Fischione 1010 ION MILL Instruction Manual Download

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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

Summary of Contents for 1010 ION MILL

Page 1: ...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: ...d Notes 9 Assessing initial condition 9 Unpacking and Inspecting 9 Accessories 10 Connections 11 Process gas 11 Exhaust gas 12 Water 12 Microscope Installation 12 Process Control Computer 13 Laser Installation optional 14 Power Connections 14 For US application 14 For non US application 14 To change operating voltage 15 OPERATION 16 Basic Startup Procedure 16 Dewar Bakeout 17 Laser Calibration 18 ...

Page 3: ...mble ion sources 45 Verify electrical connections 45 Replace ion source 46 Attach gas and electrical connections 46 Check leaks 46 Start up ion source 47 Ion Source Alignment 47 Adjust source alignment 47 Verify alignment 48 Dewar Maintenance 48 Remove Dewar 48 Change Zeolite desiccant 51 Install Dewar 52 Evacuate Dewar wall space 52 Chamber and Specimen Stage Cleaning 52 Stage maintenance 52 Ion ...

Page 4: ...C o n t e n t s Model 1010 Ion Mill Standard Magnification Version ...

Page 5: ...n cause severe injury or death If hazardous materials will be inserted into the Model 1010 for processing the ion mill must be connected directly to an exhaust system capable of accommodating the hazardous material If radioactive materials will be milled the instrument must be enclosed in protective shielding LASER HAZARD Laser beams can cause severe eye damage Do not point the laser beam into you...

Page 6: ... 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 Ion Milling Theory Ion milling uses an impinging incident HAD Hollow Anode Discharge ion to remove sputter ions from the surface of a sample If an inert gas for example Ar or Ar is used fo...

Page 7: ...p to 400 microamps To a first approximation varying voltage varies the average ion energy while varying current varies the ion flux The milling rate for a given material generally increases as either parameter is increased They are fabricated from a combination of aluminum brass ceramics polymers and stainless steel Hollow Anode Discharge HAD ion source Basic Procedure for Sample Preparation and I...

Page 8: ...4 Model 1010 Ion Mill Standard Magnification Version S y s t e m O v e r v i e w Turbomolecular pump TMP Ion source Mass flow controller MFC LN2 Dewar Dewar rod Microscope Sample chamber Process control computer Front access door ...

Page 9: ...alignment flanges Radial o ring seals ensure the vacuum integrity between the ion sources and the chamber Bottom A vacuum flange mounted on the chamber bottom contains The Pirani gauge for sensing vacuum 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 ...

Page 10: ...was open exposing the chamber to ambient conditions Pump down times are also increased following ion source cleaning or chamber maintenance The turbomolecular pump is directly mounted to the chamber by two bolts An inlet protection screen prevents debris from entering the pump and damaging the turbine blades An electro mechanical vent valve is installed directly onto the chamber and all venting is...

Page 11: ...pens allowing water flow into the alignment flanges thus cooling the ion sources A solenoid valve conserves water by only permitting flow when required to cool an energized ion source The temperature of the inlet water is not critical but should be maintained between 5 C and room temperature Water flow of approximately 0 5 lpm is recommended In the unlikely event of the drain line becoming obstruc...

Page 12: ...ion raises the temperature and controls the time at temperature Laser Detector Calibration Program Calibrates the laser detector according to the transmissive properties of the window protecting the laser sensor Allows the user to choose the minimum and maximum sensitivity values Data Logging Program Controls logging retrieval and display of milling parameters Specifications Ion source type Hollow...

Page 13: ...r is installed Remove the microscope laser and post assembly before initiating service Opening the Model 1010 while these components are installed could damage the microscope and the enclosure CAUTION Do not energize the ion sources unless Argon gas is supplied CAUTION Do not energize the ion sources without a specimen in the specimen holder Failure to follow this caution will result in the ion be...

Page 14: ...tside 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 Accessories 1 Open the box containing the accessories This box includes Microscope microscope and spacer Specimen loading station and accessories Tool set Optional laser Dewar cap...

