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Fischione 1010 ION MILL Instruction Manual

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MODEL 1010 ION MILL
Standard Magnification Version
INSTRUCTION MANUAL
E.A. Fischione Instruments, Inc.
9003 Corporate Circle
Export, PA 15632 USA
Phone (724)325-5444
FAX (724)325-5443
www.fischione.com
PN 009-0988 Rev.3

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  • Page 1 MODEL 1010 ION MILL Standard Magnification Version INSTRUCTION MANUAL E.A. Fischione Instruments, Inc. 9003 Corporate Circle Export, PA 15632 USA Phone (724)325-5444 FAX (724)325-5443 www.fischione.com PN 009-0988 Rev.3...

  • Page 2: Table Of Contents

    Laser Calibration Loading TEM Specimens Specimen Cooling (optional) Ion Milling Insert specimen Microscope Endpoint determination (optional) Set milling parameters Set data logging options Save recipe Start milling View Data Basic Shutdown Procedure MAINTENANCE Model 1010 Ion Mill – Standard Magnification Version...
  • Page 3 Mass Flow Controllers Verify electronics Evaluate flow Replace mass flow controller Leak Detection High pressure Vacuum Turbomolecular Vacuum Pump Reinstall Enclosure Back Panel TROUBLESHOOTING Diagnosis chart Error messages Laser SPARE PARTS AND CONSUMABLES REFERENCES Model 1010 Ion Mill – Standard Magnification Version...
  • Page 4 C o n t e n t s Model 1010 Ion Mill – Standard Magnification Version...

  • Page 5: Safety

    S a f e t y S a f e t y The following hazards are associated with the Model 1010 Ion Mill. ELECTRICAL HAZARD. High voltages can cause severe injury or death. Do not connect the power cord until after the initial inspection and after making gas connections.

  • Page 6: Background

    (metallic or semimetallic). Ion mills bombard the substrate surface with an energetic ion beam. E.A. Fischione’s Model 1010 Ion Mill is a state-of-the-art, compact, tabletop precision ion milling/polishing system that consistently produces high-quality TEM specimens with large electron transparent areas.

  • Page 7: Ion Sources

    4. Dimple grind (3 mm diameter by <10 µm center thickness). 5. Ion mill the top and bottom surfaces until they are electron transparent (3 mm diameter by <100 nm thick). 6. Plasma clean. Model 1010 Ion Mill Standard Magnification Version...

  • Page 8: System Overview

    S y s t e m O v e r v i e w Microscope Process control computer Dewar Dewar rod Mass flow controller (MFC) Turbomolecular pump (TMP) Front access door Ion source Sample chamber Model 1010 Ion Mill Standard Magnification Version...

  • Page 9: Sample Chamber

    ● The bottom lamp assembly for observing the specimen using transmitted light. ● The detector for milling termination. Rear: The rear of the chamber includes: ● The specimen stage rotator assembly. ● A series of electrical connections. Model 1010 Ion Mill Standard Magnification Version...

  • Page 10: Vacuum System

    +10°C, to prevent contamination of the specimen. If the main instrument power switch is turned off while the vacuum system is energized, the vacuum will be maintained, keeping the chamber sealed and free from ambient contamination. Model 1010 Ion Mill Standard Magnification Version...

  • Page 11: Gas Flow

    The Model 1010 can be programmed to automatically de-energize the ion sources when either a perforation in the sample is achieved or when the sample permits the transmission of laser light. The detector circuitry is designed with a variable sensitivity Model 1010 Ion Mill Standard Magnification Version...

  • Page 12: Visual Monitoring

    70 lps (minimum). With no gas flow, ultimate chamber vacuum is 1 x 10 torr. pump Under normal milling conditions, the system vacuum is between 1 x 10 and 2 x 10 torr Model 1010 Ion Mill Standard Magnification Version...

  • Page 13: Installation And Setup

    The ion mill requires about 1 square meter of bench space. Assessing initial condition 1. If the shipment has been received in good condition, proceed with unpacking. 2. If the shipment has been received with obvious damage, contact E.A. Fischione Instruments before proceeding. Unpacking and Inspecting 1.

  • Page 14: Accessories

    7. Examine the outside of the Model 1010 for visible damage. 8. If there is evidence of damage, contact both the freight carrier and E.A. Fischione Instruments before proceeding. 9. Place the Model 1010 on the surface where it will be operated.

