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Gatan 600 DUOMILL Instruction Manual

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Summary of Contents for Gatan 600 DUOMILL

  • Page 1 sales@artisantg.com artisantg.com (217) 352-9330 | Visit our website - Click HERE...
  • Page 2 Serial Number _____________________ MODEL 600 DUOMILL INSTRUCTION MANUAL Gatan Inc. (USA) Gatan Online Gatan GmbH (Germany) Gatan (Singapore) Tel: 925 463 0200 http://www.gatan.com Tel: 089 352 374 Tel: 65 235 0995 Fax: 925 463 0204 info@gatan.com Fax: 089 359 1642 Fax: 65 235 8869 Gatan Inc.
  • Page 3 Part number: 600.82001...
  • Page 4 Used to highlight advice directed at getting the best perfor- mance from the equipment. Copyright, Trademarks, and Patents © Gatan, the Gatan logo is registered to Gatan, Inc. The product names DuoMill and Whisperlok are trademarks belonging to Gatan, Inc.

  • Page 6: Table Of Contents

    Table of Contents 1. GENERAL DESCRIPTION 1 1.1 Main Work Chamber 1 1.2 Gas Control System 1 1.3 Vacuum System 1 1.4 Electrical System 1 2. INTRODUCTION TO ION MILLING 3 2.1 Factors Influencing Sputtering Rates 3 2.2 Ion Current and Specimen Thinning Rate 4 3.
  • Page 7 6.5.2 Operating Procedure 17 6.5.3 EGC Balance Procedure 17 6.5.4EGC Functional Setup Procedure 18 6.5.5 Switching off the Ion Beams 18 6.6 Chemical Milling 18 6.6.1 Installation of the CAIBE System 19 6.6.2 Loading the Chemical Source into the CAIBE System 19 6.6.3 Operation of the CAIBE System 19 6.7 Digital Process Timer 20 6.8 Sector Speed Control (SSC) 20...

  • Page 8: General Description

    1. GENERAL DESCRIPTION The Models 600DDM/600CDDM DuoMill™ are instruments that can simultaneously ion mill two independent specimens for transmission electron microscopy (TEM). The DuoMills are protected by US patent 4272682. This Guide pertains to both DuoMill models. Each DuoMill contains four subassemblies: •...
  • Page 9 Each Whisperlok contains a specimen height-sensing switch that automatically shuts off power to the high-voltage supply and gas to the ion guns if the specimen is raised into the Airlock. The high-voltage supply to each pair of ion guns is con- trolled by two potentiometers mounted on the sloping front panels.

  • Page 10: Introduction To Ion Milling

    2. INTRODUCTION TO ION MILLING 2.1 Factors Influencing Sputtering Rates The primary factors influencing the sputtering rate are: • The flux and velocity of the incident particles, i.e., ions and neutrals. • The angle of incidence of the sputtering beam. •...

  • Page 11: Ion Current And Specimen Thinning Rate

    2.2 Ion Current and Specimen Thinning Rate The sputtering performance of commercially available ion mills is often related to the so-called ion current picked up either by the specimen or by a removable current sensor (see Figure 2.2a). This practice is unfortunate because it not only neglects to take into consideration the sputtering power of the energetic neutrals, but it also fails to recognize that the cur- rent actually measured is not the true ion current.

  • Page 12: Installation Procedure

    No decrease in the pressure reading should be visible during a period of 2 min after closing the main valve. Plug the DuoMill into a grounded AC power outlet having the voltage designated on the Gatan label located on the right side of the cabinet.
  • Page 13 January 1999, Rev. 1...

  • Page 14: Operating Instructions (Short Form)

    4. OPERATING INSTRUCTIONS (short form) 4.1 Pre-Start-Up Check List Switch A should be off, i.e., depress lower face of switch. Raise the main circuit breaker (right side of cabinet). Check that the argon pressure is set at 8 psig (0.55 bar). Set the red pointer of the thermocouple gauge to the far right position.

