Leica EM ACE200 Manual
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Leica EM ACE200 Manual

Leica EM ACE200 Manual

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Important note
Please read this instruction manual carefully before operating the instrument. This user
manual is intended to provide essential information about the Leica EM ACE200
coating system. It includes important information regarding operation, servicing and
troubleshooting. Following these instructions will help to prevent hazards, reduce repair
and downtime costs and prolong the system's life.
Users must familiarize themselves with the system before operation. Particular
attention must be paid to the aspect of safety. The Leica EM ACE200 must not be used
beyond the limits specified in the technical data sheet.
When hazardous substances (e.g. radioactive, toxic or explosive substances) are
processed, the substance-specific safety precautions must be implemented. It is
forbidden to process substances that release corrosive or poisonous gases when they
are placed in vacuum and/or are coated.
Any warranty claims can only be considered when the instrument is used according to
the guideline given in this manual.
In addition, all generally applicable legal and otherwise binding regulations for
preventing accidents and protecting the environment must be observed and
communicated.
Leica reserves the right to change technical specifications as well as manufacturing
processes without prior notice. Only in this way is it possible to continuously improve
the technology and manufacturing techniques used to provide our customers with
excellent products.
Copyright of this document is retained by Leica Mikrosysteme GmbH, Vienna. Any
reproduction of text and illustrations (or any parts thereof) by printing, photocopying, or
other methods (including electronic systems and media) as well as handing over to
third parties requires approval of Leica Mikrosysteme GmbH.
Danger!
The Leica EM ACE200 coater system can be handled safely and
easily provided it is operated in accordance with the instructions in
this manual. Ignoring safety instructions may endanger people
and the system.
Seite 1 von 68

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Summary of Contents for Leica EM ACE200

  • Page 1 Users must familiarize themselves with the system before operation. Particular attention must be paid to the aspect of safety. The Leica EM ACE200 must not be used beyond the limits specified in the technical data sheet. When hazardous substances (e.g. radioactive, toxic or explosive substances) are processed, the substance-specific safety precautions must be implemented.
  • Page 2 Symbols used in this manual Danger! Instructions regarding possible hazards are identified with this symbol. Ignoring these alerts may result in serious injury! Users of the instrument must comply with instructions at all times. Caution! This symbol alerts the user to important information which may endanger staff or result in damage to the system if it is ignored.

  • Page 3: Table Of Contents

    Table of contents INTRODUCTION ......................5 1.1 Safety ............................... 6 1.2 Instrument Overview ........................8 INSTALLATION AND SET UP ..................9 2.1 Delivery of the instrument ....................... 9 2.2 Installation requirements ......................... 9 2.3 Unpacking and connection ......................10 2.4 Pump set-up ........................... 12 2.5 Shutter installation ........................
  • Page 4 5. TROUBLESHOOTING ...................... 61 5.1 Error messages – User self-assistance .................... 61 5.2 Malfunction ........................... 62 5.3 Error messages complete list – description for Leica service ............63 5.3.1 Carbon thread ..........................63 5.3.2 Sputtering ............................. 64 5.3.3 Low Vac Mainboard Controller ..................... 66 6.

  • Page 5: Introduction

    1.Introduction The Leica EM ACE200 coating system is used for precise coating of samples for subsequent examination with an electron microscope (EM). The optional glow discharge makes grids hydrophilic. Also optional are quartz crystal measurement to accurately determine the layer thickness and a planetary drive stage for even distribution of coating material.

  • Page 6: Safety

    The housing must not be opened except by an authorized Leica representative. If the Leica EM ACE200 coating system is damaged or malfunctions, all use of the system should be suspended until the malfunction or damage has been corrected.
  • Page 7  Repairs may only be made by Leica authorized service staff or authorized representatives.  If the Leica EM ACE200 coating system is installed incorrectly, the system may be damaged and may incur injury to the user. Emergency procedure...

  • Page 8: Instrument Overview

    1.2 Instrument Overview 1. Source cover 2. Source head (sputter or carbon thread) 3. Shutter 4. Chamber 5. Sample stage 6. Touch sensitive control panel 7. Adjustable feet 8. Chamber door 9. USB port 10. Outlet to vacuum pump 11. LAN connection (Inactive, for future connection) 12.

  • Page 9: Installation And Set Up

    The Leica ACE200 has to be set up on a stable laboratory workbench with a surface area of at least 660mm depth and 410mm width. The coater is 450 mm high.

