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Operating Manual Leica EM ACE600

Version 01/19

Page 54

Each thread is degassed separately before it is used.
The system waits after outgassing to stabilize the vacuum.

4.7

Sputter coating

Magnetron 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. This coating process can be more directional (sputtering at
better vacuum low 10

-3

mbar) or diffuse (more even coating on a bigger surface

and fissured samples, sputtering at low 10

-2

mbar). This also influences the

coating rate (diffuse means slower rate) and the grain size (directional means
finer grains). With the quartz thickness measurement (QSG) the layer thickness
can be calculated because of the changed quartz crystal resonance frequency
(3.8).

Targets
Various targets can be supplied by Leica Microsystems for the EM ACE600 for
example:



Gold



Gold-Palladium



Platinum



Platinum-Palladium



Silver



Chromium



Tungsten



Iridium



Copper



Nickel

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Содержание EM ACE600

Страница 1: ...From Eye to Insight OPERATING MANUAL EM ACE600 167202032 Version 01 19 ...

Страница 2: ...d manufacturing techniques used to provide our customers with excellent products Any copyrights of this document are retained by Leica Mikrosysteme GmbH Vienna Any reproduction of text and illustrations or any parts thereof by printing photocopy ing or other methods including electronic systems and media requires express prior permission in writing Issued by Leica Mikrosysteme GmbH Hernalser Haupt...

Страница 3: ... EM ACE600 Serial Number Date of purchase For the instrument serial number please refer to the name type label on the back of the instrument Please read this instruction manual carefully before operating the instrument For Research use only ...

Страница 4: ......

Страница 5: ...stances 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 subjected to vacuum and or coating procedures Warranty claims will only be considered if the instrument is used according to the guidelines specified in this user manual In add...

Страница 6: ...h nitrogen 11 2 4 6 Emergency procedure 15 3 Installation and set up 15 3 1 Warranty 15 3 2 Instrument overview 16 3 3 Delivery of the instrument 17 3 4 Installation requirements for the instrument 17 3 5 Unpacking and connection 18 3 6 Inserting chamber shielding 22 3 7 Shutter installation 26 3 8 Quartz crystal measurement installation 28 3 8 1 Eccentric quartz holder 30 3 9 Stage installation 3...

Страница 7: ...ng 84 4 9 1 Loading a carbon rod 85 4 9 2 Choosing a carbon rod protocol 91 4 9 3 Carbon rod materials 94 4 10 Glow discharge 95 4 10 1 Choosing a glow discharge protocol 95 4 11 Sequence 98 4 12 Rotating stage difference in user interface and set up 102 4 13 Running a process 103 4 14 Load lock 106 5 Maintenance and service 110 5 1 General instructions for maintenance and cleaning 110 5 1 1 Sourc...

Страница 8: ......

Страница 9: ...ng these instructions will help prevent hazards reduce repair and downtime costs and prolong the system s service life In this user manual symbols are used to alert the user about important information such as necessary safety precautions activites relating the operation and or maintenance of the system and relevant process oriented descriptions or remarks Symbols used in this manual and their mea...

Страница 10: ...bols and indications on the instrument and their meaning The plug is equipped with a locking mechanism Please do not pull on the cable Grasp the knurled part of the plug and retract for disconnecting the cable Hazardous Voltage Enclosed Voltage or current hazard is sufficient to cause shock burn or death Disconnect and lockout power before servicing Danger of pinching the fingers when closing the ...

Страница 11: ...as been tested to the requirements of CAN CSA C22 2 No 61010 1 second edition including Amendment 1 or a later version of the same standard incorporating the same level of testing requirements 1 1 Identification 1 1 1 Product Leica EM ACE600 High Vacuum Coater 1 1 2 Name and address of the manufacturer Leica Mikrosysteme GmbH Hernalser Hauptstraße 219 A 1170 Vienna Tel 43 1 488 99 0 Fax 43 1 488 9...

Страница 12: ...n coating The Leica EM ACE600 coater can be configured with up to two some limitations of the following processes sputtering carbon thread evaporation carbon rod evaporation e beam evaporation The removable shielding shutter source and door are designed to enable easy and comprehensive cleaning of the system The vacuum system creates an ultimate vacuum 2x10 6 mbar Pressure is monitored by a combin...

Страница 13: ...bout 20 mm more in depth and 5 kg heavier Dimensions for the Leica EM ACE600 with a VCT500 are in the technical data sheet and the manual for cryo outfits 2 3 Environmental conditions for operation and storage Indoor use altitude up to 2000 m Power supply 100 115 230 V Humidity 80 RH no condensation Temperature range 15 C 30 C Pollution degree IEC 61010 1 2 ...

Страница 14: ...es are protected against overheating If at any time the source temperature reaches 65 C the system automatically pauses the current process only to continue after the temperature has sank below 45 C In case of a sudden and unexpected vacuum break the instrument switches off automatically to protect the pump and electric parts All electrical parts are safely separated from the user by the front cov...

Страница 15: ... rules for safety at work The operating personnel responsible for operating and maintaining the Leica EM ACE600 coating system must satisfy the specific professional requirements for their respective duties The operating personnel must have received training and must be familiar with the duties that have been assigned to them and for which they are responsible 2 4 4 Residual hazards The Leica EM I...