  • Page 15: Connections

    Water Out Water In Laser Process gas Note: For plasma processing, E.A. Fischione Instruments recommends using argon with a grade equal to or better than 99.998% purity. WARNING! COMPRESSED GAS HAZARD. High-pressure gas stream can injure exposed skin or eyes. Point tubing away from personnel while connecting or disconnecting gas cylinders.

  • Page 16: Exhaust Gas

    5. Connect the exhaust of the diaphragm pump to a suitable fume hood or equivalent venting system. Water The Model 1010 Ion Mill requires a minimum water flow of 0.5 liters per minute (lpm). Water temperature should be maintained at or below room temperature. E.A. Fischione Instruments recommends using an in-line filtering system.

  • Page 17: Process Control Computer

    High magnification microscope installed Process Control Computer The process control computer is shipped already installed. The connections to the rear of the computer should be checked before operation. Process control computer Sample chamber Model 1010 Ion Mill Standard Magnification Version...

  • Page 18: Laser Installation (Optional)

    2. Verify that the operating voltage matches the requirements of the Model 1010. 110, 220, or 240 VAC can be used with the appropriate fuse. 3. Connect the power cord between the power entry module and a suitable receptacle. Model 1010 Ion Mill Standard Magnification Version...

  • Page 19: To Change Operating Voltage

    Model 1010 has been configured to operate with the operating voltage of the country of the original purchase order. If the Model 1010 is to be used under other power conditions, contact E.A. Fischione Instruments for more information. The instrument must be reconfigured...

  • Page 20: Operation

    O p e r a t i o n O p e r a t i o n CAUTION: Do not install any program onto the Model 1010 Ion Mill computer. Installing other programs, including word processing and data management programs, could interfere with the real-time control of the ion mill and will void the warranty.

  • Page 21: Dewar Bakeout

    4. Click Press to Enable Pumps to turn on the pumps. 5. Engage the Dewar conductor rod until thermal contact is made with the specimen stage. Rotate the Dewar knob clockwise, as viewed facing the instrument’s rear Model 1010 Ion Mill Standard Magnification Version...

  • Page 22: Laser Calibration

    Note: A yellow message box will appear in the Display Area, to remind the user to disengage the conductor rod. Laser Calibration 1. Install the laser into the receptacle above the viewing window. Laser cord Laser Model 1010 Ion Mill Standard Magnification Version...

  • Page 23: Loading Tem Specimens

    12. Close the program by clicking the X in the upper right corner of the program window. Loading TEM Specimens Note: Specimen thickness should not exceed 150 µm. 1. Place the TEM specimen into the recessed bottom plates (attached to the specimen gear) with manual or vacuum tweezers. Model 1010 Ion Mill Standard Magnification Version...

  • Page 24: Specimen Cooling (Optional)

    Double line Recess for insertion tool Specimen Cooling (optional) 1. Bake out the Dewar. (See page 17.) 2. Make sure the Dewar conductor rod is engaged. 3. Fill the Dewar flask with liquid nitrogen. Model 1010 Ion Mill Standard Magnification Version...

  • Page 25: Ion Milling

    The Start button will appear at the bottom of the window. Default values will appear for the first step. 3. Click Vent to release the vacuum. The chamber will not vent until the temperature rises to (+10ºC). Model 1010 Ion Mill Standard Magnification Version...

  • Page 26: Insert Specimen

    3. Make sure the chamber lights are turned off. The lights might cause the laser to give a false reading. Set milling parameters 1. Edit the default parameters for the ion sources (voltage and current), stage rotation, and milling angle. Model 1010 Ion Mill Standard Magnification Version...
  • Page 27 An effective threshold cannot be chosen for specimens that fully transmit. An example is a XTEM specimen that is held together by epoxy joints. 8. Type a value between 1 and 10. Model 1010 Ion Mill Standard Magnification Version...

  • Page 28: Set Data Logging Options

    Selected variables will appear in the data logging program (see page 27). 3. Click Close. Save recipe 1. Click Save to Disk to store the edited ion milling recipe on the computer’s hard drive. Model 1010 Ion Mill Standard Magnification Version...

  • Page 29: Start Milling

    6. Wait for the temperature to reach the minimum desired value, often –120 Omit steps 4 through 6 if the specimen is not to be cooled. 7. Click Start. The following dialog box will appear asking whether to create a log of this run. Model 1010 Ion Mill Standard Magnification Version...
  • Page 30 At the end of the ion milling program, the system initiates a resetting chamber sequence, which includes purging the gas line, returning the stage to horizontal, and recentering it. An audible signal notifies the user that the resetting chamber sequence is complete. 10. Click OK. Model 1010 Ion Mill Standard Magnification Version...