  • Page 10: Unpacking And Connection

    2.3 Unpacking and connection The Leica EM ACE200 coating system should be transported with a forklift truck Remove bands and open box Fold down the sides of the box and remove vacuum hose (if ordered) Remove accessories box Lift out the unit by grasping underneath the...
  • Page 11 Place the ACE 200 on a stable bench Adjusted all feet and counter lock (flat spanner 13mm) to maintain level and stable positioning. Connect vacuum hose to the ACE200 Connect MAINS IN cable for rotary pump Connect MAINS OUT cable to rotary pump Connect mains cable For sputtering process only: Connect argon gas (6mm diameter)

  • Page 12: Pump Set-Up

    2.4 Pump set-up If a pump is not included, a roughing pump with a capacity of 5m /hour or higher and an ultimate vacuum of at least 5x10 mbar is needed. This has to be attached to the coater (KF 25 ISO flange, see picture below) If the delivered parts include a rotary vane pump please set up the pump as described below.
  • Page 13 A hose ordered with the instrument includes 1. A metal hose 2. Two clamps 3. Two seals With the oil pump (If ordered) you will get an oil mist filter, another clamp and a seal (like above). Install oil mist filter to rotary pump exhaust flange using the seal and clamp (see 3 and 2 above) Fill the pump with oil included in the pump...

  • Page 14: Shutter Installation

    2.5 Shutter installation Remove the shutter from the packaging  Shutter without the glow discharge electrode Thumb screw (1)  Shutter with a glow discharge electrode and contact (optional) Electrode plate (2) Glow discharge connection (3) Glow discharge cable (4) Screw the shutter into the hole in the middle of the rear of the coating chamber by the thumb screw...
  • Page 15 If a glow discharge is present guide the cable through the recesses on the shutter (1) and plug in the connection (2) Slide the shutter spring (1) on to the pin on the shutter (2) Page 15 of 68...

  • Page 16: Stage Installation

    2.6 Stage installation The coater is delivered with a stage to hold up to 18 SEM stubs. Optional stages for a glass slide or a planetary drive stage are available. This stage is used for loading up to 18 standard 1/2” SEM stubs with a pin diameter of 3.2mm This optional stage is used for one 76mm x 26mm (3”...
  • Page 17 Take the rod and place it as shown in the coating chamber Place the stage on the rod (stub, glass slide or planetary) Tighten the thumb screw To remove a stage, reverse the above procedure Adjust the height to the desired level and tighten the thumb screw (see also 2.4.2) Page 17 of 68...

  • Page 18: Planetary Drive Stage

    The vacuum chamber equipped with a sample stage (1) a shutter (2) a glow discharge electrode (3) and a thickness measurement quartz (4) 2.6.1 Planetary drive stage The planetary stage is an optional outfit. When ordered, the instrument is outfitted with the necessary feed-through and motor control.
  • Page 19 Place the planetary drive stage on the vertical rod and fasten it by tightening the thumb screw When placing the x4 SEM stub holder take care to align the undelaying pin into the hole in the sprocket. This can be easily done by turning the stub holder till it drops into place Installed planetary drive stage Page 19 of 68...

  • Page 20: Setting The Stage Height

    2.6.2 Setting the stage height On the defined zero reference mark (lower reference pin) the distance to the target is 30mm. Grooves of 10mm distance on the rod allow an accurate setting of the sample height. Upper reference pin: Pin aligned with table/sample surface is the minimum distance from source (30mm, correction input for quartz 20mm)

  • Page 21: Quartz Crystal Measurement Installation

    2.7 Quartz crystal measurement installation The quartz crystal measurement (QSG) is an optional feature for accurately determining the thickness of the applied coating layer (see further 3.7). The QSG equipment for installation includes 1. Quartz head with cable 2. Holder 3.
  • Page 22 Replace the cover and tighten gently Place the quartz holder into the adapter block by sliding it in, the quartz head on top and the cable on the bottom In the rear left of the coating chamber are two pins to receive the quartz holder Place the quartz holder block into coating chamber by push sliding it onto the two pins Page 22 of 68...
  • Page 23 Connect the plug of quartz measuring cable to the feed through in the rear right of the coating chamber For better access the sample stage can be removed Replace the sample stage (see 2.6) Page 23 of 68...