Страница 16: ... If an unconscious person stays in a low oxygen environment then death may occur If breathing stops apply artificial respiration at once and notify doctor and ambulance immediately For the reasons given above never put LN2 Dewars in a closed storage room or chamber The evaporation rate from Dewar vessels can rise to several liters a day if they are defective due to improper handling or to natural ...

Страница 17: ...e protection which are open at the top and at the bottom Only use boots if you have loose not narrow trousers coming outside the boots d and completely covering the gap Wear only open slip on sandals f in the lab no walking shoes or court shoes Always wear cuffless trousers if you wear slip on sandals Never wear protective gloves when pouring LN2 or when putting the Dewar head on the Dewar vessel ...

Страница 18: ...gh liquid oxygen content has a faintly bluish color Concentrated liquid oxygen promotes vigorous burning Make sure that your Dewar vessel is filled only with LN2 Apply a note in the central distribution place stating clearly ONLY LIQUID NITROGEN or similar if different liquefied gases are delivered from there Check the color of cryogen Bluish color indicates the presence of a high percentage of li...

Страница 19: ...ces due to displacement of oxygen by N2 when using or dispensing large volumes of LN2 This can cause immediate fainting and unconsciousness Always use LN2 in well ventilated areas Treat it with respect Storage For reasons mentioned above do not store full LN2 Dewars in confined spaces Burns LN2 boils at 196 C It is extremely cold and can cause serious burns Please read the safety instructions prov...

Страница 20: ... of injury Burns may be sustained Caution There is danger from the edges of the metal sheet of the internal shielding and shutter Personal injury e g cuts may occur 3 Installation and set up 3 1 Warranty The Leica EM ACE600 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 cov...

Страница 21: ...cover 2 Source head sputter a or carbon thread b 3 Shutter 4 Chamber 5 Sample stage 6 Touch sensitive control panel 7 Adjustable feet 8 Chamber door 9 USB port 10 Power supply switch 11 Mains power inlet for coater 12 Argon gas inlet 13 Nitrogen gas inlet 2 a b 10 11 12 13 1 3 4 5 6 7 8 9 ...

Страница 22: ... setup location bear in mind that the system weighs approx 70 kg All feet have to be adjusted and counter locked to maintain level and stable positioning When moving the coater make sure to lift it up The membrane pump sits on 4 legs to absorb vibrations which should not be dragged The instrument must be placed on the bench in such a manner to allow access to the mains switch and mains plug at any...

Страница 23: ...perating Manual Leica EM ACE600 Version 01 19 Page 18 3 5 Unpacking and connection The Leica EM ACE600 coating system should be transported with a forklift truck Lift up the outer box Remove top foam lid ...

Страница 24: ...EM stubs 4 Carbon thread 5 Covers for the motorized stage connections 6 Back plate for the internal shielding left bottom 7 Back plate for the internal shielding right bottom 8 Electrodes for glow discharge 9 Quartz head and crystals 10 Springs for the shutter 11 Torx key and brush for the carbon thread head 12 Bayonet ring for sputter target 13 Shutters Remove the accessory box and all protection...

Страница 25: ...or hands and place it on a table Two strong people are required to lift the coater Place the Leica EM ACE600 on a stable bench Adjusted all feet and counter lock flat spanner 13 mm to maintain level and stable positioning Connect mains cable If venting with nitrogen gas connect to nitrogen gas supplied hose 6 mm diameter Regulate nitrogen pressure to 0 5 bar over atmosphere ...

Страница 26: ...ct to argon gas supplied hose 6 mm diameter Purge argon line before connecting to remove the air from inside the hose This can help to reduce the pump down time Regulate argon pressure to 0 5 bar over atmosphere We strongly recommend using a two stage pressure regulator on the argon bottle ...

Страница 27: ...g take the main shielding out of the vacuum chamber and place it on a clean surface Start with placing the glass shielding for the chamber light in the main shielding A pack of 100 glass shields is included in the delivery Take out the main shielding and unscrew the screw on the top middle of the chamber shielding which holds the part to separate and close the gap between the two shutters ...

Страница 28: ...nual Leica EM ACE600 Version 01 19 Page 23 Take out the metal holder Put in a glass shield or take out the coated round glass and replace it with a new one Put the metal bar back to its spot and screw it on gently ...

Страница 29: ...te of the shielding out of the packaging 3 flat sheets The three plates fit together in the rear of the coater like as shown here The first shield goes into the right top corner of the rear of the coating chamber Align hole to the pin on the chamber wall and push on 1 2 3 1 ...

Страница 30: ... top left corner of the chamber wall The pin on the second shield holds the third shield The third shield covers the bottom of the rear of the coating chamber Make sure the back plates are firmly pushed against the back wall of the coating chamber otherwise the shutter could be stuck 2 3 ...

Страница 31: ...ithout 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 see picture on previous page in the middle of the rear of the coating chamber by the thumbscrew Tighten firmly 1 2 3 4 ...

Страница 32: ... cable through the recesses on the shutter 1 and plug in the connection 2 Slide the extra packaged shutter spring 1 on to the pin on the shutter 2 Instrument on this picture equipped with two sources For an instrument with two sources repeat the same for the installation of the second shutter 1 2 1 2 ...