  • Page 15: Switching On The Ion Beams - Voltage And Current Regulated Mode

    Turn Current Limit knob fully clockwise. Turn High Voltage knob clockwise to desired voltage (not above 4 kV for low-energy guns). Adjust Gas Flow knob (needle valve) to give desired current (usually 0.5 mA). Turn High Voltage Selector knob to Red position. Turn on Gas Control switch for Red gun.

  • Page 16: Detailed Operating Instructions

    5. DETAILED OPERATING INSTRUCTIONS 5.1 Pre-Start-Up Check List Both High Voltage switches (sloping front panels) should be off. (Depress bottom part of rocker switches). Both Voltage Control knobs (sloping front panels) should be turned fully counterclockwise. Rotate both High Voltage Selector knobs (front of the main chamber) to their neutral positions (unmarked position on knob).

  • Page 17: Milling Modes

    Since these adjustments can be bothersome, Gatan has developed an Electronic Gas-flow Control (EGC) that constantly monitors the gun current and automatically adjusts the gas supply to obtain a constant, pre-selected specimen current. Thus, the DuoMill now becomes both current and voltage stabilized, ensuring accurate reproducible milling conditions without constant attention.

  • Page 18: Changing Cathode Hole Positions In The Octoguns

    Turn High Voltage knob clockwise to desired voltage (not above 4 kV if using low-energy guns). Adjust Gas Flow knob to give desired current (usually 0.5 mA). Turn High Voltage Selector knob to Red position. Turn on Gas Control switch to Red gun. Adjust Gas Flow knob to obtain desired current (0.5 mA).
  • Page 19 Raise both specimen holders into their Airlocks. Rotate both High Voltage selector knobs to their neutral positions. Turn off Switch A if the DuoMill is not going to be used for more than a few days. Both the diaphragm pump and MDP will stop and the MDP will automatically vent.

  • Page 20: Operation Of Accessories

    6. OPERATION OF ACCESSORIES 6.1 Dual AutoTerminators WARNING : Do not stare directly into the laser assembly . Always point the laser away from the eyes and close the shutter when the laser is not in use. The laser uses high voltages that can be lethal. Disconnect power before servicing the laser power supply.

  • Page 21: Operating Procedure

    Adjust the sensitivity control to produce a reading of 150 on the digital meter. If this reading varies by more than 10% during one revolution of the specimen rotate motor, the laser requires alignment (see Section 6.1.5). Close the shutter of the laser assembly. Switch off the TERM switch, remove the assembly from the Airlock cap- sule and place it on top of the laser control unit.

  • Page 22: Removing The Laser Autoterminator

    Transparent/Translucent Specimens Place the optical filter on the specimen capsule-viewing window (see Figure 6.1b). Determine the setting of the sensitivity control that just causes the Trip light to come on when there is no specimen in the specimen holder. This position marks the maximum allowable counterclockwise setting of the sensitivity control.

  • Page 23: Installation

    milling, the heating effect of the beams at maximum intensity will raise the specimen temperature to as much as -90°C. Beam heating can be minimized by (a) using a low beam voltage and current, (b) ensuring good thermal contact between the specimen and the specimen holder, and (c) ensuring good thermal contact between the specimen holder and the Whis- perlok piston.

  • Page 24: Liquid Nitrogen Cold Trap

    vertically oriented photoresistor mounted in the path of the reflected beam. The signal detected by the photoresistor will fluctuate as the specimen rod and mirror rotate. This makes no difference to the AutoTerminator operation when thinning opaque specimens. However, with transparent specimens, the trip point must be set carefully to the maximum value of the oscillating signal.

  • Page 25: 4Egc Functional Setup Procedure

    Lift the EGC from its compartment and rotate it slightly allowing it to rest on top of the cabinet platform. Connect a digital voltmeter (DVM) (range 50 VDC) between TP1 and the ground pin (see Figure 6.5a). Turn on the White switch and follow Steps d through j of Section 6.5.2 above on the WHITE gun only. Record the voltage measured.

  • Page 26: Installation Of The Caibe System

    CAUTION : The Liquid Nitrogen Cold Trap must not be used to trap the reactive gases during operation of the CAIBE option since trapped gases may be released more quickly than can be handled by the chemical pumping system when the Cold Trap is allowed to warm to room temperature.