  • Page 31: View Data

    A window similar to the following will appear: 4. To access display variables, use the right button to click anywhere on the window. The following dialog box will appear: Model 1010 Ion Mill Standard Magnification Version...
  • Page 32 7. To print the data, save and then copy the file to a CD, and transfer to another computer that is connected to a printer. The file can be read by a text-editing program. Model 1010 Ion Mill Standard Magnification Version...

  • Page 33: Basic Shutdown Procedure

    4. Shutdown the computer through Microsoft® Windows. 5. Press the switch on the lower rear instrument panel (mains) to the OFF position. 6. Shut off the valves that supply gas and water to the instrument. Model 1010 Ion Mill Standard Magnification Version...

  • Page 34: Maintenance

    2. Carefully position the instrument at the edge of a workbench. Do not allow the instrument project over the edge of the bench by more than required to access the filters. 3. Snap the filters off their mounts by applying steady downward pressure. Model 1010 Ion Mill Standard Magnification Version...

  • Page 35: Changing The Fuses

    4. Pull the fuse cartridge out of the power entry module. Fuse cartridge Fuse 5. Replace the fuses. For 110 VAC operation, replace two 6-amp fuses. For 220 VAC operation, replace two 3-amp fuses. Model 1010 Ion Mill Standard Magnification Version...

  • Page 36: Opening The Enclosure

    4. Remove the standard magnification microscope, microscope post and spacer. 5. Open the instrument enclosure. 6. Remove the fan wire from the fan by pulling the molded plastic plug off the pin contacts on the fan. Model 1010 Ion Mill Standard Magnification Version...

  • Page 37: Window Cleaning

    The sapphire window is permanently adhered to the bezel to assist in handling. Attempting to remove the window from the bezel will damage both components. If the window is broken, return the bezel and window to E.A. Fischione Instruments for repair.

  • Page 38: Bottom Light Window

    Attempting to remove the window from the bezel will result in damage to both components. Should the window become broken, return the bezel/window to E.A. Fischione Instruments for repair. 3. Remove sputtered material from the window surface using any type of metal or glass polish.
  • Page 39 Bumping or rubbing of the shield on the chamber flange could cause nicks or scratches which may result in vacuum leaks. Model 1010 Ion Mill Standard Magnification Version...

  • Page 40: Cleaning O-Rings

    Cleaning o-rings Before reinstalling any window, E.A. Fischione Instruments recommends removing and cleaning the sealing o-ring. 1. Remove the o-ring using a wooden toothpick from the groove around the chamber insert.
  • Page 41 Should inadvertent contact with the bulb occur, it must be wiped with methanol and a lint free tissue. Place the new light bulb into the housing and thread on the screw cap. Model 1010 Ion Mill Standard Magnification Version...

  • Page 42: Ion Source Maintenance

    Before beginning the ion source maintenance procedure, vent the instrument to atmosphere. 5. Vent the instrument. Release vacuum Ion Mill program window 6. Shut down the computer. 7. Turn the Model 1010 power switch to the off position. Model 1010 Ion Mill Standard Magnification Version...

  • Page 43: Disconnect Gas Line

    1. Remove the three socket screws that attach the cartridge to the flange. Note that the ion source ground wire (green) is connected to one of the screws. Model 1010 Ion Mill Standard Magnification Version...
  • Page 44 3. With one hand, reach into the chamber and begin pushing the ion source cartridge outward. 4. With the other hand, both pull and direct the ion source cartridge out of the alignment flange. 5. Remove the gun cover by sliding it off the cartridge. Model 1010 Ion Mill Standard Magnification Version...

  • Page 45: Remove Cathode

    Severe damage to the components, and in particular the ceramic insulators will result. 5. Insert the anode removal tool into the cathode port to apply pressure to source components. Model 1010 Ion Mill Standard Magnification Version...

  • Page 46: Inspect Components

    1. Inspect the concave surface of the cathode. With prolonged usage the concave surface of the cathode will become both discolored and pitted. This is a result of material being sputtered from this surface during the milling process. Model 1010 Ion Mill Standard Magnification Version...

  • Page 47: Clean Components

    2. Unscrew the fluorescent gun cap from the gun body. 3. Detach the brass rings from the gun body. Ensure that they remain aligned, especially before the reassembly procedure is undertaken. Model 1010 Ion Mill Standard Magnification Version...
  • Page 48 Using an iterative approach, readjust the fluorescent gun cap and thread in the contact screws until both screws have been tightened. Model 1010 Ion Mill Standard Magnification Version...