Page 15: ...he process gas supply so that it is located within five feet of the ion mill 2 Mount a suitable pressure regulator Victor HPT 270 or equivalent onto the process gas supply 3 Connect the in tubing supplied between the pressure regulator on the process gas supply and the gas inlet quick connection on the rear of the Model 1010 4 Tighten the connection 1 turns after finger tight 5 Open both the cylin...

Page 16: ...id the warranty 2 Remove the small plastic muffler from the pump exhaust 3 Thread the connector into the pump exhaust 4 Press the included Viton tubing over the barb connector 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...

Page 17: ... 10X eyepieces after removing their individual lens caps and then remove the lens cap on the microscope s lens 5 Install the microscope onto its post lowering its mount until it contacts the spacer 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 ...

Page 18: ...r US application 1 Verify that the operating voltage matches the requirements of the Model 1010 The power entry module is equipped with two 6 amp fuses for 110 VAC operation and two 3 amp fuses for 220VAC operation 2 Connect the power cord between the power entry module and a suitable receptacle For non US application 1 Attach a suitable connector to the bare wires of the power cord supplied using...

Page 19: ...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 by a qualified service technician or returned to factory ...

Page 20: ... temperature must be at least 10 C Basic Startup Procedure 1 Verify that the ion mill is supplied with electricity gas and water 2 Press the switch on the lower rear instrument panel mains to ON 3 Press and hold the power button on the computer until the computer boots up A user identification dialog box will appear 4 Click OK Note Click means to use the touch pad on the computer to move the point...

Page 21: ...keout icon on the desktop to initiate the Dewar flask heating program Note Click means to use the touch pad to move the pointer into position then press the left button of the touch pad on the computer Double click means to click twice 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 cloc...

Page 22: ...erformance is not optimal after this step the bakeout should be repeated for a time of 12 hrs 8 Click Start Note To manually turn off the heater click Disable Bakeout When the time has expired the heater and pumps will turn off the Dewar valve will close and a dialog box appears indicating the procedure is finished Click OK 9 Open the Ion Mill program see page 21 10 Click Vent to release the vacuu...

Page 23: ...m will begin checking the laser detector readings 8 Click Turn Laser On 9 Minimum reading should remain low about 0 Maximum reading should go up to about 255 10 Click Save Readings 11 If the readings are unusual or otherwise unacceptable click Reset Readings and start the calibration again 12 Close the program by clicking the X in the upper right corner of the program window Loading TEM Specimens ...

Page 24: ...s to be oscillated and milled using both ion sources align the double line on the gear so it points to the position 1 shown below If only the top source is used align the double line so it points to position 2 If only the bottom source is used align the double line so it points to position 3 Specimen Cooling optional 1 Bake out the Dewar See page 17 2 Make sure the Dewar conductor rod is engaged 3...

Page 25: ... ion milling program steps Operation area for entering the ion milling parameters and editing a given step Ion Mill program window The program goes through several initialization procedures including checking the tilt of the stage making sure the stepper motor is engaged checking the pressure and temperature and calculating some behind the scenes calibrations 2 Wait until the initializing phase is...

Page 26: ...ount and or the mount with respect to its post 3 Choose the magnification level by rotating the zoom adjustment 4 Focus the microscope by rotating the focus knob 5 Select an area of interest by further adjusting microscope with respect to its mount and or post Endpoint determination optional 1 If the endpoint determination capability is used install the laser see page 18 2 Close the shutter on the...

Page 27: ...move a step a Select the step b Click Remove Step 7 If the endpoint detection capability is used click Laser Threshold The Laser Threshold is the sensitivity of the laser detector defined in arbitrary units of 1 to 10 This sensitivity decreases as the threshold increases A threshold of 1 is optimal for specimens that do not transmit laser light such as metals A higher value may be chosen for speci...

Page 28: ...matically and a heat sensitive specimen will be protected 10 Type a value for the maximum temperature between 120 and 60o C Set data logging options Selected real time ion milling parameters may be recorded by using the data logging program The information will be automatically saved to the computer s hard drive and can be displayed in graphical form 1 Click Logging Options The tracking selection ...

