software Overview T...

Page 65: ...age Contamination caused by fingerprints Contamination caused by fingerprints can lead to vacuum deterioration or prolonged pumping times 4 Always wear lint free gloves when touching the specimen specimen holder or stage 1 To attach a specimen to the stub use conduc tive carbon adhesive metal tape carbon tape or similar Ensure that the specimen area that you want to analyze is in proper contact wi...

Page 66: ...Low Position Prerequisite ü The stage is initialized 1 In the Crossbeam SEM Control panel select the Imaging tab 2 In the Detector Active Channel section select TV from the Signal A drop down list à The inside of the specimen chamber is visible in the Image Area 3 In the Crossbeam SEM Control panel select the Stage tab 4 Activate the Track Z checkbox à The current working distance WD is displayed ...

Page 67: ...ays close the chamber door before moving the specimen stage 4 To remove parts fallen into or near to the stage use a tool e g tweezers instead of your fingers CAUTION Risk of injury Closing the chamber door Fingers can be pinched when closing the chamber door 4 Use the door handle to close the chamber door 4 Ensure not to get your fingers caught in the chamber door gap NOTICE Risk of property dama...

Page 68: ...ub under the Electron Beam NOTICE Risk of property damage Driving the stage While the stage is driven manually there is a risk of damaging the objective lens and or the specimen 4 Ensure not to hit the objective lens while driving the stage 4 Monitor the moving stage in TV mode 4 To stop the moving stage immediately press F12 or press the Break push button of the dual joystick panel 4 Manually low...

Page 69: ...roperty damage Schottky field emitter If the Schottky field emitter is switched on and off too frequently or inappropriately its lifetime is reduced 4 Avoid switching off the gun during the working week 4 Use Standby mode for the weekend or a break of up to a week 4 When using the Standby mode activate the Partial Vent on Standby function Prerequisite ü The chamber and the gun head have been evacu...

Page 70: ...tness contrast Overview The procedure contains the following steps Selecting the Column Mode and Probe Current 70 Selecting the SE Detector 70 Setting a Fast Scan Speed 71 Setting a Low Magnification 71 Setting a Long Working Distance 71 Adjusting Brightness and Contrast 71 Visualizing Details on the Specimen Surface 71 6 2 6 1 Selecting the Column Mode and Probe Current 1 In the Crossbeam SEM Con...

Page 71: ...splayed 2 In the WD input field enter 10 3 Click OK à The working distance is set to WD 10 mm 6 2 6 6 Adjusting Brightness and Contrast 1 In the Crossbeam SEM Control panel select the Imaging tab 2 In the Detector Active Channel section use the scroll bars to adjust brightness and con trast 6 2 6 7 Visualizing Details on the Specimen Surface 1 Select a detail on the specimen surface 2 Verify the M...

Page 72: ... up to Mag 50 000 x and focus in between To adjust the magnification and the focus hold down the left mouse button or the mouse wheel respectively and drag the mouse within the Image Area 6 2 7 2 Moving the Field of View at High Magnifications If you want to move the field of view at high magnifications use the Beam Shift function instead of moving the stage 1 In the Crossbeam SEM Control panel se...

Page 73: ...detail should just be pulsating without shifting 7 In the Focus Wobble window click OFF to deactivate focus wobble à The Focus Wobble window closes 8 Refocus the image 6 2 7 5 Selecting the Scan Speed 1 In the Toolbar from the Faster Slower drop down list select Scan Speed 7 Alternatively in the Crossbeam SEM Control panel select the Imaging tab and from the Scan Speed drop down list select Scan S...

Page 74: ...nalytic Normal Gun Mode In Normal gun mode the temperature of the Schottky emitter gun filament and the extraction voltage are optimized for a long lifetime of the Schottky emitter Normal gun mode is suitable for most applications Imaging Gun Mode In Imaging gun mode the temperature of the Schottky emitter and the extraction voltage are re duced in comparison to the Normal gun mode This leads to a...

Page 75: ...click Analytic INFO For maximum probe current also check the alignment of the gun INFO If you use the Analytic gun mode then the lifetime of the emitter is reduced 6 3 2 Measuring the Probe Current Measuring the probe current using the Faraday cup ensures that the current displayed in the soft ware equals the incident probe current The Faraday cup consists of a strongly absorbing material with a c...