  • Page 49: Ultrasonically Clean And Inspect Components

    1. When reassembling the ion source make sure no foreign objects are introduced onto any ion source components. E.A. Fischione Instruments recommend using nylon or talc-free rubber gloves during the assembly procedure. 2. Remove foreign substances on source components with pressurized, inert gases such as nitrogen or argon.

  • Page 50: Replace Ion Source

    The high voltage cable marked “extractor” is connected to the high voltage terminal on the ion source cartridge marked "E". Check leaks After installing the ion source into the chamber, do a vacuum leak check. See page 63. Model 1010 Ion Mill Standard Magnification Version...

  • Page 51: Start Up Ion Source

    1. Prepare a 3 mm disk cut from a glass coverslip to be used in place of a specimen. Load the alignment disk into the specimen gear. Such disks can be made using an ultrasonic disk cutter, such as the E.A. Fischione Instruments Model 170.

  • Page 52: Verify Alignment

    After prolonged use, it may become necessary to change the Zeolite® desiccant contained in the liquid nitrogen Dewar flask. This procedure should only be performed if repeated bakeout procedures are not successful and the Dewar performance cannot be optimized. Model 1010 Ion Mill Standard Magnification Version...
  • Page 53 2. Open the instrument enclosure and locate the Dewar (see page 34). Dewar 3. Before removing the Dewar knob, make sure that the orientation of the knob in relation to the shaft is clearly marked. Model 1010 Ion Mill Standard Magnification Version...
  • Page 54 It is important to have a firm grasp of the Dewar to avoid dropping it when vacuum is lost. The plastic Dewar base serves as a receptacle for the Dewar. 13. Remove the Dewar from the base. The base should remain with the instrument. Model 1010 Ion Mill Standard Magnification Version...

  • Page 55: Change Zeolite® Desiccant

    14. Clean both the Dewar bottom housing, and especially the o-ring seat. 15. Lightly coat the o-ring with Fomblin® vacuum grease 16. Reposition the o-ring with respect to the bottom housing. 17. Replace the bottom housing on the Dewar. Model 1010 Ion Mill Standard Magnification Version...

  • Page 56: Install Dewar

    Due to the nature of ion milling, the entire chamber/specimen stage will need to be periodically cleaned to remove excessive amounts of sputtered material. Cleaning frequency depends on the usage of the instrument. However, E.A. Fischione Instruments recommends complete cleaning at least once per year.
  • Page 57 This connector simply pulls straight out of its socket. 2. Remove the stage ground wire. 3. Unthread the bezel surrounding the connector to the stage heater, and then gently remove this connector from its socket. Model 1010 Ion Mill Standard Magnification Version...
  • Page 58 2. Slide the encoder/pick-up assembly clockwise to free it from the gear. It may be necessary to rotate the entire rotator assembly by hand in order to position the gear for the removal of the encoder/pick-up assembly. Model 1010 Ion Mill Standard Magnification Version...
  • Page 59 The rotator plate should be installed as straight as possible. Any angling of the rotator plate in relation to the chamber will prevent full insertion of the rotator plate leading to the inability to achieve a vacuum. Model 1010 Ion Mill Standard Magnification Version...

  • Page 60: Ion Source Flange

    The flanges contain the water cooling connections for the ion sources. Swagelok® water line fittings Disconnect water line 1. Disconnect the water supply lines from the alignment flanges by loosening the Swagelok® connection. Model 1010 Ion Mill Standard Magnification Version...
  • Page 61 1. Reconnect the water lines as described on page 12. CAUTION: For proper water flow and function of the pressure/flow switch, the water lines must be connected properly. Failure to do so could result in overheating of the ion sources. Model 1010 Ion Mill Standard Magnification Version...

  • Page 62: Pirani Gauge Tube

    6. Place the ferrule over the gauge tube. 7. Coat the o-ring with a light film of Fomblin® and slide over the gauge tube. Model 1010 Ion Mill Standard Magnification Version...

  • Page 63: Bottom Plate

    5. Carefully inspect the bottom plate for scratches with extra emphasis focusing on the bore into which the light assembly fits. 6. If scratches appear on any o-ring sealing surface, remove them and re-clean the plate. Model 1010 Ion Mill Standard Magnification Version...