Page 29: ...operators start the pump before setting milling parameters to save time 2 Close the shutter on the front window 3 Wait until a vacuum of 2x10 5 torr has been achieved 4 Engage the conductor rod by rotating the Dewar knob clockwise as viewed from the rear of the instrument Rotate until the pin on the knob contacts the pin stop 5 If the specimen is to be cooled fill the Dewar with liquid nitrogen 6 ...

Page 30: ...ature rocking angle ion source voltage and current milling angle and status of shutter lights and chamber insert Milling operation underway The Start button changes to a Stop button which allows the user to manually terminate the milling operation at any time At the end of the ion milling program the system initiates a resetting chamber sequence which includes purging the gas line returning the st...

Page 31: ... of 20 seconds the vent valve is opened and the chamber is brought to ambient pressure in approximately 10 additional seconds 13 Open the chamber access door and retrieve the specimen gear and specimen View Data 1 Click the Log Viewer icon on the desktop to start the data viewing program 2 Select a file to view 3 Select a parameter to view Possible parameters are stage temperature current and volt...

Page 32: ...urve as straight lines between points Outlined Displays points with boxes around them 5 Select the display variables desired 6 To change the view use the following keys Viewing option Key Zoom in on location of pointer i Zoom out o Recenter and rezoom to starting point r Move view of graph up down left or right Arrow keys 7 To print the data save and then copy the file to a CD and transfer to anot...

Page 33: ...t the vacuum level is 2x10 5 torr 2 Close the Ion Mill program by clicking X in the top right corner of the program window The instrument will remain under vacuum 3 Log off the computer 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 ...

Page 34: ...window As required Inspect clean if needed Page 33 Top and Bottom light windows As required Inspect clean if needed Page 34 Turbo drag pump 1 year Lubricate Manufacturer s instructions Diaphragm pump 1 year Inspect diaphragms Manufacturer s instructions Cleaning the Air Filters The Model 1010 is equipped with three ventilation fans that circulate the air through the instrument enclosure Air is dra...

Page 35: ... to ensure that any charged electronic component will discharge before disconnecting the power cord from the instrument 1 Turn the Model 1010 power switch to the off position 2 Disconnect the power cord 3 Using a small blade screwdriver gently remove the plastic cover from the power entry module on the back of the instrument 4 Pull the fuse cartridge out of the power entry module 5 Replace the fus...

Page 36: ...Firmly grasp the bottom of the hinged enclosure portion and lift upward Because the instrument is hinged in the front the enclosure will rotate forward Enclosure removal For a major cleaning remove the top instrument enclosure This will provide easy access to the various system components 1 Vent the instrument 2 Turn the Model 1010 power switch to the off position WARNING ELECTRICAL HAZARD High vo...

Page 37: ...top and bottom light assemblies Chamber access door window Although protected by a shutter assembly this window will eventually need to be cleaned 1 Ensure that the instrument is vented and not powered ON 2 Engage the pins on the door window removal wrench with the holes in the bezel 3 Rotate the wrench counterclockwise until the bezel and window can be removed CAUTION The sapphire window is perma...

Page 38: ...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 4 Use ultrasonic cleaning for final cleaning Top light window 1 Ensure that the instrument is vented and not powered ON 2 Remove the 8 32 socket head cap screw and angled brack...

Page 39: ...ve the single screw which fastens the lamp assembly to the chamber flange 3 Gently slide the light laser detector assembly downward to the instrument s base plate CAUTION The bottom light laser detector contains a sputter shield which extends from the chamber bottom flange to the specimen stage Because of the length involved in this shield extreme care should be taken when removing or re installin...

Page 40: ...g 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 CAUTION The sealing surface is easily damaged Never use a metal object to remove an o ring 2 Clean both the o ring and its corresponding seat area with ethanol or isopropyl alcohol CAUTION Use o...

Page 41: ... lint free tissue 4 Place the new light bulb into the housing and thread on the screw cap Install the light housing into the chamber and replace the L clamp Bottom Light 1 Ensure the instrument is vented and not powered ON 2 To replace the light bulb unscrew the black plastic cap until it becomes free from the assembly at which point the bulb will drop out Because the lamp is a halogen bulb care s...