Page 76: ...actor is required to change the extractor voltage 1 From the Menu Bar select Beam Gun Setup à The Gun Service dialog is displayed 2 To increase the extractor voltage double click the Extractor V Target readout à The Extractor V Target window is displayed 3 Enter a higher value 4 Click OK 6 4 Working with Different Aperture Configurations and Beam Modes 6 4 1 Determining the Installed Aperture Conf...

Page 77: ...larger aperture generates a larger probe current and is used for applications that require a high beam brightness e g EDX or a large depth of field Changing to a smaller larger aperture will reduce increase the convergence angle accordingly This could lead to decrease in resolution 1 In the Crossbeam SEM Control panel select the Control tab 2 In the Beam section select an aperture from the Apertur...

Page 78: ...tector 79 Setting up the VPSE Detector 80 Setting up the SESI Detector 82 Setting up the aBSD BSD Detector 83 Setting up the HT BSD Detector Setting up the EsB Detector 81 Setting up the aSTEM STEM Detector 85 Setting up the CL Detector 88 1 Select the Imaging tab of the Crossbeam SEM Control panel 2 Select the detector from the Signal A drop down list 6 5 2 Setting up the InLens SE Detector The I...

Page 79: ...tor collects the SE signal highlighting the topography of the specimen Fig 31 An eledone tentacle The following settings are recommended for the SE detector EHT Typical WD Collector Voltage 500 V 5 kV 2 8 mm Adjustable from 250 V to 400 V Standard applications 300 V At a high magnification you can opti mize the image by varying the collector voltage Pseudo backscattered BSE image 250 V to 50 V Thi...

Page 80: ...bias voltage 1 kV 30 kV 7 10 mm Adjustable from 0 to 1 kV The optimum value depends on the pres sure in the specimen chamber Prerequisite ü The microscope is operating in VP vacuum mode 1 In the Crossbeam SEM Control panel select the Imaging tab 2 From the Signal A drop down list select VPSE 3 Adjust the EHT and the working distance WD according to the suggestions in the table à First adjust the c...

Page 81: ...g grid voltage is set to 0 SE and BSE mixed images can be acquired Fig 33 Silver nanoparticles embedded in zeolite imaged at 1 5 kV The following settings are recommended for the EsB detector EHT Typical WD Filtering Grid 500 V 10 kV 0 5 mm EsB Grid 400 V to filter out the SE signal 20 V 500 V 0 3 mm EsB Grid 0 V for use as an additional SE de tector 1 In the Crossbeam SEM Control panel select the...

Page 82: ...IB mode FIB EHT Typical WD Collector Voltage 2 kV 30 kV Coincidence point Adjustable from 0 V to 1500 V Best detection 300 V to 400 V Settings when working in ion mode secondary ions imaging FIB mode FIB EHT Typical WD Collector Voltage 2 kV 30 kV Coincidence point Adjustable from 4 kV to 0 kV Best detection Around 4 kV 1 In the FIB Toolbar from the Imaging Mode drop down list select an imaging mo...

Page 83: ...raphy bottom left For comparison Surface contrast seen with the InLens SE detector bottom right The following settings are recommended for the aBSD detector EHT Typical WD Detector Settings 0 5 30 kV 5 12 mm Compositional mode for obtaining an image that is high in atomic number contrast Use topographic mode for showing surface details Use individual settings for channeling con trast Make use of d...

Page 84: ...istance WD according to the suggestions in the table in order to optimize the image 6 In the BSD Control panel click a quadrant symbol to toggle its status between on white inverted black and off gray 7 To choose the respective mode click BSD COMPO or BSD TOPO The default setting for BSD is BSD COMPO All six segments S1 S6 aBSD or four seg ments S1 S4 BSD are set to on and an image that is high in...

Page 85: ... output signal in order to allow dif ferent STEM imaging modes e g bright field BF or oriented dark field ODF The most com monly used STEM imaging modes are predefined and can be selected from a drop down menu in the STEM Control panel Fig 36 Asbestos oriented darkfield ODF image captured with an aSTEM4 detector left ODF image showing real information about bending and lattice defects within each ...