Страница 33: ...on The Leica EM ACE600 is equipped with quartz crystal film thickness measurement The QSG equipment for installation includes Quartz head with cable 1 Quartz crystals 2 Unscrew the cover of the quartz holder Place a quartz crystal on the copper springs 1 the grey part facing downwards 2 2 1 1 2 1 ...

Страница 34: ...ersion 01 19 Page 29 Replace the cover and tighten gently Slide quartz 1 from the top through the hole 2 in the middle of the stage Push the quartz head down until it firmly sits on the stage Quartz is placed correctly on the stage 1 2 ...

Страница 35: ...8 1 do not forget to change the settings from quartz on stage to quartz on side as described in 4 1 Changing the quartz crystal should be done when the quartz holder is not mounted This is to prevent any unintentional turning of the head against the cable which can lead to a broken cable 3 8 1 Eccentric quartz holder When installing the holder to place the quartz on the side of the stage please ma...

Страница 36: ...y the stage will slide in Do not forget to change the quartz settings from stage to side see 3 1 1 Minimum required working distance is 80mm and the measurement is calibrated to 0 tilt Note for sputter processes When using the side settings for the quartz Argon pressure of 2x10 2 to 9x10 3 mbar or lower should be used for the sputtering Above the measurement is less accurate ...

Страница 37: ...ready installed The stage distance from the source can be set between 30 and 100 mm the maximal tilt is 60 When tilted the range for the stage distance is limited to 45 to 100 mm The stage can hold up to 24 SEM stubs A stage for two glass slides or a planetary drive stage is available as an option which is easily installed by exchanging the table Cover the connections of the motorized stage with t...

Страница 38: ...talled stage Make sure the pin 1 on the stage and the hole with O ring on the table 2 connect Motorized stage 1 with table 2 to load up to 24 standard 12 7 mm 1 2 SEM stubs with a pin diameter of 3 2 mm The optional table is used for two 76 mm x 26 mm 3 x 1 standard glass slides 1 2 1 2 ...

Страница 39: ...e until the pin on the table connects with the hole on the stage Then gently tighten the small thumbscrew 1 Table installation is the same for motorized and rotating stage The following images illustrate the tilt and height adjustment for a rotating stage It is important to always have all planets placed on the planetary drive stage when coating samples The planets cover and therefore protect the ...

Страница 40: ...uals 10 degrees Left image The thumbscrew 1 defines how much force is needed to adjust the tilt The screw should not be opened for adjusting Right image Pointer for the scale of the rotating stage to adjust the height each line is 10 mm The rotating stage can be easily exchanged with a motorized stage 1 2 ...

Страница 41: ...Operating Manual Leica EM ACE600 Version 01 19 Page 36 Stage on the lowest position equals to a source distance of 100 mm 1 Tilt adjustment 2 Height adjustment 1 2 ...

Страница 42: ...Sharp pointers may damage the touch screen As an example the main screen of a highly equipped instrument is shown with sputtering 1 e beam evaporation 2 glow discharge 3 and a cryo stage 4 In addition there is a transfer system available 5 Single processes can be put into sequence 6 On the left hand side of the touch screen panel there is always an overview of the pumping and vacuum status shown a...

Страница 43: ...le processes Update 5 is used when a software update is performed The light button 6 operates the chamber light and the Service button 7 gives access to the service environment asking for a password This area is reserved for Leica authorized personnel Log files can be downloaded or deleted and protocols can be uploaded Connect a USB stick to the port on the touch screen panel and select Shows all ...

Страница 44: ...Operating Manual Leica EM ACE600 Version 01 19 Page 39 All stored processes can be exported onto a USB stick and be imported back to the instrument from a USB stick ...

Страница 45: ... fill in the required data specific weight and settings for pre sputtering Tap on a line for copying or editing the material The pre set materials are locked only new ones can be edited Example carbon thread material settings Add a new material and fill in the required data specific weight of carbon and the parameters for pulsing or flashing method Tap on a line for copying or editing the material...

Страница 46: ...z A new quartz has a frequency of 6 MHz and can be used until it shows unstable in the quartz test E g 1 nm carbon is reflected in about 15 Hz reduction 1 nm of platinum refers to around 145 Hz If a side quartz is used it has to be set accordingly on this screen otherwise the thickness calculation is wrong ...

Страница 47: ...n be saved into a USB Stick Additionaly the stage can be set to its initial position The coater is delivered calibrated If the touch seems to lose its accuracy calibrate the screen 4 1 2 Software update Enter the menu connect a USB stick to the port on the touch screen panel and press update Choose from the list which updates shall be performed by pushing the respective button on the select update...

Страница 48: ...ual Leica EM ACE600 Version 01 19 Page 43 It is required to first update the user interface and then the required controllers The update files need to be on a USB stick in a folder with the directory Leica CTupdate ...

Страница 49: ...not closed the 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 or the chamber door is not closed Time can be saved by starting the pump as soon as the sample is placed in the chamber otherwise pumping will start only when a process run is started Also the sputter process can be speed ...