Page 42: ... is unable to sustain a stable ion beam or produces a weak beam as determined visually 1 Remove the laser 2 Remove the microscope microscope post and spacer 3 Remove the three screws on the top back surface of the instrument 4 Rotate the hinged upper enclosure forward WARNING COMPRESSED GAS HAZARD Compressed gas can injure skin or eyes Before beginning the ion source maintenance procedure vent the...

Page 43: ...clockwise A stainless steel ferrule on the stainless steel gas tube maintains the vacuum integrity between of the gas tube and the fitting Allow the stainless steel ferrule to remain on the stainless steel gas tube Remove ion source cartridge Note The ion source functional components are all contained in the ion source cartridge CAUTION Ion source components are easily damaged Work in a clean area...

Page 44: ...g the ion source or source components to avoid contaminating source components 2 Don talc free rubber gloves 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 Socket screw Ground wire Flange Electrical feedthr...

Page 45: ...e remainder of the components insert the pins located on the end of the gun tool into the holes on the contact nut 2 Rotate counterclockwise to remove 3 Invert the cartridge with the cathode port facing upward 4 Cover the end of the ion source from which the beam is projected with one hand CAUTION Components may be damaged if dropped When removing ion source components from the gun body make sure ...

Page 46: ...hey are contaminated with acetone they must be replaced 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 Anode removal tool Cathode Gun body Brass ring Ceramic insulator O rings O ring O ring Brass ri...

Page 47: ...rically conductive the ion source will short circuit when the sputter build up becomes excessive Shorting of ion source components greatly decreases ion source efficiency and could lead to electronic control problems Sputtered material must either be removed from the ceramic insulators or the insulators must be replaced The cleaning procedure for the anode cathode and extraction aperture are virtu...

Page 48: ...node contact screw into the electrical contact that corresponds to the anode connection which is marked with an A on the outside of the gun body The extractor contact screw is the outer most screw whose head is accessible on the face of the extraction brass contact ring 14 Thread the extractor screw into the electrical contact that corresponds to the extraction connection which is marked with an E...

Page 49: ...ce performance 3 Stack the source components in their respective positions 4 Hold the ion source cartridge in the inverted position the cathode port facing upward and insert the component stack 5 Make sure that all components are properly seated in their respective positions 6 Rotate the ion source cartridge 180 until the extraction aperture is facing upward 7 Verify that the extractor is centered...

Page 50: ...g screw holes are properly aligned with their corresponding parts of the alignment flange 5 Apply firm even force to the ion source cartridge pushing it into the chamber until the back of the gun body flange is flush with the outer surface of the alignment flange 6 Install the three screws 7 Be sure that the ion source ground wire is attached to one of the screws Attach gas and electrical connecti...

Page 51: ... or no milling on one or both specimen surfaces or if perforations occur consistently off center it is an indication that adjustment of the ion sources may be required This can be confirmed quickly by utilizing a beam alignment disk This disk is a 3 mm diameter and 150 µm thick section of glass chosen so that a well defined ion beam could be observed with the unaided eye A 5X loupe may be placed o...

Page 52: ...re for the bottom ion source Verify alignment 1 To verify alignment ion mill a thin 25 micron sheet of Cu or Al Copper or Aluminum is suggested because of their rapid milling rates however any type of material can be used 2 Make sure that the beams are properly aligned and the perforation occurs either at or near center For Aluminum foil the time to perforation is typically 1 hour for the followin...

Page 53: ...nected 2 Open the instrument enclosure and locate the Dewar see page 34 3 Before removing the Dewar knob make sure that the orientation of the knob in relation to the shaft is clearly marked Dewar Conductor rod Dewar flange Thermal contact flange Dewar knob Conductor screw Rear cross bushing Belleville spring washer O rings Drive shaft assembly ...

Page 54: ...t connects the Dewar valve to the specimen rotator assembly 9 Remove the two screws in the Dewar base plate that attach the base plate to the supporting bracket 10 With one hand firmly grasp the Dewar housing 11 With the other hand stabilize the junction where the tube projecting from the Dewar meets the tube projecting from the stage This junction contains a radial o ring seal that maintains the ...