  • Page 24: Operation

    3.Operation 3.1 Touch screen control panel The LCD control panel is used for communicating with the Leica EM ACE200 coating system as well as for data input and output. The parameters for the coating process are edited via the touch screen.

  • Page 25: Settings

    Software updates can be performed (by the user) and the service interface accessed (by Leica service). 1. Time until a panel will close automatically 2.
  • Page 26 screen (only if needed) 4. Set system time 5. Set volume To confirm press The coater is delivered calibrated. If the touch seems to loose it‟s accuracy calibrate the screen (see 3.1.1) Connect a USB stick to the port on the touch screen panel and select „Log file‟...

  • Page 27: Pump And Vent

    Enter the menu, connect a USB stick to the port on the touch screen panel (see 3.1.3,) and press update Choose from the list which updates shall be performed by pushing the respective button on the select update column It is recommended to first update the user interface and then the controller update 3.3 Pump and Vent...

  • Page 28: Vacuum Test

    pumping cycle will not start and an error message will appear. A time out message shows if there is a leak when pumping down (e.g. the source is not placed correctly). Pump and vent buttons The vacuum level is visualised using a vacuum bar Tapping on the vacuum bar will show the vacuum read out...
  • Page 29 Select any of the processes Screen shows instrument equipped with three processes Push the pump button to start pumping down.  When tapping on the pressure bar the current vacuum will be displayed If the vacuum does not reach 0.5 mbar after 30s, the pump has to be checked or a vacuum leak needs to be found.

  • Page 30: Process Start And Stop

    3.5 Process start and stop The coating process can be started at any time (system evacuated or not) as long as the door and source cover are closed (electronic safety switches prohibit starting with open door or source cover) and the source is connected. The button will turn into a button when the system starts the coating cycle.

  • Page 31: Thickness Monitoring And Geometrical Correction (Qsg)

    Venting is done manually by pushing the “Vent” button 3.7 Thickness monitoring and geometrical correction (QSG) A quartz crystal oscillates at a certain frequency. Coated with a material, this frequency reduces according to the material and the applied thickness. With this information the accurate film thickness coated during a process run can be determined.
  • Page 32 The frequency of a new crystal is ~6 MHz and should be stable In this case the system will terminate after a set thickness. In this case the system will terminate after a set number of pulses or flashes for carbon coating or time for metal sputtering and the achieved thickness will be measured and...

  • Page 33: Carbon Thread Coating

    When the sample surface is below the 0 reference mark the height correction number is set to the appropriate negative value. 3.8 Carbon thread coating The carbon coating process is carried out by evaporating a carbon thread. It is possible to coat using short pulses of 150 milliseconds or evaporating the thread completely with maximum power, a so-called flash.

  • Page 34: Loading A Carbon Thread

    3.8.1 Loading a carbon thread The carbon thread can be loaded as a single thread or as a double thread. Thin layers from 1to at least 20 nm can be achieved (there is variance in threads). To minimize carbon thread waste, when loading a double thread, cut a piece of thread twice as long as the width of the black door .
  • Page 35 Remove any carbon thread residue using the brush supplied Loop the carbon thread around the first clamp and pull both ends gently to the left At the same time tighten the screw as shown in the picture Wind the thread around the other clamps Take care that the thread slides into the clamping groove (1) follow the path: Page 35 of 68...
  • Page 36 Pull the thread gently and tighten the last clamp Tighten the remaining 3 screws and trim thread on both ends If all screws are not tightened the instrument may not recognize the thread section Clean the sealing surface with a lint-free tissue There is an ACE200 youtube video where the loading of the...

  • Page 37: Setting Up A Carbon Thread Process

    3.8.2 Setting up a carbon thread process When the head is inserted after completing the preparation in 3.8.1, an evaporation process can be run. Turn on the mains switch on the rear of the unit. Start screen will appear Press on Press pump button to start pumping If the chamber door is not closed, an error message will indicate it...

  • Page 38: Selecting The Thread Type

    3.8.3 Selecting the thread type Push to open the drop down menu and select thread (thread 2 is a double thread) The instrument automatically chooses the correct parameter settings 3.8.4 Pulse mode When using the pulse mode the process can be terminated according to the desired coating thickness (quartz needs to be available) or a set number of pulses.