Страница 50: ...ated the coater will automatically run the complete coating cycle At the end of the process the system eithers stays under vacuum or vents automatically vent after process is activated defined within the process parameters Pressing the Stop button will terminate the process after confirmation regardless of the step of the process The system either stays under vacuum or vents automatically vent aft...

Страница 51: ...pulses Flash mode When using the flash mode the process is terminated after the selected number of carbon thread sections has been evaporated The resulting thickness is shown in the process summary For best results and fault free operation only the Leica carbon thread should be used 16771511116 To minimize carbon fiber residues dropping onto the sample we recommend using the Pulse mode rather than...

Страница 52: ...ding a carbon thread The carbon thread can be loaded as a single thread or as a double thread Thin layers from 1 to 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 frames of the coater Fold the thread into half and load it Make sure the instrument is vented se...

Страница 53: ...sh 3 Carbon thread 4 Loosen all 5 clamp screws with the Torx key Remove any carbon thread residue using the brush supplied Do not brush off the threads close to the instrument Use a bin well a side and placed on the floor This avoids fibers to reach the inside of the instrument 1 2 3 4 ...

Страница 54: ...th 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 Pull the thread gently and tighten the last clamp Tighten the remaining 3 screws and trim thread on both ends 1 ...

Страница 55: ...here is a Leica EM ACE600 YouTube video where the loading of the thread can be seen http www youtube com watch v Qj3Y WfNbvM After the carbon thread is loaded replace the head gently tighten the fastening screws and connect the cables and close the cover Do not tighten the screws when the instrument is under vacuum They can t be opened when vented and there is a risk of damaging the thread ...

Страница 56: ...vailable and can be chosen Tapping on the characteristics of the protocol 2 opens the list of recipes There the parameters for the process can be changed and saved Thickness or pulses flashes can be adjusted on the process screen 3 Once everything relevant for the coating process is defined the process can be started 4 Select a protocol by tapping on it Once it is marked by tapping on a specific c...

Страница 57: ...r flashes are done 3 or if the process is finished by a thickness threshold 4 In case the thread was mounted doubled to reach higher thickness the double thread box must be ticked 5 Defining the sample height ensures that the working distance is kept constant The carbon thread source is angled 25 towards the stage Tilting the stage influences the coating angle Rotation can be either set to continu...

Страница 58: ...nd material management Select an existing material or add a new one Set the parameters for the degassing process heat current heat voltage and heat time Pulse power is the value the instrument tries to reach adjusting current and voltage accordingly Time between the pulses and duration of a pulse is defined Flash current and voltage are a limit The flash voltage can be adjusted to desired value 1 ...

Страница 59: ...rds the area below the target and coat the sample This coating process can be more directional sputtering at better vacuum low 10 3 mbar or diffuse more even coating on a bigger surface and fissured samples sputtering at low 10 2 mbar This also influences the coating rate diffuse means slower rate and the grain size directional means finer grains With the quartz thickness measurement QSG the layer...

Страница 60: ...g vacuum Stabilizing plasma Pre sputtering if target requires to clean the target from oxidation and enable a stable sputter rate Starting the sputtering process by opening the shutter and starting rotation if set to rotate Unclean targets can cause plasma instability and therefore abort the process Only using Leica targets can insure problem free sputtering Rotation should be used for the evapora...

Страница 61: ...t by gently tightening the bayonet ring Tighten the ring by hand only There is a Leica EM ACE600 YouTube video which also shows the loading of the target http www youtube com watch v Qj3Y WfNbvM When the target is secured replace the sputter head gently tighten the fastening screws and connect the cable and close the cover 2 3 1 ...

Страница 62: ...r the process screen In the library of recipes 1 all stored protocols are available and can be chosen Tapping on the characteristics of the protocol 2 opens the list of recipes There the parameters for the process can be changed and saved Only thickness can be adjusted on the process screen 3 Once everything relevant for the coating process is defined the process can be started 4 Select a protocol...

Страница 63: ...m as defined for the sputter process are used Pre sputter current is defined under the material file see also chapter 4 1 Defining the sample height ensures that the working distance is kept constant The sputter source is angled 25 towards the stage Tilting the stage influences the coating angle Rotation speed can be set from 1 to 5 equals to 20 rpm Settings can be checked by pushing the Test butt...

Страница 64: ...ch will be adjusted by letting argon gas in Purging flushes argon gas through the tubes into the chamber to clean out other molecules If the focus is on fast coating rather than finest layers a low base vacuum can be set and the turbo pump run in standby The sputter vacuum will be reached much faster in this way Purge cycles Argon is let in for 10 seconds and then pumped for 30 seconds Sputter mat...

Страница 65: ... nm s W 90 60 4 10 8x10 3 50 3 no 2x10 5 3x10 6 0 4 nm s Ir 80 3 10 8x10 3 50 3 no 2x10 5 3x10 6 0 1 nm s Al 100 60 9 60 1x10 2 50 3 no 5x10 5 5x10 6 0 15 nm s Ti 100 60 4 50 1x10 3 50 3 no 5x10 5 5x10 6 0 12 nm s Md 90 60 6 15 8x10 3 50 3 no 5x10 5 5x10 6 0 4 nm s Ni 100 60 10 40 2x10 2 50 3 no 5x10 5 5x10 6 0 25 nm s Cu 60 30 10 50 2x10 2 50 3 no 5x10 5 5x10 6 0 2 nm s Co 100 60 4 50 2x10 2 50 3...