Page 86: ...S3 ODF S2 S3 ODF90 S3 S2 ODF BF S1 S2 S3 ODF90 BF S1 S2 S3 BF DF S1 S2 S3 ADF S2 S3 S4 HAADF Middle S4 HAADF outer S5 HAADF S4 S5 User defined name Custom combination of segments Active segments with signs Custom combination of segments on inverted 86 Instruction Manual ZEISS Crossbeam 350 en US Rev 3 349500 8111 000 ...

Page 87: ...ed in the selected zone 3 From the Signal A drop down list select a STEM detector e g aSTEM1 4 In the Panel Configuration Bar double click STEM Control To open the Panel Configuration Bar from the Menu Bar select Tools Goto Panel à The STEM Control dialog is displayed In the upper section the STEM Control dialog displays the status of the diode seg ments The status is either on white inverted blac...

Page 88: ...30 kV 6 10 mm min 4 mm 1 In the Crossbeam SEM Control panel select the Imaging tab 2 From the Signal A drop down list select CL 3 Adjust the EHT and the working distance WD according to the suggestions in the table in order to optimize the image 6 6 Working with Variable Pressure VP mode offers the possibility of analyzing and mapping non conducting strongly gassing or moist specimens without any ...

Page 89: ...cceleration voltage is activated 6 6 2 Returning to HV Mode HV mode is the standard mode of a FESEM It offers the possibility of analyzing and mapping con ducting specimens In HV mode the pressure in the specimen chamber is less than 10 mbar Info A higher pressure can be set within a few seconds Achieving a lower pressure may require some more time because the specimen chamber has to be evacuated ...

Page 90: ... The microscope is in ON mode 1 In the Crossbeam SEM Control panel select the Gun tab 2 Activate the EHT Off Log Off checkbox 3 Activate the Leave Gun On at Shutdown checkbox 4 Only when interrupting work for longer periods between 2 and 7 days In the Vacuum tab activate the Partial Vent on Standby checkbox à This maintains the gun vacuum and switches off and protects the turbo pump 5 Exit the Sma...

Page 91: ...m the microscope 6 To disconnect the power connection at the facility installation remove the power plug male connector from the socket female connector 7 To secure the microscope against accidental re activation refer to Performing a Lockout Tagout 91 See also 2 Finishing the Work Session 90 2 Performing a Lockout Tagout 91 6 7 3 Performing a Lockout Tagout The Lockout Tagout LOTO procedure defin...

Page 92: ... the high voltage circuitry mainly the cathode 4 Use the emergency off only in an emergency situation with personnel injury 1 Depending on whether the EMO option is installed on your microscope or not operate the respective control element If the EMO option is installed press the EMO button on the top of the plinth If the EMO option is not installed set the MAIN switch at the rear side of the plin...

Page 93: ...is accomplished according to standardized maintenance plans and is recorded by the ZEISS service representative 7 2 Maintenance Intervals The maintenance intervals depend on the period of application of the device 24 hours 7 days a week semiannually 8 hours 5 days a week annually Info Keep track of maintenance work and contact the ZEISS service representative in time A list of ZEISS locations and ...

Page 94: ...ld emission gun filament 1 Yearly or as required and after exchange of field emission gun Multihole singlehole aperture Anode aperture Extractor aperture Anode aluminum seal Copper seal at gun head Yearly or as required Tip seal of the pre vacuum pump Yearly performance check SE detector InLens SE detector EsB detector As required approx 3000 µAh Ion source FIB apertures If used up Precursors 1 Th...

Page 95: ...urce may be used up 3000 μAh Contact the ZEISS service rep resentative to have the ion source replaced FIB No emission Ion source needs to be regen erated Refer to Regenerating the Ion Source by Heating 105 Ion source may be used up Contact the ZEISS service rep resentative to have the ion source replaced FIB No image Aperture position is not cor rect Initialize the FIB aperture in the FIB tab of ...