Page 55: ...e top of the Dewar housing onto its bottom 7 Lift and remove the top of the Dewar housing from the bottom 8 Remove the four wires that attach the desiccant screen to the inner vessel 9 Remove the desiccant and dispose of it properly 10 Wipe the bottom of the inner vessel with methanol and allow to dry 11 Replace the desiccant 12 Install the desiccant screen 13 Remove the o ring from the Dewar bott...

Page 56: ...e to its support 10 Re connect the electrical connections to the Dewar switch 11 Connect the flexible Viton tube to the rotator assembly 12 If no further maintenance is required replace the instrument s back panel and reconnect the Dewar valve Evacuate Dewar wall space The volume between the inner vessel and outer housing of the Dewar needs to be evacuated in order to ensure proper vacuum for insu...

Page 57: ...ill discharge before disconnecting the power cord from the instrument 3 Disconnect the power cord 4 Remove the Dewar and the instrument s back panel as described on page 48 Disconnect electrical connections 1 Disconnect the electrical connections to the temperature sensor This connector simply pulls straight out of its socket 2 Remove the stage ground wire 3 Unthread the bezel surrounding the conn...

Page 58: ...omponent of the flexible coupler Remove angle encoder 1 Remove the optical encoder and zero position optical pick up by removing the two screws that fasten the bracket to the chamber Once these screws are removed TAKE CARE TO NOT DAMAGE THE OPTICAL PICK UP 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 or...

Page 59: ...ucting service on the rotator plate Any scratches or nicks on the face of the rotator plate will lead to vacuum leaks Install rotator 1 Prior to installation remove the o ring from the chamber and clean thoroughly with methanol or isopropyl alcohol 2 Wipe the chamber surface with acetone 3 Allow to dry 4 Apply a light film of Fomblin grease to the o ring and position the o ring into the chamber 5 ...

Page 60: ... gear mounted to the rotator plate 4 To install the rotation motor make sure that the plastic component of the flexible coupler is in place in one half of the coupling 5 Mate the shafts together with the plastic component in between 6 Secure the motor with the two screws Attach electrical connections 1 Attach the electrical connection for the heater and temperature sensor The connector on the end ...

Page 61: ...nt screws 2 Remove the three shoulder screws and their springs The alignment flange is now free from the chamber Install flange 1 Following the service to the chamber reinstall the alignment flange to the chamber with the three shoulder screws 2 Be sure to place a compression spring onto each screw prior to insertion into the alignment flange Connect water line 1 Reconnect the water lines as descr...

Page 62: ...or pulls off the end of the gauge tube Remove gauge tube 4 Loosen the knurled bezel nut that fastens the Pirani gauge into the vacuum bulkhead fitting on the bottom plate 5 Slide the gauge tube out of the bulkhead fitting 6 Clean and inspect the tube Install gauge tube 1 Remove the bezel nut o ring and ferrule 2 These parts should be cleaned and the o ring should be inspected 3 If signs of damage ...

Page 63: ... 1 Remove the light source photo detector refer to page 34 and the Pirani gauge tube page 58 CAUTION Once the screws holding it are removed the bottom plate drops out of the chamber Be sure to support the bottom plate when removing the screws to prevent damage 2 Remove six socket head cap screws holding the bottom plate 3 Remove the o ring 4 Soak and then clean the plate in acetone and allow to dr...

Page 64: ... chamber surface resulting in vacuum leaks 5 Install the Pirani gauge tube page 58 and transmission light photo detector assemblies page 34 Mass Flow Controllers Two mass flow controllers supply the appropriate argon gas flow to each ion source Argon flow is automatically controlled through a feedback control loop There are no internal or external adjustments required for the flow controllers They...

Page 65: ...n a flow of 0 5 sccm 9 Submerge the end of the gas tube in the beaker of methanol Approximately two bubbles per second should emerge from the end of the tube 10 If excessive bubbling occurs replace the flow controller Excessive bubbling is an indication of a failed flow controller which must be replaced Such a flow condition would result in the inability of the instrument to achieve a proper opera...