Страница 66: ...lled recess holds a platinum inlet of 2 mm The platinum inlet is either glued into the recess with conductive carbon cement or slightly deformed so it does not fall out of the rod To melt the inlet in the rod is mounted in the same way as for evaporation see protocol below and heated up with the degassing process For low angle rotary shadowing applications two extra stages including a holder to mo...

Страница 67: ... steps automatically see 3 9 2 and 3 9 3 Pumping Pumping until base vacuum is reached Setting the stage Degassing the target material if activated Opening the shutter and starting rotation if activated Evaporating until final thickness is reached or defined time has elapsed Closing the shutter Displaying the results of the process venting or staying in vacuum Caution Be careful when reloading a ju...

Страница 68: ...ts delivered with the e beam source one for the 3 mm carbon rod 1 and one for the 2 mm carbon rod for a platinum inlet 2 Make sure the instrument is vented Open the source cover 1 Unplug the connectors 2 Unscrew the 2 evaporation head screws to remove the flange 3 Prepare the following parts on a clean desk 1 2 3 1 2 ...

Страница 69: ...ource 4 Special tool to push out the carbon rod from the collet 5 Alignment tool for the tungsten filament 6 Wrench size 5 for exchanging for the collet 7 Allen key size 2 for opening the Wehnelt cylinder 8 Allen key size 3 for exchanging the tungsten filament 1 Carbon rods 2 Tungsten filaments 3 Carbon rods for platinum 4 Platinum inlets Place the e beam source on a clean table 1 2 3 4 5 6 7 8 1 ...

Страница 70: ...rating Manual Leica EM ACE600 Version 01 19 Page 65 Use the special tool to unscrew the holding ring Remove the holding ring and place the holding ring next to the e beam source Holding ring e beam source ...

Страница 71: ...to get the e beam source out of the housing When the source is hot separate the rod and the e beam source after taking it out Due to the heat expansion it could be permanently stuck together For easy further operation the e beam source can be placed into the holding ring Open the screw to access the filament and target The filament can be seen through this window ...

Страница 72: ...ise the Wehnelt cylinder is stuck on the tungsten filament The placement of the target can be seen when adjusted through the window The tip of the carbon rod should be in the middle of the coil Same for the platinum tip To adjust the rod turn the collet holder on the bottom of the e beam source ...

Страница 73: ...t compressed air oil and water free can be used to blow through the hole Thorough cleaning with scotch brite sandblasting or similar is recommended every time the filament is changed Filaments are not changed preventively their lifetime varies a lot They are changed when they cannot stabilize the evaporation anymore ...

Страница 74: ...00 Version 01 19 Page 69 To change the filament the Wehnelt cylinder has to be removed by opening the two screws on the top Take out the screws and lift up the Wehnelt cylinder Carbon rod 1 inside the tungsten filament 2 can be seen ...

Страница 75: ...ting Manual Leica EM ACE600 Version 01 19 Page 70 To change the carbon rod screw out the collet holder If the carbon rod is stuck in the collet there is a pin available to push it out from the back side 1 2 ...

Страница 76: ...Operating Manual Leica EM ACE600 Version 01 19 Page 71 To prepare a carbon rod take a new rod and cut it in half Use a razor blade to score the middle After scoring the surface it can be broken in half ...

Страница 77: ... To prepare a carbon platinum rod take a new 2 mm carbon rod with recess and a platinum inlet Method 1 Take some pliers and bend the round platinum into a slightly oval shape Then put the inlet into the carbon rod If bent enough the inlet stays in the rod ...

Страница 78: ...Operating Manual Leica EM ACE600 Version 01 19 Page 73 Method 2 Take some fibers of a carbon thread and place them on the platinum pellet Push the carbon rod on the pellet Some fibers will stick out ...

Страница 79: ...lint free paper over the surface will remove all the fibers The platinum pellet is now fixed into the rod and ready for melting in Method 3 Glue the pellet with some carbon cement into the carbon rod A tooth pick or similar and forceps are needed Apply some carbon cement ...

Страница 80: ...n Clean the squeezed out cement with a tissue The platinum carbon rod is prepared for melting in degassing image shows a melted in rod When changing from carbon evaporation to platinum or the other way round the collet is screwed out of the collet holder Usually this can be done by hand In case it is too tight the wrench number 5 is used ...

Страница 81: ...Operating Manual Leica EM ACE600 Version 01 19 Page 76 ...

Страница 82: ... Manual Leica EM ACE600 Version 01 19 Page 77 Take the prepared rod and push it into the collet Fix the rod with the collet ring To exchange the tungsten filament loosen the two screws clamping the filament down ...

Страница 83: ...ne Place the centering rod and tighten the clamping screws Try to avoid tension in the filament When the tungsten coil is fixed take out the centering rod Screw in the collet holder with the carbon rod Tungsten coil and target are loaded Make sure the spacers are in place before mounting the aperture ...

Страница 84: ...on 01 19 Page 79 Put the Wehnelt cylinder on top and fix it with the two screws Make sure the window is closed Screw in the rod to hold the e beam source align the pins of housing and e beam source and put the e beam source into the housing ...