  • Page 64: Mass Flow Controllers

    (0 to 5 vdc proportional) Zero volts indicates zero flow. +5 vdc indicates 1 sccm of flow. These values should be approximately equal to the flow indication on the computer’s display. Model 1010 Ion Mill Standard Magnification Version...

  • Page 65: Evaluate Flow

    5. Remove the three screws. 6. Lift the flow controller assembly from the instrument. 7. Remove the two screws that attach the flow controller to the bracket. Model 1010 Ion Mill Standard Magnification Version...

  • Page 66: Leak Detection

    Turn off the instrument. Wait one minute to ensure that any charged electronic component will discharge before disconnecting the power cord from the instrument. 2. Disconnect the power cord. 3. Close the cylinder valve and observe for a pressure drop. Model 1010 Ion Mill Standard Magnification Version...

  • Page 67: Vacuum

    Attempt to identify the leak location. 7. If any leak is detected, disassemble, clean (ensure all seal surfaces are free of dirt, oil, hair and dust) and repair the component. Model 1010 Ion Mill Standard Magnification Version...

  • Page 68: Turbomolecular Vacuum Pump

    If the green LED is lit, the pump is operating correctly. If the red LED is lit, the pump may need to be serviced or replaced. Consult the manufacturer’s manual or E.A. Fischione Instruments for more information. Reinstall Enclosure At the conclusion of major service, reinstall the enclosure.

  • Page 69: Troubleshooting

    Gas leak (See page 62.) or clean the ion source. (See page 38.) Weak ion beam as determined visually Check the high voltage connections and ion source power supplies (after contacting E.A. Fischione Instruments) Little or no milling on one or both specimen Align the ion source. (See page 47.) surfaces...
  • Page 70 Water leak Check water connections. (See page 12.) Service water inlet solenoid. (See page 61.) Gas leak High pressure argon gas leak. (See page 62.) Condensation forms on the Dewar Bakeout. (See page 17.) Model 1010 Ion Mill Standard Magnification Version...

  • Page 71: Error Messages

    If the thermal safeguard is enabled and the temperature exceeds the set value during milling, the sequence will be terminated and the user informed. Model 1010 Ion Mill Standard Magnification Version...

  • Page 72: Laser

    The laser operates independently from the ion mill. It turns on whenever the checkbox for laser threshold is checked and turns off whenever the box is unchecked. This allows the user to test the light penetration of the sample without actually milling it. Model 1010 Ion Mill Standard Magnification Version...

  • Page 73: Spare Parts And Consumables

    387-0028 O-RING; Buna; .650 x .024 009-0206 500-0073 Power Supply; +24V, 300W 009-0679 500-0105 Power supply, 100W, +5,+15,-15V 009-0679 009-0696 PCB Assembly; Stepper Motor Network Module 009-0679 009-0694 PCB Assembly; Network Backplane 009-0683 Model 1010 Ion Mill Standard Magnification Version...
  • Page 74 477-0018 Grid Storage Box 009-0381 009-0413 Low Angle Bottom Plate 009-0378 009-0414 Top low Angle Plate 009-0378 387-0004 O-Ring; Viton®; -015 009-0297 009-0081 Drive Shaft 009-0297 009-0360 Conductor Rod 009-0297 387-0063 O-Ring; Viton®; -337 009-0620 Model 1010 Ion Mill Standard Magnification Version...

  • Page 75: References

    Liquid nitrogen cooling during ion milling promoted retention of the dopant distribution. Annular dark field (ADF) STEM images of the electron transparent material were acquired with atomic resolution. These images could be used to quantify the dopant concentration. Model 1010 Ion Mill Standard Magnification Version...
  • Page 76 0.4 µm field of view. Images were acquired at the interphase interface with resolution on the atomic scale, specifically 1.9 Angstroms. Model 1010 Ion Mill Standard Magnification Version...
  • Page 77 ADF STEM images were acquired at grain boundaries within the electron transparent region. Situated at the boundaries, the Ca dopant acts to couple the superconducting current between adjacent grains. Liquid nitrogen cooling during ion milling is critical to retaining the distribution of Ca. Model 1010 Ion Mill Standard Magnification Version...
  • Page 78 P.J. Goodhew, “Final thinning: ion beam thinning and mechanical techniques”, in Thin Foil Preparation for Electron Microscopy, Elsevier, 1985. D.B. Williams and C.B. Carter, “Specimen Preparation” in Transmission Electron Microscopy: A Textbook for Materials Science, Plenum Press, New York, 1996. Model 1010 Ion Mill Standard Magnification Version...

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