Glovebox MBraun Glovebox System Standard Operating … · Glovebox – MBraun Glovebox System Standard Operating Procedure 4D LABS Confidential Revision: 1.1 — Last Updated: November

Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6

E [email protected] T 778.782.8158 F 778.782.3765 www.4dlabs.ca

Glovebox – MBraun Glovebox System

Standard Operating Procedure

4D LABS Confidential

Revision: 1.1 — Last Updated: November 28, 2016, Revised by Chris Balicki

Overview

This document will provide a detailed operation procedure of the Glovebox System. Formal Training is re-

quired for all users prior to using the system.

Revision History

# Revised by: Date Modification

0 Chris Balicki 2016/05/20 Document Initial Release

1 Chris Balicki 2016/11/28 Added Appendix E - Glovebox Evaporator Operation

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Table of Contents

Overview.................................................................................................................................................. 1

Revision History ........................................................................................................................................ 1

Table of Contents ..................................................................................................................................... 2

General Information ................................................................................................................................. 3

References and Files ................................................................................................................................. 3

Contact Information ................................................................................................................................. 3

Important Safety Information .................................................................................................................... 4

First Steps Prior to Operation .................................................................................................................... 5

Review Safety Information ................................................................................................................... 5

System Checks .................................................................................................................................... 5

Sample Loading/Unloading ....................................................................................................................... 7

Loading Via Small Antechambers ......................................................................................................... 7

Unloading Via Small Antechambers ..................................................................................................... 8

Loading Via Large Antechamber .......................................................................................................... 9

Unloading Via Large Antechamber .................................................................................................... 10

In Case of Catastrophic Breach or Emergency ......................................................................................... 11

System Shutdown / Startup ..................................................................................................................... 12

APPENDIX A – Solvent Filter (LMF) Regeneration .................................................................................... 14

APPENDIX B – Cleaning the Moisture Sensor .......................................................................................... 16

APPENDIX C – Purification Reactor (RKM) Regeneration ......................................................................... 20

APPENDIX D – Sample Loading/Unloading Via Small Antechambers ........................................................ 23

APPENDIX E – Glovebox Evaporator Operation ....................................................................................... 27

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General Information

The MBraun Glovebox System is a controlled, inert environment workspace with a nitrogen atmosphere

and a rated specification of <1ppm H2O and < 1ppm O2. The system has several antechambers for quick

sample insertion and removal. It also contains a built in 3-source thermal evaporator deposition system and

a basic spin coating system. The glovebox is an ideal workspace for samples that are sensitive to air, oxy-

gen, and moisture.

References and Files

Installation Notes and Vendor Training

MBraun Operating Manual

Contact Information

Questions or comments in regard to this document should be directed towards Chris Balicki (balic-

[email protected]) in 4D LABS at Simon Fraser University, Burnaby, BC, Canada.

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Important Safety Information

The following safety protocols and guidelines are required of all users:

1. Users must not wear any sharp or jeweled hand jewelry while wearing the glovebox gloves.

2. Users must wear disposable safety gloves and safety eyewear when using the glovebox.

3. Users must receive prior approval and consultation from 4D LABS staff for any inbound materials

or work samples.

4. For inbound chemistry, users must follow the 4D LABS New Chemical Approval procedures. This

includes filling out the new chemical intake form(s) and supplying the MSDS(s).

5. Users must report all safety hazards, including but not limited to, chemical spills, tears in the

glovebox gloves, system alarms, and/or any other items/issues that have the potential to be a safe-

ty hazard.

6. Users must remove all items from the glovebox at the end of each session unless otherwise ap-

proved for glovebox storage by 4D LABS staff.

7. Users must contain all potential wastes and spills within the glovebox by using secondary con-

tainment and/or disposable absorbent pads.

8. Unless dedicated waste storage is provided within the glovebox, users must place all waste mate-

rials inside ziplock bags, which in turn must be removed from the glovebox, labelled, and discard-

ed to the nearby glovebox waste bin.

9. For the large antechamber covers, do not overtighten the spindles or tighten them further once

vacuum is reached as this will result in overtightening when the antechamber is repressurized.