Страница 85: ...eam protocol When the head is inserted after completing the preparation in 3 8 1 an evaporation process can be run Select e beam at the first screen to enter the process screen In the library of recipes 1 all stored protocols are available and can be chosen Tapping on the characteristics of the protocol 2 opens the list of recipes There the parameters for the process can be changed and saved Only ...

Страница 86: ...s 1 by ticking or un ticking the quartz usage box 2 Ticking the degas box 3 has the effect that the target material is heated up for cleaning before evaporation is done shutter stays closed Degas parameters are stored in the material file The target power will influence the coating rate 4 Stage allows setting a coating angle or tilt of the stage When setting a coating angle the tilt is automatical...

Страница 87: ... the horizontal table to the Wehnelt cylinder 4 8 3 Parameter suggestion e beam coating Carbon Density 2 25 g cm3 Quartz 15 Hz nm Degassing 75W 1 5kV 50mA 5min Evaporation 150W 1 8kV 80mA Platinum Carbon Density 19 45 g cm3 Quartz 130 Hz nm Outgassing melting in 50W 1 0kV 50mA 2min Evaporation 100W 1 6kV 60mA Carbon should be operated between 90 150 W Platinum between 60 100 W ...

Страница 88: ...01 19 Page 83 4 8 4 E beam material New e beam materials can be defined Open Menu tab file and material management Select an existing material or add a new one Density is the specific weight g m3 of the material Set if degassing power and time ...

Страница 89: ...with quartz measurement to enable a reproducible result Accessories delivered with the instrument 1 2 5 Allen key 2 Brush to remove loose carbon 3 Special tool for mounting the carbon rods 4 Special tool keep the carbon rod evaporation source open for mounting 5 Carbon rod sharpener 6 Copper clamps for carbon rod 7 Special holding tool for the carbon rod clamps 8 Special tool to hold the carbon ro...

Страница 90: ...taying in vacuum 4 9 1 Loading a carbon rod Make sure the instrument is vented see 4 2 Open the source cover Unscrew the two evaporation head screws 1 to remove the cover 2 The evaporation head 3 stays mounted in the instrument it is only removed for extended cleaning Note Make sure the copper band is not in contact with any other part In case it can be easily adjusted by hand For regular cleaning...

Страница 91: ...l for mounting the carbon rods 4 Copper clamps for carbon rod 5 2 5 Allen key 6 Carbon rod sharpener 7 Special tool to hold the carbon rod for sharpening 8 Special holding tool for the carbon rod clamps To prepare a carbon rod take a new rod and cut it in half approximately Use a razor blade to score the middle After scratching the surface 1 2 3 4 5 7 8 6 4 ...

Страница 92: ...ack into stock and mount the other one in the copper clamp Take a new rod and fix it in the holding tool to grind a sharp tip Turn the carbon rod holder in circles until the top is sharp Flatten the tip to about 1 mm diameter This will allow an exact positioning against the flat rod for evaporation ...

Страница 93: ...in the first copper clamp 2 As shown on the image a rod which cannot be used for the sharp tip anymore can still be used on the flat side On the shorter side 1 mount the flat rod aligned with the edge of the recess On the longer side 2 mount the pointy rod the tip aligned with the edge 1 2 ...

Страница 94: ...ugh the rod can slip through the connection between tip and flat part will not be under spring force and evaporation is not possible When taking out a rod to exchange and or sharpen it open the screw 1 and push down The clamp will open and the rod can be easily taken out Use the special tool to keep the carbon rod evaporation source spring loaded open 1 2 1 ...

Страница 95: ... in the evaporation source Make sure the clamp 2 sits straight in the recess and firmly tighten the screw It is recommended to start with the flat rod on the front side in respect to the instrument When the second rod is mounted in the same way the tool which keeps the evaporation source open is removed 1 The two rods should push against each other 2 1 2 1 2 ...

Страница 96: ...osing a carbon rod protocol When the head is inserted after completing the preparation in 4 9 1 an evaporation process can be run Select evaporation on the first screen to enter the process screen In the library of recipes 1 all stored protocols are available and can be chosen Tapping on the characteristics of the protocol 2 opens the list of recipes There the parameters for the process can be cha...

Страница 97: ...nes if the coating process is finished by a time or certain thickness 1 by ticking or un ticking the quartz usage box 2 Using the quartz allows to set a time between 20 and 3600s The voltage will be increased gradually until set thickness is reached In the example below this means reach 5nm in 60 seconds the voltage is increase 16 67 mV from 5 2V to max 6 2 V until the 5nm are reached for informat...

Страница 98: ...e is kept constant The carbon thread source is angled 25 towards the stage Tilting the stage influences the coating angle Rotation speed can be set from 1 to 5 equals to 20 rpm Settings can be checked by pushing the Test button Init stops the testing and moves the stage to the init position A vacuum is set which needs to be reached before the coating process starts base vacuum 1 2 3 ...

Страница 99: ...aterial file under method 1 Density is the specific weight g m3 of the material Select a material by tapping on it Once it is marked by tapping on a specific category the parameters can be changed Alternatively a material can be copied and then modified or a new one added The default materials are locked and cannot be overwritten 2 Screenshot for the parameters under Method 1 2 ...