  • Page 39: Flash Mode

    3.8.5 Flash mode When using the flash mode the process is terminated after the selected number of carbon thread sections has been evaporated. If a QSG is available the resulting thickness can be shown. For QSG setting please refer to 3.7. Select Using the flash mode, the process is defined by the number of flashes (1-4)
  • Page 40 If not sufficient threads are available a warning will be shown. If no threads are available a warning is shown. Pumping to 5x10 mbar Measuring the threads Pumping to base vacuum 3x10 mbar Page 40 of 68...
  • Page 41 Degassing the threads Each thread is degassed separately before it is used. The system waits after outgassing to stabilize the vacuum Coating in progress Number of pulses (1) performed and present thickness are displayed (2) Coating is finished, the report summary indicates the number of pulses/flashes and (if quartz crystal measurement is available) the deposited thickness in nm...

  • Page 42: Sputter Coating

    3.9 Sputter coating Sputter coating is performed using ionized argon to create a plasma. The argon ions are accelerated by high voltage and directed towards the source via a magnet where they collide with the target and displace surface atoms. Due to this collision the surface atoms are directed towards the area below the target and coat the sample.

  • Page 43: Loading The Sputter Target

    3.9.1 Loading the sputter target Make sure the instrument is vented (see 3.3) and open the source cover Unplug the connectors Unscrew the 2 sputter head screws to remove the flange Remove the bayonet ring by turning and insert the sputter target Fix target by gently tightening the bayonet ring.

  • Page 44: Setting Up A Sputtering Process

    Tighten the ring by hand only. When the target is secured replace the sputter head, gently tighten the fastening screws and connect the cable and close the cover There is an ACE200 youtube video which also shows the loading of the target http://www.youtube.com/watch?v=y Kd1IyKIDT8 3.9.2 Setting up a sputtering process...

  • Page 45: Selecting The Material

    If the chamber door is not closed, an error message will be shown. While the system pumps down to 3x10 mbar all process parameters can be set: 1. Target material 2. Process: directional or diffuse 3. Process termination 4. Stage height from defined “0” position (only for QSG, see 2.6.2) 5.

  • Page 46: Diffuse Mode

    3.9.5 Diffuse mode The diffuse mode is intended for more topographic samples. The vacuum for diffuse sputtering is 8x10 mbar. Select diffuse 3.9.6 Sputter current and purge cycles Different targets require different sputter currents. A recommended value is pre-set when the target is chosen (see 3.9.3). The vacuum chamber can be purged with argon. Press to open the panel to adjust the number of purge cycles with argon and to...
  • Page 47 Quartz measurement is activated Height adjustment for the correct quartz tooling factor For quartz details refer to 3.7 Termination by time Quartz measures the achieved thickness No quartz available, termination by time Page 47 of 68...

  • Page 48: Running The Sputtering Process

    3.9.8 Running the sputtering process After setting the parameters as described in 3.9.2 - 3.9.5 , the process can be run by pressing the … … which will turn into a button If the door is not closed an error message will be shown.
  • Page 49 If the sputter head cover is not closed the an error message will be shown. Preparing vacuum level to purge with argon (5x10 mbar) Purging the chamber with argon (number of cycle sis displayed) Pumping down to base vacuum (2x10 mbar) Page 49 of 68...
  • Page 50 Stabilizing argon flow to reach the process vacuum (in this example 4x10 mbar for directional mode) Starting pre-sputtering to clean the target and stabilize parameters Opens the shutter and start sputter coating Current coated thickness Hint, in case process vacuum cannot stabilize check if the argon valve on the bottle is open Page 50 of 68...
  • Page 51 Coating is finished, the report summary Replace image - this is for carbon shows the coating time and (if quartz crystal measurement is available) the achieved layer thickness If starting a new coating without venting the total layer thickness accumulates, therefore the display shows the total thickness.

  • Page 52: Glow Discharge

    3.10 Glow discharge The glow discharge is an optional process which is used mainly to make TEM grids hydrophilic. Air is used to create plasma. This process can also be used to clean the sample surface before coating. After setting the glow discharge parameters the system will perform the following steps automatically.

  • Page 53: Planetary Drive Stage

    3.11 Planetary drive stage The optional planetary drive stage is useful for coating highly topographic or fissured samples. After installing the planetary drive stage as described in section 2.5.1 the rotation function can be used. The Rotation button is found on the bottom row of the main operating screen (choose on the main...

