Dielectric Evaporator Procedure Rev
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1 Wisconsin Center for Applied Microelectronics 1550 Engineering Drive Phone: 608/ Madison, WI Dielectric Evaporator Procedure Rev Material Restrictions: All materials on your sample must be on the allowed materials list for this tool before using it. NO EXCEPTIONS. It is the user s responsibility to make sure that the material(s) they are putting in a tool is on the allowed materials list for that tool. Here is how to check the Allowed Materials list for WCAM tools: 1. Go to WCAM s website at: 2. Click on the Chemicals in the Lab link. 3. Click on the link at the top of the page LIST OF APPROVED MATERIALS. 4. Scroll thru the document to find the tool you want to check the materials list for or hit Ctrl + F to bring up a search bar for the document and type in the tool s name that you want to check the materials list for. 5. If the material(s) that you want to use in a tool are not on the approved list for that tool you may not put your sample in the tool. If you have no other way to process your sample and think it makes sense to use a particular material in a tool you may request that it be added to that tool s material list by filling out the form on the Chemicals in the Lab webpage listed as New Material Request Form. Then your material request form along with a MSDS for the material to the WCAM lab manager. The request will be reviewed by the WCAM advisory committee and you will get an back from the lab manager approving or denying your material request for a particular tool. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 1 20
2 Using FOM with the Dielectric Evap System: Users that have scheduled the tool will login at the start of their work. If you fail to show up within 30 minutes of the start of your reservation the system will release your reservation and the tool is available for scheduling or immediate use. Use of the tool in this case by a walkup user or new reservation must be completed before the next reservation. The login to the VACUUM session lets others know that you are in the system. If you load the system with your work and fail to log into FOM the tool is considered to be available after 30 minutes of the reservation start or immediately if no reservation was made. Another user can use the tool as long as their work is completed before the next reservation. If you are the user that opens the system and finds that another user is in the system, try to locate the user and have them remove their material so that you can use the system or contact the lab Staff. Do not run past your reservation if another user s reservation follows. Respect the other user s needs and finish in the time that was allowed. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 2 20
3 Safety: 1. Emergency Power Off 1.1. If during operation an emergency occurs, the emergency power off button is located on the upper left of the control panel This will turn off the power to the entire system. 2. E-Gun 2.1. High Voltage will exist in the Chamber Make sure Power for the E-gun is OFF and locked OFF on the Telemark power supply before working inside the chamber Make sure to check with the grounding rod before working in the tool chamber. 3. Pinch points 3.1. Keep hands clear of the chamber door seal when opening and closing. 4. Hot Surfaces and Components 4.1. During the operation of the heater or targets, surfaces and components will heat up. Make sure you follow the cooling times for these since they will cool slower in a vacuum than you would think of outside of the vacuum chamber. 5. Viewing Source material 5.1. When viewing the hot and very bright source material in the hearth, wear proper eye protection. Dark welding goggles are available at the tool. 6. Personal Protection Equipment (PPE) 6.1. Wear all of the required PPE while operating the tool Make sure your gloves are clean and free of all oils and contaminants. Requirements: 1. Do not operate the tool unless trained and certified to. 2. Do not log in for another user to operate the tool. 3. Follow the procedures contained in this document. 4. Notify staff of any issues with the tool or process. 5. Do not exceed deposition thicknesses of 800nm. 6. Do not introduce materials into the tool that are not in the allowed material list and make sure that all coatings that are allowed are fully baked and cured. The only metals allowed as source material are Ti, Cr and Si for adhesion layers that are < 10nm in thickness. 7. Kapton tape is not allowed in the system to mask or hold samples. 8. Use only sample holders approved for the tool. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 3 20