Page 96: ... Image is bad at low EHT e g 1 kV Working distance is too long Reduce the working distance to a maximum of 7 mm InLens image is noisy Working distance is too long Reduce the working distance No InLens image can be obtained EHT exceeds 20 kV Reduce EHT to a maximum of 20 kV Microscope is dead Circuit breaker is tripped lower position Refer to Checking the Position of the Circuit Breakers 103 Stored...

Page 97: ...isplayed Specimen or specimen holder has touched objective or wall of the specimen chamber Refer to Resetting the Touch Alarm 100 Vac ready OK is not displayed after specimen exchange System vacuum is bad due to a vacuum leak at the chamber door Check the chamber door seal for cleanliness If required refer to Replacing the Chamber Door Seal 100 Vac ready OK is dis played very late after specimen e...

Page 98: ...e plugged in correctly 3 If this does not help reset the workstation as described in the instruction manual of the mi croscope INFO If the problem persists contact your ZEISS service representative 8 3 Chamber 8 3 1 Initializing the Stage If a stored stage position cannot be approached or if the stage does not move or does not move accurately the stage needs to be initialized Prerequisite ü The sp...

Page 99: ...ove to opposite directions This is because the selected CCD camera is installed at a certain angle relative to the stage Thus the camera shows a side inverted view To remedy this you need to change the joy stick TV angle setting in the software Info If you are working with two CCD cameras The joystick TV angle can only be set for one CCD camera When selecting the other CCD camera you have to chang...

Page 100: ...OTICE Risk of property damage Contamination caused by fingerprints Contamination caused by fingerprints can lead to vacuum deterioration or prolonged pumping times 4 Always wear lint free gloves when touching the specimen specimen holder or stage 1 Carefully open the chamber door 2 On the inside of the chamber door remove the chamber door O ring NOTICE Risk of property damage If you use a metal to...

Page 101: ...akeout 101 Switching on the Gun 69 8 4 1 1 Switching off the Gun NOTICE Risk of property damage Schottky field emitter If the Schottky field emitter is switched on and off too frequently or inappropriately its lifetime is reduced 4 Avoid switching off the gun during the working week 4 Use Standby mode for the weekend or a break of up to a week 4 When using the Standby mode activate the Partial Ven...

Page 102: ...ng select Overnight For 43 hours heating 7 hours cooling select Weekend For a cycle defined by the operator select User 4 To start the bakeout procedure click Bakeout Start 8 4 2 Calibrating the Probe Current This function enables you to automatically calibrate the probe currents within a few minutes Calibrating the probe current can be necessary in the following cases Before performing analytical...

Page 103: ...uit breakers on the rear side of the plinth is tripped 2 If one of the circuit breakers is tripped push it upwards 8 6 Detectors 8 6 1 Lubricating the Rod The rod from the aSTEM BSD4 and VPSE detector mechanics needs to be lubricated once a year with TEM oil 300 Parts and Tools Designation Part no TEM oil 300 000000 0484 955 Isopropanol Lint free cloth Lint free gloves CAUTION Risk of injury TEM o...

Page 104: ...ive detector 2 Clean the rod with isopropanol with a clean lint free cloth 3 Spread some drops of TEM oil 300 across the rod Use a clean lint free cloth 8 7 Focused Ion Beam 8 7 1 Checking the Lifetime of the Ion Source The ion source is a consumable that is used up during operation In order to keep track of the ion supply the ion source lifetime needs to be checked regularly Info When the lifetim...

Page 105: ... Heating à The FIB Ga Source Heating window is displayed 2 Click Multi Heat à An automatic heating routine is performed 3 If the ion source still does not start emitting find a new extractor value Refer to Manually Finding a New Extractor Value 105 8 7 3 Manually Finding a New Extractor Value If emission still fails after performing the multi heating routine see Regenerating the Ion Source by Heat...

Page 106: ...urce in this condition for about 5 minutes adjust the extractor voltage if neces sary to keep the emission at 2 μA 10 Click Save Value 11 Deactivate the FIB Extractor Manual Override checkbox 12 Select the FIB tab 13 To enable the suppressor regulation activate the Regulate checkbox Info During the process of finding a new extractor target the FIB gun will be automatically switched to the On state...