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First Steps Prior to Operation

Review Safety Information

Review and follow the safety information provided in this procedure as well as protocol communicated by 4D LABS staff and guidelines listed in relevant MSDS forms. The glovebox system is basically an open bench top in an enclosed inert environment. A wide variety of work may be performed within; however, work and/or experiments must first be consulted and approved by 4D LABS staff. Many of the proposed experiments and tasks will require specific safety consideration in addition to that which is provided in this procedure.

System Checks

1. Verify the glovebox parameters on the main status screen. a. Pressure should be between 1-5mbar. b. H2O should be < 10ppm. c. O2 should be < 10ppm. d. Box 1 and Box 2 should be active (green). e. LMF, VPG, RKM, and GB1 should all be on (green). f. Alarms should be clear.

NOTE: If Alarms is either flashing or steady red, or any of the above parameters are not satisfied, seek

assistance from 4D LABS staff.

Figure 1: Main Status Screen

Functions

(Large) Antechamber Alarms

Box Isolation Control

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2. Enter the Functions screen located on the left hand side of the main status screen. a. Verify that Cirulation Reactor 1, Vacuum Pump VPG, and Analyzer are online (green). b. Turn on the box lights.

Figure 2: Main Functions Screen

3. Return to the main status screen by clicking on END. 4. Enter the Antechamber screen by clicking on the blue square located on the bottom right.

a. Turn on Vacuum Pump VP1.

Figure 3: Antechamber Screen

5. Return to the main status screen by clicking on END.

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Sample Loading/Unloading

The process of loading items into the glovebox requires the user to be conscientious of maintaining the integrity and purity of the glovebox atmosphere. Items to be introduced to the glovebox must undergo, at minimum, 3 purge/refill cycles in order to cleanse the antechamber environment prior to exposure to the glovebox interior. Items that are porous, have high surface area, or have an ample amount of trapped gas, will likely require extended purge times in the antechamber, e.g. HEPA filters require ~4hrs purging in the antechamber. It is important that users follow all safety information outlined in this procedure.

NOTE: For additional information, consult APPENDIX D – Sample Loading/Unloading via Small Ante-chambers. The concepts provided are also applicable for the large antechamber.

Loading Via Small Antechambers

Figure 4: Small Antechamber

NOTE: The typical idle state of the small antechambers should be at vacuum with the 3-way valve set to

the ‘Closed’ position.

1. Confirm that the antechamber is under vacuum. 2. Within the Antechamber submenu (see User Menus above), confirm that Vacuum Pump VP1 is on. 3. Refill the antechamber by turning the 3-way valve to the ‘Refill’ position. 4. Wait until pressure has reached 0 bar(g). 5. Turn the 3-way valve to the ‘Closed’ position. 6. Unlock and open the outer cover. 7. Load your inbound material onto the moveable tray.

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8. Close and lock the outer cover. 9. Purge the antechamber by turning the 3-way valve to the ‘Evacuate’ position. 10. Evacuate the antechamber until pressure has reached approximately -0.9bar(g). 11. Refill the antechamber by turning the 3-way valve to the ‘Refill’ position. 12. Refill the chamber to approximately -0.2 bar(g). 13. Repeat steps 9-12 two more times. 14. On third refill cycle, continue refill until pressure has reached 0 bar(g). 15. Turn the 3-way valve to the ‘Closed’ position. 16. Don the glove pair closest to the inner cover. 17. Unlock and open the inner cover. 18. Observe the main status screen. If the H2O / O2 levels increase substantially, immediately close

and lock the inner cover. Consult with 4D LABS staff on how best to proceed. Additional purge/refill cycles may be required and/or an extended/overnight purge at the discretion of 4D LABS staff. If H2O / O2 levels remain satisfactory, proceed to step 19.

19. Remove inbound material from the moveable tray. 20. Close and lock the inner cover.

The antechamber may remain at 0 bar(g) for the duration of work taking place within the glovebox. The antechamber environment is considered inert and may be accessed at any time from within the glovebox in order to remove materials. However, if for any reason the antechamber is compromised (e.g. opening the outer cover by accident), then the 3x purge/refill cycle will have to executed before opening the inner cover.

Unloading Via Small Antechambers

1. Is the antechamber environment is inert? If so, proceed to step 2. Otherwise, perform 3x purge/refill cycles as described in the Sample Loading procedure.