Страница 100: ...r choosing a protocol the system will perform the following steps automatically Pumping until process vacuum is reached Letting in air to adjust vacuum to set pressure Stabilizing vacuum and starting glow discharge with closed shutter purple plasma is visible Termination of glow discharge process by the set time Displaying the results of the process Venting or staying in vacuum 4 10 1 Choosing a g...

Страница 101: ... discharge option ensures that the glow discharge electrode is mounted Select a protocol by tapping on it Once it is marked by tapping on a specific category the parameters can be changed Alternatively a protocol can be copied and then modified or a new one added 1 2 4 3 ...

Страница 102: ... the length of it Defining the sample height ensures that the working distance is kept constant The glow discharge source is angled 25 towards the stage Rotation speed can be set from 1 to 5 equals to 20 rpm Settings can be checked by pushing the Test button Init stops the testing and moves the stage to the init position ...

Страница 103: ...ow discharge process please make sure the electrode is cleaned regularly especially when sputtering thicker layers 4 11 Sequence Single processes can be combined into a sequence Depending on the configuration of the instrument sputtering evaporation processes and glow discharge can be automatically run one after the other If hardwear is present transfer processes can be included in a sequence They...

Страница 104: ...haracteristics of the protocol 2 opens the list of sequences There the sequence can be changed and saved Once everything is defined the processes can be started 3 Select a protocol for a sequence by tapping on it Once it is marked by tapping on the name or included processes the details can be changed Alternatively a sequence can be copied and then modified or a new one added 1 2 3 ...

Страница 105: ...01 19 Page 100 The total sequence can run over several screens change by button 1 Tapping on add a new process can be implemented into the sequence First the method is selected then the specific protocol and then the position in the sequence 1 ...

Страница 106: ...Operating Manual Leica EM ACE600 Version 01 19 Page 101 Mark a step in the sequence to modify it Tapping on an already implemented process allows changing the process itself or moving the position 2 1 ...

Страница 107: ...M ACE600 Version 01 19 Page 102 4 12 Rotating stage difference in user interface and set up Rotating stage is indicated in the stage editing screen 1 It is important to set the height and tilt before starting the process 2 1 1 ...

Страница 108: ...rface of the stage 4 13 Running a process Once a process is started as example here e beam the instrument automatically runs through all the steps including setting the stage stabilizing the process coating and post processing when quartz measurement is activated Tapping on the process box Carbon in this case shows the most important parameters of that process ...

Страница 109: ...Operating Manual Leica EM ACE600 Version 01 19 Page 104 While the sample is coated the average coating rate 1 as well as the current thickness 2 and the thickness to be achieved 3 is displayed 2 1 3 ...

Страница 110: ...ayer thickness during evaporation to stop when the desired value is reached This includes a correction for the influence of the light radiation onto the quartz crystal However at the end of the process the quartz reading is again taken after waiting a suitable time to avoid any influence of the radiation and is then compared to the reading before starting the deposition The result is given at the ...

Страница 111: ...eeded base vacuum is already reached Also is it beneficial when using targets which corrode This way they do not have to get into contact with air when the coater is vented for removal of the sample VCT holders up to four have to be used to transfer the sample into the coater with the load lock Mount the VCT holder carrying the sample on the load lock manipulator tip 1 Attach the load lock to the ...

Страница 112: ...mounted on a VCT holder to be transferred A table which can receives up to four VCT holders is part of the outfit With the buttons 1 to 4 1 the stage can be moved to that position to receive the transferred holder Settings 2 allows adjusting the pump and purging time of the load lock as well as closing and removing the cover of the VCT dock Push load lock 3 to attach the load lock open the gate va...

Страница 113: ...l Leica EM ACE600 Version 01 19 Page 108 In case the stage must be aligned to transfer the VCT holders push Adjust and align height 1 angle 2 and tilt 3 Set will save the values for the respective position 1 2 3 1 2 3 ...

Страница 114: ... open 2 and the load lock manipulator rod is inside the vacuum chamber After placing all the samples up to four the load lock manipulator has to be pulled out It is recommended to close the gate valve after finishing load lock manipulation With the button Vent the gate valve is closed 1 2 ...

Страница 115: ...rther questions regarding malfunctions refer to the error list under chapter 5 Example Caution Injuries or damage to the system may be caused by servicing and cleaning the system incorrectly 5 1 General instructions for maintenance and cleaning External elements dust grease etc may prevent achieving the required vacuum When working on the vacuum chamber or parts which are in the vacuum chamber of ...

Страница 116: ... If contamination is observed during EM imaging Pumping time to reach base vacuum increases significantly All coating sourced should be cleaned as as soon as there is Clearly seen a thicker film of coating on the source The risk that material could peel off Latest when material starts to peel off Thin threads can peel off the anode ring and cause a short circuit Recommendation Usually only the gla...

Страница 117: ...er and letting them dry off is an easy way to finish the cleaning In addition Isopropanol or Ethanol can be used for the finish Caution Do not use thin tissues and ethanol for removing platinum there is a risk of the tissue catching fire Door Remove the door by lifting it from its hinges see 4 2 1 Place the door on a flat soft surface with the inner surface up To remove carbon coatings use a 70 is...