Page 107: ...ioning body parts can be crushed 4 Maintain a safe distance 4 Do not walk or place your hands or feet under the load while it is being lowered 4 Wear safety shoes and gloves CAUTION Risk of injury or property damage GIS precursors If a gas injection system GIS is used the precursors may be explosive reactive toxic or irritant when they come into contact with the environment or a person 4 Do not re...

Page 108: ...n crates Microscope plinth Wrapped with recyclable polyethylene foil and shipped in a reusable wooden crate Dimensions and weight of crate 1450 1450 2200 mm W D H appr 1224 kg Microscope console and accessories Console valve damper monitors cables pipes etc are wrapped with recyclable polyethyl ene foil or packed in separate cartons and shipped in a reusable wooden crate Dimensions and weight of c...

Page 109: ... Disposal Schottky field emitter Tungsten ceramics Used up emitters may be re turned to the emitter manu facturer Apertures Platinum iridium gold Very small amounts May be disposed of in accordance with local regional regula tions Ion source gallium Gallium To be returned to ZEISS GIS Precursors For information regarding the disposal of precursors refer to the instruction manual of the GIS 9 3 2 D...

Page 110: ...ariable in 10 Volt steps Probe current SEM High Resolution configuration 5 pA to 20 nA High Current configuration 12 pA to 100 nA Magnification Range 12x to 2 000 000x SEM referenced to Polaroid image format Adjustment Continuously variable in either coarse or fine modes Auto Compensation Magnification is precisely corrected automati cally for changes in working distance or acceleration voltage El...

Page 111: ...aperture sizes 7 10 15 20 30 60 120 µm High Current configuration 6 aperture sizes 10 20 30 60 120 300 µm Electromagnetic selection precise alignment due to retrievable coordi nates Beam shift Control Adjustment with hardpanel or PC mouse For precise adjust ment of image position at high magnifications Width 200 µm 100 µm at 20 kV and WD 8 5 mm Focused Ion Beam Column Optional Parameter Descriptio...

Page 112: ...tions available via condenser lens Control Software control for automatic operation Specimen Chamber and Stage Parameter Description Specimen chamber dimensions 330 mm inner diameter 270 mm height Free accessory ports 18 for EDS EBSD SIMS manipulators etc Chamber Viewing Two color CCD cameras with IR and white light illumination provided as standard Analytical working distance 8 5 mm Coincidence p...

Page 113: ...detector channels and up to 3 TV inputs optional Any two detector signals can be mixed for enhanced image information TV Camera image and detector images can be displayed simultaneously InLens detectors InLens SE detector High efficiency annular scintillator detector mounted in GEMINI col umn with optically coupled photomultiplier EsB detector optional Column mounted high efficiency scintillator d...

Page 114: ...Chamber camera Color CCD camera with white light illumination and IR illumination Specimen current monitor 6 range auto ranging for precise current measurement in the range of 1 pA to 10 µA For more details refer to the document Product Specification 10 2 Installation Requirements For a complete list of the installation requirements refer to the document Installation Require ments Location Require...

Page 115: ... 3 7 kVA dependent on accessories Maximum current 16 A Circuit breaker at house installation 25 A type K Ampere interrupt ing capacity AIC Min 10 000 A rms Protective ground High leakage currents are present in the microscope Therefore the microscope has to be connected to an equipotential bonding bar An exclusive grounding connection to earth must be provided i e the grounding terminal must not b...

Page 116: ...ent Typical flow rate Approx 12 l min at 0 6 MPa pressure during air leveling system infla tion Pressure 0 6 0 8 MPa 6 8 bar Quality Oil free Connection hose 6 mm inside diameter 10 m are delivered with the microscope Environmental Requirements Parameter Requirement Ambient tempera ture Appr 21 4 C Stability of ambi ent temperature 0 5 C h For long running experiments Long term stability of ambien...

Page 117: ...than 52 dB 120 450 Hz less than 43 dB Above 450 Hz less than 47 dB 10 2 1 Layout and Connections A B C D E F G H I 1 2 3 4 1 Static vibration damper A Mains power supply 208 230 V 25 A L1 N L2 PE 2 Pre vacuum pump Equipotential bonding bar 3 Computer workplace Pressure reducer water nitrogen compressed air 4 Emergency Off EMO button optional Main shut off valves Water supply Water runback Nitrogen...