2. Don the glove pair closest to the inner cover. 3. Unlock and open the inner cover. 4. Load your outbound material onto the moveable tray. 5. Close and lock the inner cover. 6. Unlock and open the outer cover. 7. Remove outbound material from the moveable tray. 8. Close and lock the outer cover. 9. Purge the antechamber by turning the 3-way valve to the ‘Evacuate’ position. 10. Evacuate the antechamber until pressure has reached approximately -0.9bar(g). 11. Turn the 3-way valve to the ‘Closed’ position.

The antechamber is now under vacuum. This is the recommended idle state.

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Loading Via Large Antechamber

Figure 5: Large Antechamber

NOTE: The typical idle state of the large antechamber should be at vacuum.

1. Confirm that the antechamber is under vacuum. 2. Within the Antechamber submenu (see User Menus above), confirm that Vacuum Pump VP1 is on. 3. Remain in the Antechamber submenu. 4. Activate ‘Refill’. 5. Wait until pressure has reached 0 bar(g). 6. Unlock the front cover by turning the spindle counterclockwise until it is loose. 7. Push forward the front cover strut, release the retention latch at the bottom of the strut, and open

the front cover by lifting the strut upwards. 8. Load your inbound material onto the moveable tray. 9. Close and lock the front cover by turning the spindle clockwise. The spindle should spin freely.

Once resistance is felt, turn the front spindle another 1/4 turn. Do not overtighten! 10. Activate ‘Evacuate’. 11. Evacuate the antechamber until pressure has reached approximately -0.9bar(g). 12. Refill the antechamber by deactivating ‘Evacuate’ and activating ‘Refill’. 13. Refill the chamber to approximately -0.2 bar(g). 14. Repeat steps 10-13 two more times. 15. On third refill cycle, continue refill until pressure has reached 0 bar(g). 16. Deactivate ‘Refill’. 17. Don the glove pair closest to the inner cover. 18. Unlock and open the inner cover by rotating the spindle counterclockwise and lifting the cover arm.

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19. Observe the main status screen. If the H2O / O2 levels increase substantially, immediately close and lock the inner cover. Consult with 4D LABS staff on how best to proceed. Additional purge/refill cycles may be required and/or an extended/overnight purge at the discretion of 4D LABS staff. If H2O / O2 levels remain satisfactory, proceed to step 20.

20. Remove inbound material from the moveable tray. 21. Close and lock the inner cover. As with the front cover, turn the spindle clockwise until resistance

is felt plus another 1/4 turn.

The antechamber may remain at 0 bar(g) for the duration of work taking place within the glovebox. The antechamber environment is considered inert and may be accessed at any time from within the glovebox in order to remove materials. However, if for any reason the antechamber is compromised (e.g. opening the outer cover by accident), then the 3x purge/refill cycle will have to executed before opening the inner cover.

Unloading Via Large Antechamber

1. Is the antechamber environment is inert? If so, proceed to step 2. Otherwise, perform 3x purge/refill cycles as described in the Sample Loading procedure.

2. Don the glove pair closest to the inner cover. 3. Unlock and open the inner cover by rotating the spindle counterclockwise and lifting the cover arm. 4. Load your outbound material onto the moveable tray. 5. Close and lock the inner cover. Turn the spindle clockwise until resistance is felt plus another 1/4

turn. Do not overtighten! 6. Unlock the front cover by turning the spindle counterclockwise until it is loose. 7. Remove outbound material from the moveable tray. 8. Close and lock the front cover by turning the spindle clockwise until resistance is felt plus another

1/4 turn. 9. Within the Antechamber submenu (see User Menus above), activate ‘Evacuate’. 10. Evacuate the antechamber until pressure has reached approximately -0.9bar(g). 11. Deactivate ‘Evacuate’.

The antechamber is now under vacuum. This is the recommended idle state.

Closing Steps Prior To Leaving

1. Confirm that all materials inserted into the glovebox have been removed. 2. Verify that all antechambers are under vacuum. 3. Verify that the 3-way valves for the two small antechambers are both set to the ‘Closed’ position. 4. Enter the Antechamber screen by clicking on the blue square located on the bottom right.

a. Verify that ‘Refill’ and ‘Evacuate’ are both deactived.