  • Page 27: Digital Process Timer

    that the chemical jet will be directed onto the specimen. Also, specimens are kept cleaner because contamination by secondary sputtering of reactants from the specimen mount is avoided. Finally, specimens can be thinned at much lower angles, thereby reducing radiation damage and creating larger thin areas. The disadvantage of the support post is that it does not allow two-sided milling.

  • Page 28: 1Operating Procedure

    tor. Both versions incorporate a DC motor to rotate the specimen at two different angular speeds: 2 rpm in the selected sec- tor (Φ) and 10 rpm outside it. Additionally, continuous rotation at either of the two speeds is available (see Figure 6.8b for circuit diagram).
  • Page 29 January 1999, Rev. 1...

  • Page 30: Routine Maintenance And Servicing

    7. ROUTINE MAINTENANCE AND SERVICING 7.1 Cleaning the Airlock Capsule Viewing Window After ion milling, raise the specimen into the Airlock and vent. Remove the capsule and push out the viewing window. Check capsule O-rings and if necessary clean or replace. Flip and replace the window so that the dirty side is exposed to atmosphere.

  • Page 31: Changing Cathodes And Insulators

    Remove and clean the small window. Remove any dirt from the window O-ring seal and the aperture tube. Remove and clean the upper O-ring Lubricate both O-rings, assemble them along with the window and screw the retaining cap on lightly; then screw the assembly back into the Airlock piston.

  • Page 32: Argon Gas Leaks

    Tools required: Allen wrenches (1.5 mm) & (3.0 mm), open end wrench (7.0 mm), and locking ring or snap ring pliers. NOTE: The anode, igniter, and O-ring are consumable items and must eventually be replaced. Disassembly Unplug the connector from the gauge tube by first unscrewing the retaining screw at the center of the connector. Remove the gauge tube by pulling it straight out from its chamber.

  • Page 33: Vacuum System Maintenance

    assembly is vented to atmosphere through the valves, allowing the piston to rise into the Airlock. Should the valve seats become dirty or defective, SV2 or SV3 may not seal properly when de-energized and cause argon to leak from the tank. Leak Detection Locate the gas-distribution assemblies behind the cabinet doors in the upper left and right hand corners.

  • Page 34: Routine Maintenance Schedule

    Recharging the Chemical Filter Shut down the DuoMill and vent the system. Remove the filter by uncoupling the KF flanges, one at its output to the flexible hose and the other at the input to the viewing tube. In a well-ventilated area, empty the contaminated activated carbon into a Zip-Loc storage bag and refill the canis- ter with a new charge.
  • Page 35 January 1999, Rev. 1...

  • Page 36: Spare Parts List

    8. SPARE PARTS LIST 8.1 Specimen Holders Standard specimen holder 600.380A2 (2.3mm) 600.380A3 (3mm) Cold style specimen holder 600.380B2 (2.3mm) 600.380B3 (3mm) Room temp holder for cold stage(1) 600.380C2 (2.3mm) 600.380C3 (3mm) Specimen support plates Molybdenum (Set of 5) 600.38211 (3mm) 600.38212 (2.3mm) Specimen clamping plates Molybdenum (Set of 5) 600.38221 (3mm)

  • Page 37: Auto-Terminator (Model 600.32000)