Page 118: ... Ion sculptor FIB 200 mm airlock 2 Table PC 3 Static damping block 4 Pre vacuum pump 5 FIB rack Description Size mm appr Distribution of load kg Footprints Plinth column Ion sculptor FIB 940 1070 1800 4 250 4 Ø 80 mm Plinth column Ion sculptor FIB 200 mm airlock 1080 1070 1800 4 260 4 Ø 80 mm Table PC 1650 1000 838 or 1100 1000 838 4 24 3 4 Ø 50 mm 118 Instruction Manual ZEISS Crossbeam 350 en US ...

Page 119: ...0 160 1 12 0 180 mm 180 mm Pre vacuum pump 432 265 295 1 24 5 200 mm 180 mm FIB rack 560 810 1600 4 50 on wheels Chiller optional water or air cooled 530 640 740 4 22 5 on wheels Compressor 281 139 239 1 25 0 281 mm 139 mm Actual measurements are country dependent different manufacturers Instruction Manual ZEISS Crossbeam 350 en US Rev 3 349500 8111 000 119 ...

Page 120: ...nciples for design EN 60204 1 2006 Safety of machinery Electrical equipment of machines Part 1 Gen eral requirements EN 61010 1 2010 Safety requirements for electrical equipment for measurement control and laboratory use EN 61326 1 2013 Electrical equipment for measurement control and laboratory use EMC requirements Part 1 General requirements Electrical Field The workstation is a class A device i...

Page 121: ...and consumables must be installed by a ZEISS service representative 11 1 Consumables Required Parts Tools Part Number Schottky field emitter gun by DENKA 000000 0302 460 Multihole aperture On request Anode aperture On request Extractor aperture 348520 0097 001 Anode aluminum seal 348520 0266 001 Copper seal gun head single use 000000 0546 290 Tip seal for pre vacuum pump BOC Edwards XDS 10 000000 ...

Page 122: ...s Tools Part Number Faraday cup 348342 8055 000 3 mm Allen key 000000 0015 247 1 5 mm Allen key 000000 0151 883 Small pliers Specimen holders Refer to specimen holder catalog Stubs Tweezers Lint free cloth Lint free gloves 122 Instruction Manual ZEISS Crossbeam 350 en US Rev 3 349500 8111 000 ...

Page 123: ...verhart Thornley 37 InLens SE 36 78 SE 37 79 SESI 42 82 STEM 85 VPSE 41 80 103 Detector mechanics Lubricating the rod 103 Detector settings 78 Disposal 107 Microscope 109 Solid waste 109 Dual joystick 40 E Electron optical column 30 Emergency off EMO option 18 Emergency shutdown 92 Emitter life 94 EsB detector 43 81 Everhart Thornley detector 37 Extractor voltage 76 F Faraday cup 75 FIB column 32 ...

Page 124: ...onnel 13 Resetting the touch alarm 100 S Safe operation condition 13 Safety 12 Safety equipment 17 Safety label 20 Safety procedure 13 Saving images 74 Scintillator 94 SE detector 37 79 Secondary electron 34 Secondary electrons secondary ions detector 42 Service 13 SESI detector 42 82 Shortcuts 62 Shutdown Emergency 92 Finishing the work session 90 Microscope 107 Signal detection 34 SmartFIB Progr...

Page 125: ...e plate 23 U User access level 54 User interface 52 User privilege 54 V Vacuum mode 88 High Vacuum HV 89 Variable Pressure VP 88 89 Vacuum system 26 Variable pressure 88 VPSE detector 41 80 103 Instruction Manual ZEISS Crossbeam 350 en US Rev 3 349500 8111 000Instruction Manual 125 ...

Page 126: ...rl Zeiss Promenade 10 07745 Jena Germany phone 49 1803 33 63 34 fax 49 3641 64 3439 info microscopy de zeiss com www zeiss com microscopy Instruction Manual ZEISS Crossbeam 350 en US Rev 3 Modifications reserved Printed in Germany ...

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