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b. Turn off Vacuum Pump VP1. c. Return to the main status screen by clicking on END.

5. Enter the Functions screen located on the left hand side of the main status screen. a. Turn off the box lights. b. Return to the main status screen by clicking on END.

6. Verify that all gloves are folded onto each other inside the glovebox.

Figure 6: Folded Gloves

7. Verify the glovebox parameters on the main status screen.

a. Pressure should be between 1-5mbar. b. H2O should be < 10ppm. c. O2 should be < 10ppm. d. Box 1 and Box 2 should be active (green). e. LMF, VPG, RKM, and GB1 should all be on (green). f. Alarms should be clear.

NOTE: If Alarms is either flashing or steady red, or any of the above parameters are not satisfied, seek

assistance from 4D LABS staff.

In Case of Catastrophic Breach or Emergency

In the case of a catastrophic breach, most commonly a torn glove, the user must take immediate steps to

remedy the situation.

1. If available within the affected glovebox, grab the inner sealing cover through the gloveport feed-through whose gloves should be replaced. Latch the sealing cover onto the gloveport feedthrough

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by tightening the knob clockwise. Once complete, of if sealing cover is not available, proceed to step 2.

Figure 7: Gloveport Sealing Cover

2. Within the main status screen, isolate the unaffected box by clicking on the box isolation control.

For example, if a torn glove occurs on the left side box (Box 1), click on ‘Box 2’ in order to deacti-vate (isolate) the right side box (Box 2) from circulation. Once deactivated, the ‘Box 2’ icon will appear grey.

3. Enter the Functions screen located on the left hand side of the main status screen. a. Turn off Cirulation Reactor 1. b. Turn on Quick Purge.

4. Immediately notify 4D LABS staff so that a repair can be made. In the case of a critical emergency, e.g, massive breach, exposed electrical, water leak, etc., immediately

vacate the room, notify others nearby, and notify the 4D LABS staff. In case of fire, evacuate the room, pull

the fire alarm, and evacuate the building.

System Shutdown / Startup

NOTE: This procedure should only be undertaken by 4D LABS Staff in the event of a planned power out-age, extended facility shutdown, emergency, or extended equipment maintenance.

1. Enter the Functions screen located on the left hand side of the main status screen. 2. Turn off Cirulation Reactor 1, Vacuum Pump VPG, and Analyzer. 3. Return to the main status screen. 4. Isolate Box 1 and Box 2. 5. Confirm that the evaporator is vented and that the turbopump and roughing pump are at idle.

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6. Wait 1/2 hour. 7. Switch off power to the glovebox (right side of purifier) and evaporator (left side of Box 2) via the

corresponding power switches (Figure 8).

Figure 8: Glovebox System and Glovebox Evaporator Power Switches

8. Follow the procedure in reverse to restart the glovebox system and evaporator.

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APPENDIX A – Solvent Filter (LMF) Regeneration

The function of the solvent filter (LMF) is to remove solvent vapours from the box atmosphere and protect

the purifier (RKM) against the adverse effects of solvents.

The procedure to regenerate the LMF is straightforward and requires minimal user interaction. The process

involves activating the LMF regeneration function via the software, which starts an automated 16hr pro-

cess. Thus, it is best to start this process towards the end of a working day and allow the glovebox to run

the regeneration overnight. During this time, the glovebox may be used, however, it is recommended to

avoid glovebox use as the gas only circulates via the H2O / O2 purifier reactor (RKM) and the solvent filter

is unable to trap solvent vapours. The recommended maintenance interval for LMF regeneration is once per

month.

NOTE: LMF regeneration does not use the 2.5% H2 regeneration gas. Rather, it uses the inert pure box gas (operating gas).

The following procedure outlines the necessary steps to regenerate the LMF.

1. Confirm glovebox status is normal. 2. Ensure O2 content is < 30ppm. If higher, purge the system until <30ppm. 3. Enter the LMF submenu via the main screen. 4. Disable “Circulation LMF Filter 1”. 5. Activate “Regeneration LMF Filter 1”.