4 Operation Log: 1. Please fill out as you process. 2. Date Date you are using the tool. 3. User Your Name 4. Time IN Time when you started using the tool. 5. Time OUT Time when you are done with the tool. 6. Pump Start Time after loading sample that you started the Auto Pump Down 7. Base Pressure Pressure system pumped down to prior to Dep. 8. Seq# is the order you did depositions or deps. and heat cycles 9. Material Used/ Htr Record what target was used or if heater was used. 10. Thickness _ Thickness in nm that you deposited. 11. Dep Rate Record if you know what it is for the conditions used. 12. Current Record the current used for the evaporation. DIELECTRIC EVAP LOG HGilles Rev-00 DATE USER Reservation: 8am 11am 2pm 5pm 8pm 11pm 2am 5am Contact # Time IN Time OUT PUMP START BASE PRES. SEQ MATERIAL THICKNESS DEP RATE CURRENT Material Location HH:MM HH:MM HH:MM Torr # USED nm A/Sec ma 1 Comments: 2 3 HTR Temp: Time: DATE USER Reservation: 8am 11am 2pm 5pm 8pm 11pm 2am 5am Contact # Time IN Time OUT PUMP START BASE PRES. SEQ MATERIAL THICKNESS DEP RATE CURRENT Material Location HH:MM HH:MM HH:MM Torr # USED nm A/Sec ma 1 Comments: 2 3 HTR Temp: Time: DATE USER Reservation: 8am 11am 2pm 5pm 8pm 11pm 2am 5am Contact # Time IN Time OUT PUMP START BASE PRES. SEQ MATERIAL THICKNESS DEP RATE CURRENT Material Location HH:MM HH:MM HH:MM Torr # USED nm A/Sec ma 1 Comments: 2 3 HTR Temp: Time: D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 4 20
5 Pre-Run Check: 1. Ensure that the Cryo Pump is on. The temperature should read < 20 K. 2. Ensure that the CVC AVC-485 is in AUTO mode. 3. Ensure that the water-cooling is turned off. 4. Check the logbook and FOM to see if there are issues with the tool recorded. 5. Check the chamber pressure with the Ion Gauge to see if the pressure is < 2E-6 torr Verify that the chamber is at vacuum before turning on the Ion Gauge by checking the chamber pressure on the Vacuum Gauge on the AVC On the Ion Gauge Controller, press and release the top part of the FILAMENT ON/OFF switch to turn ON the filament If it is not <2E-6 torr, there may be a problem with the tool. Check the logs to see if the tool was recently vented and not enough time has passed to produce a good low pressure If you feel there is a vacuum problem with the tool, contact the Staff. 6. Check to see if there are spare Alloy crystals for the thickness monitor. 7. Check to see if there are clean replacement mirrors. 8. Check the source material that you plan to use to verify that it is in a useable state. 9. If you feel there is problem with the tool contact the staff. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 5 20
6 Venting the Tool: 1. Turn off the ionization gauge if it is on On the Ion Gauge Controller, press and release the top part of the FILAMENT ON/OFF switch to turn off the filament. 2. Press VENT on the left of the Automatic Valve Control. 3. After system reaches atmosphere, the GREEN lamp on the front panel will light. 4. The chamber door can now be opened. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 6 20
7 5. CAUTION Potential High Voltage present! 6. Verify the High Voltage Supply is OFF and Key Lock is in OFF position. 7. Check that there is no High Voltage by using the grounding rod to touch the high voltage leads and a chamber shield. Mounting your sample with the allowed fixtures: 1. There are several fixtures that can be used to hold your sample in the system inch wafers inch to 2 inch adapters inch wafers 1.4. Small sample (not wafers) Holder with clips Holder with screws Add pictures 2. Add your sample to the holder and verify that it is secure when it is held upside down in the fixture for deposition. 3. Install the holder into the upper rack of the system. Add Picture D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 7 20
8 Crystal Monitor: 1.1. Check the life of the Crystals. There are two in this system Change the Crystals for the Crystal Monitors if they show >15% life The Crystals are the Metal Alloy crystals (gray/silver color). Crystal monitor #2 (Upper) Crystal monitor #1 (Lower) D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 8 20
9 Replace the Mirror if needed: 1. Slide (to the right) out the old mirror. 2. Dispose of the old mirror in the sharps container. 3. Slide in a new mirror. 4. Verify that you can see the source material in the crucible when look at the mirror from the door window position. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 9 20
10 Install Source material: 1. Verify that you have the correct material and that it is in good shape for the deposition. 2. Install the materials in the pockets of the hearth using either method pictured below. 3. Note the location of the materials so that you can rotate to the correct material for your film stack. 4. Note the location of the Handle to rotate the pockets when the Crucible is in the proper position. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 10 20