    8.5 Auto-terminator (Model 600.32000) Replacement laser tube 05486 Optical filter 600.32060.0 8.6 Cold-Cathode Gauge (Model 600.22000) Gauge tube repair kit 600.22160 NOTE: Please have your serial # available when ordering. 8.7 Gas Distribution Assembly (Model 600.07000) 3-way solenoid valve 03564 Solenoid valve coil 115 V 03501 Solenoid valve coil 230 V...
  • Page 38 SECTOR SPEED CONTROL WHISPERLOK ASSEMBLY PORTS FOR WHISPERLOK 1. airlock evacuate MOLECULAR 2. raise/lower gas DRAG PUMP 3. airlock vent Side View gatan 9/98 Figure 1.1 Main Work Chamber GAS IN 8 PSIG (.55BAR) MICROMETER AIRLOCK CAPSULE NEEDLE VALVE NEEDLE VALVE...
  • Page 39 (SV2 & AC NEUTRAL) (SV3 & AC NEUTRAL) FLOW RESTRICTING ORIFICE VENT VALVE THERMOCOUPLE GAUGE TUBE CHEMICAL FILTER SUPPLIED ONLY ON CHEMICAL MODELS DIAPHRAGM PUMP 31Mar, 1999 gatan 3/99 Figure 1.3 Model 600 Dual Ion Mill Vacuum System January 1999, Rev. 1...
  • Page 40 TMP READY LIGHT COLD CATHODE GAUGE T/C GAUGE RELAY 2A/115VAC 1A/230VAC DIGITAL PROCESS TIMER (See Figure 1.4c) Output to left and right ion beam controls Live Neutral Figure 1.4a Vacuum Control Unit - Model 600 DDM 9/98 gatan January 1999, Rev. 1...
  • Page 41 VOLTAGE LIMIT -5V Reference 5 Gun Voltage 6 ION GUNS ROTARY SPECIMEN HV SWITCH µA SPECIMEN CONTACTING TERMINAL CURRENT NON-CONTACTING TERMINAL 10 Sept, 1998 Figure 1.4b Circuit diagram - Model 600 Ion beam control gatan 9/98 January 1999, Rev. 1...
  • Page 42 11 Sept, 1998 Figure 1.4c Model 600 DDM Wiring Diagram 10/91 gatan January 1999, Rev. 1...
  • Page 43 Material: Copper Gun Current: 0.5mA Beam Angle: 20° Gun Voltage (kV) gatan Figure 2.1a Typical Thinning Rate for Copper in Range 4-11kV 1/86 9 kilovolts 1 mA (total current) ION BEAM SPECIMEN Beam Angle (degrees) 14Aug,1990 Figure 2.1b Specimen Current versus Beam Angle for Copper...
  • Page 44 ION GUN specimen ION GUN Figure 2.2a Ammeters in these Circuits do not measure Ion Current gatan 1/86 IONS FARADAY CAGE electrons TARGET Secondary ion and electrons must be collected and returned to ground through ammeter...
  • Page 45 AUSTRIA FINLAND GERMANY NORWAY BELGIUM FRANCE NETHERLANDS SWEDEN U.S. CANADA JAPAN gatan 6/85 FIG 3.1a Plugs supplied with the Model 600 DuoMill MAIN POWER BREAKER AUTOTERMINATOR SOCKET 40" (1016mm) ARGON IN 20" (508mm) 41" (1035mm) 16.25" (420mm) 2.5" (65mm) 16.0"...
  • Page 46 06225 600.05160.0 WINDOW SIZE-026 SPUTTER SHIELD CAPSULE SIZE-120 SIZE-224 600.05320.0 SPUTTER SHIELD SIZE-154 600.05150.0 SIZE-117 TOP PLATE TOP VIEW OF SPUTTER SHIELD Front of the DuoMill™ TO SEE ION BEAMS DURING OPERATION ORIENT SPUTTER SHIELD THIS WAY 11 Sept, 1998 9/98 Sputter Shield Figure 5.3...
  • Page 47 LEFT GUNS Start Finish Remarks Name Date RIGHT GUNS Start Finish Remarks Name Date 11Jan, 1989 gatan Figure 5.5 Record of Octogun Use 1/86 January 1999, Rev. 1...