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6. Follow the screen prompts as shown below (replace ‘Purifier’ with ‘Solvent Filter’). When prompt-ed, confirm gas flow is sufficient (15L/min) on the left side flow meter, located on the bottom right of the purifier (wait 1min to stabilize). If necessary, adjust the black knurled knob regulator on the back of the purifier to adjust the flow (typically not necessary).

7. Once gas flow is confirmed and acknowledged via the software, the regeneration of the LMF has started. The process will complete in approximately 16hrs time. Once finished, the glovebox status should be checked to confirm that moisture, oxygen, and pressure readings all look normal.

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APPENDIX B – Cleaning the Moisture Sensor

The following procedure is taken from the MBraun glovebox operating manual. The recommended mainte-

nance interval for cleaning the moisture sensor is every 2000hrs. The glovebox registers an alarm every

2000hrs which has to be manually cleared in the service menu. Given minimal use of the glovebox, it is

permitted to extend the cleaning interval to every 4000hrs. Thus, it is permitted to clear the automatic

alarm every other 2000hr interval provided sensor cleaning occurred during the previous 2000hr interval.

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APPENDIX C – Purification Reactor (RKM) Regeneration

The function of the purification reactor (RKM), also referred to as purifier, or reactor, is to recycle the inert

box atmosphere and remove moisture and oxygen from the box atmosphere. The purifier is capable of

achieving and maintaining <1ppm O2 and H2O, though it is common for moisture and oxygen levels to

increase over time as new items are continuously introduced into the glovebox and the purifier becomes

increasingly saturated.

The procedure to regenerate the RKM is slightly more complex than regenerating the LMF but nonetheless

requires minimal user interaction. The process involves activating the RKM Regeneration function via the

software, which starts an automated 16hr process. Thus, it is best to start this process towards the end of

a working day and allow the glovebox to run the regeneration overnight. During this time, the glovebox

should not be used as box circulation and purification is inactive. There is no recommended maintenance

interval for RKM regeneration. Instead, staff should monitor the idle moisture and oxygen levels. Particular-

ly, a rise in O2 levels of >1ppm is an indication that RKM regeneration should soon be considered. Most

glovebox operators elect to regenerate the purifier once idle O2 levels reach between 5-10ppm.

NOTE: RKM regeneration does use the 2.5% H2 regeneration gas. Care should be taken to ensure that the gas cylinder is open and has sufficient pressure.

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NOTE: MBraun specifies the regen gas to contain 3-10% hydrogen in a balance of inert gas, e.g. nitro-gen. The 4D LABS 2.5%H2 content regen gas is tentatively approved for RKM regeneration. It is estimated that the regeneration process will deplete a standard T-cyl from a typically full 2500psi down to about half full, e.g. 1200psi. If using a H2 gas mixture of less than 5%, a second RKM re-generation will likely necessitate replacement of the cylinder as a minimum 1300psi is required. If permitted, a 5-10% H2 mixture may be considered for future regenerations. In this case, it is criti-cal that the systems settings are adjusted to account for this change. A higher H2 content will al-low for less regen gas usage and lower the minimum threshold to 700psi on the supply side. Thus, it may be possible to perform 2-3 regeneration cycles on 1 cylinder, resulting in cost savings.

The following procedure outlines the necessary steps to regenerate the RKM.

1. Confirm glovebox status is normal. 2. Ensure O2 content is < 30ppm. If higher, purge the system until <30ppm. 3. Ensure the 2.5% H2/N2 balance gas cylinder (located behind the XPS) is open, has > 1300psi

supply pressure, and has the output pressure set at 5 ± 1 psi. 4. Log the regen gas supply pressure. 5. Enter the RKM submenu via the main screen. 6. Disable “Circulation Reactor 1”. 7. Activate “Regeneration Reactor 1”. 8. Follow the screen prompts as shown below. When prompted, confirm regen gas flow is sufficient

(15L/min) on the right side flow meter, located on the bottom right of the purifier (wait 1min to stabilize). If necessary, adjust the gas cylinder regulator to set the flow accordingly.

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9. Once gas flow is confirmed and acknowledged via the software, the regeneration of the RKM has started. The process will complete in approximately 16hrs time. Once finished, the glovebox status should be checked to confirm that moisture, oxygen, and pressure readings all look normal.

10. Log the regen supply pressure and calculate usage. Maintain a record and compare against previ-ous regeneration cycles to identify trends.