11 Pump down: 1. Check the door seal for contamination and wipe the o-ring if needed. 2. Close the door and close the door latch. 3. Using the controller labeled CVC AVC-485: 3.1. Press START on the Automatic Valve Control to start the pumping sequence Wait (typically <1 hour) for the system to reach a low base pressure of less than 2.1e When the system has been pumping for about 10 minutes and the Chamber TC gauge shows that the pressure is zero, the base pressure can be checked on the Ion Gauge Controller Press the FILAMENT ON/OFF switch to light the filament Read the pressure on the display above the switch Record in logbook. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 11 20
12 Program the Rate Monitor #1: 1. Turn ON the POWER switch on the XTC front panel if it was turned off. 2. Press PROG to enter the program mode enter the 2.2. The cursor should now be at Z-RATIO. Using the numeric keypads enter the z Advance the cursor until TOOLING FACTOR #1. Ensure that the tooling factor is correct. If not, using the numeric keypads enter the tooling factor then press E 3. Press PROG to exit the program mode. 4. Press STOP and RESET. 5. Press MPWR on the XTC to use the manual power control. It should read MANUAL in lower right corner of display. Program the Deposition Monitor #2: 6. Turn ON the POWER switch on the XTC front panel if it was turned off. 7. Press PROG to enter the program mode enter the 7.2. The cursor should now be at Z-RATIO. Using the numeric keypads enter the z Advance the cursor until TOOLING FACTOR. Use TF #2 from the table at the end of this SOP. Ensure that the tooling factor is correct. If not, using the numeric keypads enter the tooling factor then press E Advance to the Final Thickness and enter the thickness that you want to deposit for the layer, then press E. 8. Press PROG to exit the program mode. 9. Monitor #2 will be used to open the shutter at the start of dep. and it will close the shutter when the thickness programmed is deposited. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 12 20
13 Setting the Oxygen background Optional Some Oxides deposited benefit from the deposition being done in a vacuum with a low level of oxygen introduced to the chamber. You should review deposition conditions for your material to see if this is needed. Once the system is pumped down to < 2E-6 torr: 1. Open the Oxygen Isolation Valve. MKS Flow ON MKS Flow Adjust O2 Isolation Valve 2. Turn ON the Oxygen flow on the MKS 246 controller for Oxygen. 3. Increase the Oxygen flow slowly till the Chamber pressure is in the range of 2 to 4E-5 torr Monitor the cryo pump temperature. It should not rise above 25 deg. K If the cryo temp exceeds25 deg. K., turn off the Oxygen and contact the tool owner. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 13 20
14 Deposition Options and Adjustments: The control of the deposition thickness can be done totally manual or it can be slightly automated using the Rate Control Monitor. Manual Control: The Shutter Control is in the Manual position and the Shutter Switch will be used to manually open/close the shutter. 1. Start with shutter closed 2. Start the heating and adjustments in the Deposition Process to set the desired rate (A/sec). 3. Zero the thickness on the Controller. 4. Open the shutter with the Switch. 5. Close the shutter when the desired thickness is reached. 6. Reduce the heating of the source in the Deposition Process. Semi-Automatic Control: The Shutter Control is in the Inficon Remote position and the Shutter will be run by Rate monitor controls. 1. Start with the shutter Closed. 2. Press CLOSE on the controller. 3. Start the heating and adjustments in the Deposition Process to set the desired rate (A/sec). D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 14 20
15 4. Zero the thickness on the controller. 5. When ready to deposit Press OPEN on the Inficon Shutter controller The shutter will stay open till the programmed thickness is reached and then the controller will close the shutter. 6. Reduce the heating of the source in the Deposition Process. Sweep Controls: The beam position and movement are controlled by the Seep Controller. 1. Use the lateral and longitudinal POSITION potentiometer to adjust location of the beam. 2. The AMPLITUDE is the distance range of the e-beam oscillation. 3. The FREQUENCY is the rate of oscillation. 4. Circle or Pattern mode may be used based on the source material needs. 5. DO NOT have the beam sitting in one spot. It must be moving over 1/3 to 2/3 of source material surface or the beam will possibly drill a hole into the crucible or through it. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 15 20