  • Page 48 RIGHT DIGITAL DIGITAL METER METER RESET RESET SENSITIVITY SENSITIVITY CONTROL CONTROL CR14 CR13 CR15 CR16 GREEN GREEN TRIP OPERATE OPERATE TRIP SWITCH PC BOARD 11 Sept, 1998 gatan Figure 6.1a Dual Laser AutoTerminator Circuit Diagram 9/98 January 1999, Rev. 1...
  • Page 49 LASER SHUTTER SHOWN IN CLOSED POSITION . ROTATE 90° TO OPEN ALIGNMENT SCREW (x4) LOCKING SCREW (x4) LASER SUPPORT BASE MOUNTING NUT OPTICAL FILTER 600.32060.0 11 Sept, 1998 gatan Figure 6.1b Laser Head Assembly (600.32000.0) 9/98 January 1999, Rev. 1...
  • Page 50 SPECIMEN MOUNT FOR LIQUID NITROGEN TEMPERATURE (OPTIONAL ITEM) COMPRESSION NUT BRASS FLEXIBLE COPPER BRAID 600.5115C.0 SINGLE SIDED LOW ANGLE SPECIMEN MOUNT FOR ROOM TEMPERATURE (OPTIONAL ITEM) 11 Sept, 1998 gatan 9/98 Figure 6.2a Model 600.48003,600.48004 Liquid Nitrogen Cold Stage January 1999, Rev. 1...
  • Page 51 MIRROR DEFLECTS LIGHT FROM LASER ONTO EVACUATED STAINLESS PHOTO RESISTOR ONCE PER REVOLUTION STEEL JACKET ALUMINUM CONDUCTOR COMPRESSION NUT ALIGNMENT MARKS LEFT HAND THREAD FLEXIBLE COPPER BRAID 11 Sept, 1998 Figure 6.2b Cold Stage Auto-terminator Mirror Mount gatan 9/98 January 1999, Rev. 1...
  • Page 52 UNDERSIDE OF MAIN WORK CHAMBER DO NOT REMOVE SOCKET HEAD SCREWS VENT MAIN CHAMBER ROTATE WHISPERLOK™ CLOCKWISE 15° AND PULL ASSEMBLY STRAIGHT DOWN 14 Sept, 1998 gatan Figure 6.2c Whisperlok™ removal 9/98 January 1999, Rev. 1...
  • Page 53 First, close down and vent the ion mill as described in Section 5.8 and then pry up the cover to the central port and replace it with the cold trap. 11 Sept, 1998 gatan 9/98 Figure 6.3 Model 600.35000 Liquid Nitrogen Cold Trap...
  • Page 54 ADJUSTABLE FIXED EYEPIECE EYEPIECE FOCUS KNOB REFLECTOR TO REMOVE LAMP (08323) SLIDE OFF REFLECTOR AND UNPLUG LAMP. AIRLOCK CAPSULE 11 Sept, 1998 Figure 6.4 Model 600.36500 Microscope with Built-in Illuminator gatan 9/98 January 1999, Rev. 1...
  • Page 55 ASTERISK* INDICATES ITEMS ON 115 VAC UNITS - OMIT JUMPER J3 THE UPPER PCB OF THE CONTROL 230VAC UNITS - OMIT JUMPERS J1, J2 11 Sept, 1998 gatan 9/98 Figure 6.5a Circuit of the Electronic Gas Flow Control Unit January 1999, Rev. 1...
  • Page 56 RED GUN WHITE GUN Electronic Gas Flow Control FROM GAS OUTLET OF PRESSURE REGULATOR GROUND K25U 685M RED VALVE WHITE VALVE ADJUST KNOB ADJUST KNOB gatan 9/98 Figure 6.5b Model 600.21000, 600.21001 Electronic gas flow control January 1999, Rev. 1...
  • Page 57 Subject to US Patent application OCTOGUN MOUNT RETRACTION LIMIT SCREW VITON (SIZE-006) VALVE FAST VITON CHEMICAL NEUTRAL (SIZE-111) BEAM SPECIMEN SPECIMEN POST 600.51161.0 VITON (SIZE-010) SPECIMEN MOUNT BASE 600.5115A.0 PROTECTOR 600.5115C.0 CHEMICAL VITON SOURCE (SIZE-032) RAISE/LOWER PISTON CAUTION: USE ONLY VITON O-RINGS. DO NOT APPLY VACUUM GREASE TO VALVE SEAL (-006). LATCH JET ASSEMBLY IN THE RETRACTED POSITION BEFORE RAISING SPECIMEN INTO THE AIRLOCK.
  • Page 58 SPECIMEN MUST BE ORIENTED SO OF SINGLE SLOW SPEED SECTOR THAT GLUE LINE IS PARALLEL IN LINE WITH REAR ION BEAM TO AXIS OF ION MILL CHAMBER 14 Sept, 1998 Figure 6.8a Model 600.48000 Sector Speed Control gatan 8/98 January 1999, Rev. 1...