  • Page 54: Switching Between Processes

    3.12 Switching between processes A coater equipped with several options such as sputter coating, carbon thread evaporation or glow discharge can be easily switched form one process to the other. This is done by exchanging the source and choosing the desired process from the main screen.

  • Page 55: Maintenance And Service

    Provide a standard maintenance schedule  Deal with malfunctions Malfunctions during operation of the Leica EM ACE200 coating system are reported in an information window. A clear text error message provides information about the cause of the malfunction and the action required.

  • Page 56: Vacuum Pump

    If contamination is observed during EM imaging  Pumping time to reach base vacuum increases significantly Extensive cleaning and parameter check is recommended once a year by a trained Leica service engineer to ensure flawless operation. Page 56 of 68...
  • Page 57 Recommendation Usually, only the glass door needs to be cleaned, depending on the layer thickness and your visibility needs. The chamber shielding, especially when always using the same material, does not need to be cleaned very often. Cleaning material Any abrasive works well such as scotch-brite or metal cleaning paste. Washing the parts afterwards with soapy water and letting them dry off is an easy way to finish the cleaning.

  • Page 58: Removing Shutter And Internal Shielding

     The glow discharge electrode is available as a spare part. One extra spare is supplied with the system Housing  All surfaces can be cleaned with a damp, lint-free cloth moistened with either aqueous cleaning agents or 50% ethanol (ethanol - water 1:1) NOT use ACETONE! ...
  • Page 59 Remove the shutter retaining spring If the instrument is configured with glow discharge, disconnect the push-in connector in the upper left side of the chamber before removing the shutter Unscrew the shutter thumb screw and take out the shutter assembly Caution! There is danger from the edges of the metal sheet of the internal...

  • Page 60: Removing The Door

    Remove the internal shielding by holding it on the side with the small handles and pulling it out To install shielding and shutter, reverse the above procedure. 4.2.2 Removing the door To remove the door lift up the door and take it out Place it flat on a soft surface to clean The complete glass can be exchanged by unscrewing both...

  • Page 61: Troubleshooting

    5. Troubleshooting 5.1 Error messages – User self-assistance Error text SOURCE x SHORT-CIRCUIT Possible cause Short circuit in head caused by extensive coating Remedy For the sputter head: Take off the head from the system and remove the target Clean the ring that holds the target in place Clean the head surface from deposition layer Clean the area in the chamber that is around the sputter head For the carbon thread head:...

  • Page 62: Malfunction

    5.2 Malfunction Malfunction System does not start when switched on Cause The cable is not connected to the mains power supply Remedy Connect to the mains power supply Pump does not start when pressing “Pump” or “Start” Malfunction Cause 1 Fuse on the rear of the coater popped out Press “Stop”...

  • Page 63: Error Messages Complete List - Description For Leica Service

    5.3 Error messages complete list – description for Leica service 5.3.1 Carbon thread Warning or Error number with Text on the screen description W4000 "W4001" Warning No threads available, cancel only after Threads available measurement of resistor. CANCEL W4002 "W4002" ...no threads left for the...

  • Page 64: Sputtering

    5.3.2 Sputtering Text on the screen Warning or Error number with description E2001 "E2001" ..HV-Board is not Process supplied with voltage door or Sputtering terminated cover sensor could be the Mains supply voltage fault. reason. Check door and cover E2002 "E2002"...
  • Page 65 E2009 "E2009" ..Sputtering Process terminated. Short circuit in Sputtering terminated sputter head, ring or target is Sputter source short circuit not placed correctly or material Check target and sputter source deposition on the shutter. E2010 "E2010" ..Sputtering Process terminated plasma was not Ignition fault ignited, possible reason is Check argon flow...

  • Page 66: Low Vac Mainboard Controller

    5.3.3 Low Vac Mainboard Controller Text on the screen Warning or Error number with description E1001 "E1001"..Shutter motor is not Shutter motor connected to board. Motor is not connected. Please contact service on the Service Screen E1001 Shutter Motor Motor is not connected Please check cable X20 at board 661531106...

  • Page 67: Servicing And Repair

    6. Servicing and repair The Leica EM ACE200 is covered by a WARRANTY according to the conditions of sale. If functional errors should occur or if the components of the system sustain damage that is subject to warranty coverage during the warranty period, the manufacturer will repair or replace the faulty components following examination thereof.

  • Page 68: Attachments

    7. Attachments 7.1 Technical data sheet 7.2 EC declaration Page 68 of 68...

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