Page 66: ...responding screws 14 Re connect both the inlet line to the flow controller manifold and the outlet lines to the ion sources 15 Leak check the instrument both on the pressure and vacuum sides using the procedure in the following section Note When reconnecting the argon line to the instrument follow the purge procedure described on page 11 Leak Detection High pressure To evaluate the instrument for ...

Page 67: ...aching this vacuum it is an indication of a possible vacuum leak NOTE If the instrument has not been used for or has been open to atmosphere for prolonged periods of time pumping times will be longer that usual Pump the instrument repeatedly before concluding that a vacuum leak exists 1 To vacuum leak check the instrument open the enclosure See page 32 2 Locate the black Viton tube that connects t...

Page 68: ...ure in front of the instrument 2 Insert the six studs projecting from the instrument enclosure through the holes in the hinges 3 Fasten with the six hex nuts 4 Re connect the audible alarm fan and computer 5 Slowly lower the enclosure into the closed position making sure that no wires or other objects are caught trapped or pinched Back Panel If the back panel has been removed it should be replaced...

Page 69: ...lly 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 surfaces Align the ion source See page 47 Maintaining temperature problem Problem Possible causes and solutions Insufficient cooling Check for disengaged or damaged conductor rod If neither condition applies then bakeout the Dewar See page 17 ...

Page 70: ...oid See page 61 Power problem Problem Possible causes and solutions Ion mill won t turn on No power check the powercord See page 14 Check the fuses and replace if necessary See page 31 Safety interlock on lid is not engaged Make sure the enclosure is closed See page 64 No light in the chamber Check lamps and replace if necessary See page 36 Check or service top and bottom light sources Consult ill...

Page 71: ...e representative Gun X gas flow is outside of tolerance Please contact your service representative Stage temperature is outside of tolerance Please power down the unit and contact your service representative For warnings that include Abort Retry Ignore options Abort will terminate the sequence but leave the program window running Retry will clear the message but continue normally until another war...

Page 72: ... Magnification Version 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 ...

Page 73: ... 10 475 0037 Fitting O seal Straight Thread 5 16 24 Male 0 062 O D 009 0708 46 475 0247 Fitting 1 4 Straight Thread to 8mm Elbow Push Lok 009 0708 7 009 0002 Anode Contact Ring 009 0206 12 009 0003 Anode Insulating Ring 009 0206 11 009 0007 Extractor 009 0206 6 009 0010 Extractor Insulating Ring 009 0206 10 009 0016 Anode Insulator 009 0206 14 009 0019 Extractor Screw 009 0206 7 009 0024 Anode Scr...

Page 74: ... 387 0003 Lamp Halogen 5 2V 0 85A 009 0764 2 387 0024 O RING Viton 116 009 0764 3 387 0027 O Ring Viton 238 009 0767 8 444 0001 Vacuum Gauge Tube 009 0767 5 009 0762 Assembly Vacuum Gauge Controller 115VAC 009 0768 6 327 0002 Mass Flow Controller 009 0768 1 009 0378 Low Angle Gear 009 0381 2 458 0003 Tweezer Dumont 5 Antimagnetic Stainless Steel 009 0381 5 477 0018 Grid Storage Box 009 0381 6 009 ...

Page 75: ...Extractor voltage and current should be chosen to avoid damaging a specimen through amorphization ion implantation or overheating It is recommended that liquid nitrogen cooling always be used to avoid overheating Typical instrument parameters for milling materials are summarized below Material Extractor Voltage kV Extractor Current mA Temperature Degrees C Polymers 2 5 90 Metals 2 3 5 90 Silicon 3...

Page 76: ...yers of La and Sr titanates The results are included in the following two images After wedge polishing ion milling with liquid nitrogen cooling and plasma cleaning the electron transparent region yielded a 0 4 µm field of view Images were acquired at the interphase interface with resolution on the atomic scale specifically 1 9 Angstroms ...

Page 77: ...eaning of a specimen consisting of YBCO superconducting material Atomic resolution 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 ...

Page 78: ... the grain boundary was identified existing on the nanoscale R e f e r e n c e s General references on ion milling theory and practice include 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 Plenu...

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