  • Page 59 HEIGHT SWITCH U4 74LS14 .001uF LM311 MOTOR 25pF INDEXING DISC LASER 10uF OPTO DIODE MC68705P3 SPECIMEN CURRENT CONTACT RP1 4.7K RP1 4.7K MODE SELECTOR SWITCH 14 Sept, 1998 gatan Figure 6.8b Model 600.48000 SSC Circuit Diagram 9/98 January 1999, Rev. 1...
  • Page 60 LASER BEAM O-RING (Size-010) APERTURE ASSEMBLY 600.03010 RAISE/LOWER PISTON ROD O-RING (Size-004) WINDOW 06226 WINDOW RETAINING CAP 14 Sept, 1998 Room Temperature Whisperlok Aperture Assembly Figure 7.3 gatan 9/98 January 1999, Rev. 1...
  • Page 61 The beam is on axis when the HV end cap assy is screwed in as far as possible and then backed off 3/4 to 1 1/4 turn where the reference marks will coincide. gatan 9/98 Figure 7.4a Model 600.01002 Ion Gun Mount...
  • Page 62 UPPER POSITION LOWER POSITION O-RING (Size-010) O-RING (Size-224) O-RING O-RING (Size-117) (Size-154) IMPORTANT: Evacuate capsule before depressing the cleaning tool gatan Figure 7.5 Airlock O-ring cleaning and lubrication tool 2/86 MAGNET SCREW ELECTRONIC ASSEMBLY MODULE SOCKET HEAD SCREWS POLE ANODE...
  • Page 63 A BRIGHT SILVER TO A DULL OR SATIN FINISH, DEEP YELLOW OR BROWN INDICATES THE ACTIVATED CARBON IS CONTAMINATED AND MUST BE CHANGED. THE INDICATOR STRIP MAY BE REUSED AFTER CLEANING WITH A POLISHING COMPOUND TO REMOVE THE TARNISH. 14 Sept, 1998 9/98 gatan Figure 7.8.3 Chemical Filter 600.09200 January 1999, Rev. 1...
  • Page 64 After the expiration of the warranty period described above, Gatan will provide service support for Gatan manufactured products at Gatan’s service labor rates and parts pricing in effect at the time of the repair. Gatan will continue to provide billable service support for the products for a period of three years after dis- continuance or design obsolescence by Gatan.
  • Page 66 Gatan Distributors and Agents Argentina Hungary Mexico Coasin S.A. Auro-Science Consulting Kft. IACSA de C.V. Virrey Del Pino 4071 1031 Budapest, Varosfal Koz 5. Insurgentes Sur #3807-3 1430 Buenos Aires, Argentina Budapest, Hungary Tlalpan, CP 14269 011-54-1-551-9361 011-36-1-173-0166 Mexico, D.F.
  • Page 67 Republic of South Africa P.O. Box 4144 Premier Technologies (PTY) Ltd. (So NL-5004 JC Tilburg, The Netherlands Afr.) 011-31-13536-4000 12 Executive City 011-31-13535-6279 Industrial Road, Kya Sand Randburg 2162 Turkey Republic of South Africa Tekser 011-27-11-466-1313 Bagdat Cad No. 300/6 011 27-11-466-1410 Erenkoy, Istanbul, Turkey 011-90-216-302-4116...
  • Page 68 DECLARATION OF CONFORMITY (According to ISO/IEC GUIDE 22 and EN 45014) Gatan Inc. Manufacturer’s Name: Manufacturer’s Address: 5933 Coronado Lane Pleasanton, CA 94588 U.S.A. DECLARES THAT THE PRODUCT Product Name: DuoMill Model Number: Serial Numbers: CONFORMS TO THE FOLLOWING EUROPEAN DIRECTIVES...

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