16 Deposition Process: 1. Log in to FOM for the Deposition. 2. Turn ON the Cooling Water. 3. Turn ON the KeyLock on the front of the Telemark Power Supply. 4. Press MAIN POWER ON. 5. Ensure that all of the GREEN INTERLOCK LAMPS are lit. 6. Press the green High Voltage ON push button Observe the proper high voltage reading on the HV meter (typ. 10Kev) If required, adjust using the VOLTAGE ADJUST potentiometer. 7. Ensure the Source Emission Adjust potentiometer is fully counter-clockwise (0). 8. Press the green FILAMENT ON push button. 9. Slowly increase the Source Emission Adjust potentiometer till enough heat is applied so that you can see the source material and beam pattern. 10. Slowly increase the Source Emission Adjust potentiometer to the desired deposition rate (A/Sec). 11. Perform the deposition on your sample by opening the shutter either manually or using the Deposition Monitor Controller. 12. When the desired thickness is deposited close the shutter manually or if the Rate Monitor Controller is used it will close automatically. 13. Slowly decrease the Source Emission Adjust potentiometer to zero. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 16 20
17 14. Turn OFF Filament. 15. Turn OFF the High Voltage. 16. Turn OFF the Main Power. 17. Turn OFF the KeyLock. Cooling: If you are doing only one deposition then let the source cool for 30 minutes before turning off the water. If you are not done and you need to deposit another layer let this source cool for 15 minutes before rotating the turret to the next material. Continue with the ADDITIONAL DEPOSITION section. Additional Layers: 1. Before depositing another layer, wait 15 minutes for the source to cool The cooling time is needed to protect the O-ring seals. Damage will occur and loss of vacuum including filling the chamber with water if the seal is broken. 2. After cooling the source, rotate the hearth to the crucible containing the new material. 3. Ensure the cooling water is on. 4. Reprogram the XTC RATE MONITORS for the new layer. 5. Run the DEPOSITION PROCESS for the new layer. Deposition Completed: 1. Verify that the MAIN POWER is OFF and the KEYLOCK is OFF. 2. Log out of FOM DEP Dielectric Evaporator DEPOSIT. 3. If the Oxygen backfill was used: 3.1. REDUCE the Oxygen setting to zero Turn OFF the Oxygen Flow at the Controller Turn OFF the Oxygen Inlet Valve. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 17 20
18 Venting and Unloading Samples: 1. Venting can begin after the 30 minutes of cooling time. 2. Turn OFF the cooling water. 3. Ensure the Main power and Keylock are OFF 4. Turn Off the filament of the Ion Gauge if it is ON. 5. Press VENT on the Automatic Valve Control. 6. When the system is vented to atmosphere the GREEN Atmosphere light will be lit. 7. Open the chamber door. 8. Check the HV leads with the grounding rod to make sure there is no high voltage present before going into the chamber. 9. Remove your Samples. 10. Remove and store the evaporation source materials. 11. Clean the chamber as needed with wipes or the vacuum cleaner so that it is ready for the next user. Pumpdown and Log Off: 1. Close the chamber door 2. Press START on the Automatic Valve Control. 3. Record final use information if the log book. 4. Log out of FOM for the VACUUM reservation/use. 5. Stay with the system and monitor the pumping. Do not leave till the crossover to the cryo pump is complete. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 18 20
19 Changing the Crystal Sensor OPERATING PROCEDURE Dielectric E-Beam Evaporator To replace crystals, following the instructions below: 1. Grip the back part of the sensor with your fingers and pull it straight out to separate it from the water-cooled front part Pull the crystal holder straight out from the back of the sensor. 2. Remove the ceramic retainer from the crystal holders by pulling it straight out with the crystal snatcher Using the crystal snatcher: 2.2. Insert crystal snatcher into ceramic retainer (A) 2.3. Apply a small amount of pressure. This locks the retainer to the snatcher and allows the retainer to be pulled straight out (B). 3. Turn the crystal holder upside down so that the crystal drops out. 4. Drop a new crystal into the crystal holder with the patterned electrode facing the back and contacting the leaf springs on the ceramic retainer. 5. Put the ceramic retainer back into the crystal holder and put the holder into the front cover of the sensor. 6. Use the crystal snatcher to re-insert the retainer into the holder after the crystal has been changed. 7. Release the crystal snatcher with a slight side-to-side motion. 8. Snap crystal holder back onto the water cooled base. 9. Check that the controller does not show a X-Tal Fail in the bottom right corner of the display. D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 19 20
20 MATERIAL DATA vapor temp C TF # 1 TF # 2 Density Z- Ratio Melt Point C 1.00E E E- 04 Tooling factor g/cc C C C C % % Aluminum Oxide Al2O ## ## 1550 Tooling factor Silicon Si Silicon Dioxide SiO ## ## 1025 Titanium Dioxide TiO ## ## 1300 Titanium Ti Silicon Monoxide SiO ## ## 850 Chromium Cr Tantalum Oxide Ta2O ## ## ## D i e l e c t r i c E v a p o r a t o r P r o c e d u r e P a g e 20 20
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