Страница 118: ...ite or metal cleaning paste Finish with soap water and then clean with water or isopropanol It is available as a spare part Anode ring The anode ring is implemented in the opening for the sputter head It can be removed by pushing downwards when the internal shielding is removed see 3 6 Occasionally it can happen that an elongated flake builds up by the sputtered material This can cause a shirt cir...

Страница 119: ...beam ceramic If necessary clean the ceramic 1 of the collet holder 2 Cleaning is required when no deposition rate can be achieved even though rod and filament are functional A dark film can be seen on the ceramic This is more likely to happen for a platinum source than a carbon source Cleaning can be done with sandpaper or sandblasting Housing All surfaces can be cleaned with a damp lint free clot...

Страница 120: ...ved immediately with a damp lint free cloth moistened with aqueous cleaning agents 5 2 1 Removing and cleaining the door with a metal polisher To remove the door lift it up and take it out Place the door flat on a soft surface to clean Do not use abrasive cleaning material Scratches could cause a vacuum leak The complete glass can be exchanged by unscrewing both screws on the side to hold the glas...

Страница 121: ...scharge electrode and loosen the cable Unscrew the shutter and take it out This process is clearly described under 3 6 and 3 7 For removing the process only needs to be reversed 5 2 3 Exchanging the glass shielding for the chamber light To exchange the glass shielding for the chamber light please refer to 3 6 Before first use please install a glass shielding When the chamber light becomes too dark...

Страница 122: ...CB W0003 Warning Cannot load configuration file Configuration cfg ini not loaded correctly Auto repair in software when restarting W0004 Warning Specific image is missing Specific image could not be loaded Maybe UI update process went wrong W0005 Warning Cannot load method related file Unable to load method related file Processes and sequences not detected W0006 Warning Service interval diaphragm ...

Страница 123: ...tem No available coating method controller detected Check communication cables and HiVac controller status W0014 Warning Service interval gauge exceeded Service gauge Gauge service interval exceeded Reset interval in software after service W0016 Warning Gauge pressure out of bounce Restart system Invalid gauge pressure value received Check gauge connection or restart controller E0017 Error Sudden ...

Страница 124: ...uarantee valid measurement Change quartz in case and try to run process again E1600 Motor error Shutter motor error detected Initialization of shutter motor failed Try re initialization and learning E1601 Motor error Shutter motor not connected Check cable and restart system Shutter motor not detected during software init Restart or check cable connections E1700 Motor error Rotation motor error de...

Страница 125: ...ing of threads available of flashes not possible Process stopped Amount of existing threads smaller than desired number of flashes E4011 Process Process terminated no power detected Check door and cover Process aborted Carbon Thread supply not powered Check door and cover sensors E4012 Process Process terminated Main supply voltage fault Check door and cover Process aborted Carbon Thread mains rel...

Страница 126: ...ircuit because of invalid assembly of head ring or target Check deposited solid material on shutter E2010 Process Process terminated ignition fault Check argon flow Check target and sputter source Process aborted Unable to establish plasma ignition E2011 Process Process terminated Sputter current could not be stabilized Process aborted Unstable plasma current Unclean target could be the reason cle...

Страница 127: ...a current Cryo Controller Specific E8002 Process Process terminated Unable to reach desired temperature Check N2 Dewar empty Process aborted Reaching reference temperature timeout E8003 Process Dewar empty E8004 Process Etching Temperature lower LN2 empty VCT Specific E1401 Process VCT Transfer Terminated Stage Initialization Timeout E1402 Process VCT Transfer Terminated Stage Position Incorrect E...

Страница 128: ...nnected E1411 Process No Shuttle Connected W1412 Process Shuttle Already Under Good Vacuum P X mbar E Beam Controller Specific E9001 Warning E Beam supply already switched on Process aborted Could not switch on power due power is still active E9002 Warning Invalid high voltage value Set valid parameter and try again Process aborted Invalid parameter voltage sent E9003 Warning Invalid current value...

Страница 129: ...nt Process aborted Change filament Filament broken or short circuit inside head clean source E9011 Process Process terminated E beam voltage current not stabilized Process aborted Voltage current not stabilized Restart process or check source E9012 Process Process terminated Operation response timeout Process aborted Communication response timeout occurred Unable to stabilize or comm Error Restart...

Страница 130: ...device service device tab E5007 Process Process terminated insufficient contact in source Check source mounting Process aborted Resistance too high Contact insufficient Check source mounting rod E5008 Process Process terminated short circuit in source Check source mounting Process aborted Resistance too low Short circuit or change rod E5009 Process Source Exhausted Contact Loss E5010 Process Sourc...

Страница 131: ... der Richtlinie conformément aux dispositions de directive Electromagnetic compatibility Elektromagnetische Verträglichkeit 2014 30EU Low Voltage Equipment Niederspannungsrichtlinie 2014 35EU RoHS directive RoHS Richtlinie 2011 65 EU declares in exclusive responsibility that the product erklärt in alleiniger Verantwortung dass das Produkt déclare sous sa responsabilité que le produit Model Modell ...

Страница 132: ...Leica Mikrosysteme GmbH Vienna Austria T 43 1 486 8050 0 F 43 1 486 8050 30 www leica microsystems com CONNECT WITH US ...

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