11. Observe the regen waste water collected in the waste water trap located behind the purifier. The water should be clear and approximately 100mL in volume. Log the appearance and quantity and compare against previous regeneration cycles to identify trends. If the water quantity diminishes or is cloudy/stinky, it is a sign that the catalyst is poisoned and is in need of replacement. Contact MBraun if this situation should arise.

12. Discard the waste water.

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APPENDIX D – Sample Loading/Unloading Via Small Antechambers

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APPENDIX E – Glovebox Evaporator Operation

The built in evaporator is a simple 3 source thermal evaporator complete with source shutters, dedicated

deposition rate monitors, substrate rotation, and substrate heating. As the evaporator is installed inside

the glovebox, extra care must be taken in sample insertion/removal and when verifying the sources. The

majority of chamber setup should be conducted by staff; in the event of any issues/questions, the user must

request assistance before proceeding. The following is a simple guide to operation.

1. Enter the ‘Evaporator Chamber’ screen.

2. Verify that ‘Vacuum pump’ is on. 3. Verify that ‘Handmode’ is on. 4. If the chamber is at atmosphere, proceed to step 6. Otherwise, deactivate ‘Auto/Evacuate’ and ac-

tivate ‘Refill’. Wait until chamber is vented up to atmosphere. 5. Deactivate ‘Refill’. 6. Open the chamber and perform chamber tasks as required, e.g. sample loading, source check, etc.

Request assistance from staff if necessary. 7. Close the chamber door. 8. Activate ‘Auto/Evacuate’. Wait until chamber is <1E-5mbar.

NOTE: Users are permitted to wait for a higher vacuum level if desired.

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9. Enter the ‘Layout’ screen.

10. Open the desired source shutter. 11. Activate ‘Rotary Holder’ to turn on substrate rotation. 12. Switch to the Inficon SQC-310C Deposition Controller.

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13. Enter the ‘Process Menu’. 14. Select the desired process w/ the control knob. Process name should start with ‘4D_’. 15. Press ‘Select’. 16. Press ‘Start’. Wait for |Deposit| and ‘Attention: Min. Power’ notifications. 17. Press ‘Next Menu’. 18. Press ‘Next Graph’ in order to display the Rate (A/s vs. Time) graph. 19. Begin slowly increasing the source power by rotating the knob clockwise. Power % should increase

at a rate of roughly 1.0% for every 2-3 seconds. 20. Increase the power slowly until the desired power set point is reached (refer to the deposition log

sheet for recent operating conditions). 21. Monitor the deposition rate and adjust the power accordingly.

NOTE: BE AWARE and decrease the power quickly if an abrupt spike in deposition rate occurs. This is par-ticularly common for certain materials, e.g. silver.

22. When the deposition rate is stable, press ‘Zero’ and simultaneously open the substrate shutter. 23. Monitor the thickness deposited. 24. When the desired film thickness is achieved, close the substrate shutter. 25. Slowly decrease the power back to 0% at a rate of roughly 1.0% per second. 26. Press ‘Stop Layer’. 27. Press ‘Next Menu’. 28. Press ‘Reset’. 29. Press ‘Next Menu’. 30. Close the source shutter. 31. Deactivate ‘Rotary Holder’ to turn off substrate rotation. 32. Deactivate ‘Auto/Evacuate’. 33. Activate ‘Refill’. Wait until chamber is vented up to atmosphere. 34. Deactivate ‘Refill’. 35. Wait 5 minutes to let the chamber internals cool down.

NOTE: BE AWARE the chamber may still be hot after 5min if venting after a long deposition. The user

must wear the blue nitrile gloves on the inside of the glovebox in order to protect the black butyl glovebox gloves from heat damage, vice versa, protect the chamber from butyl contamination.

36. Open the chamber and perform chamber tasks as required, e.g. sample unloading, source check,

etc. Request assistance from staff if necessary. 37. When finished, close the chamber door. It is permissible to leave the chamber vented (at atmos-

phere).

Documents

Glovebox MBraun Glovebox System Standard Operating … · Glovebox – MBraun Glovebox System Standard Operating Procedure 4D LABS Confidential Revision: 1.1 — Last Updated: November