nSIL Glovebox – Training and Operating Manual
Overview
A custom-built, dual-chamber N2 glovebox for sample preparation and spin-coating at reduced oxygen and moisture content. The left-side contains spin-coater and hot-plates, while the right one presently has a transfer station and a dual hot-plate/stirrer setup with stands for supporting glassware. Custom setups may be accommodated, with prior approval from staff.
Allowed Materials
To limit moisture, all materials loaded into the glovebox should be free of water or sealed air pockets. Absolutely no water or aqueous solutions (i.e. inorganic acids or bases) are allowed.
The catalyst used to remove oxygen from the glovebox atmosphere is sensitive to certain chemical reactions. Therefore the following organic solvents are prohibited:
1. Chlorinated or Fluorinated Solvents (Cl-, F-)
2. Amines, Amides or other Nitrogen-rich substances (N-).
3. Phosphates / Phosphides and Thiols (P-, S-)
4. Large amounts of Alcohols (ethanol, IPA), Ketones (Acetone), or Ethers.
Special-accommodations can be made, only with prior consultation, though this may require upwards of a day of purging the system or catalyst regeneration.
Allowed Chemicals include the following:
1. Toluene and Benzene as solvents
2. Anisole or Ketone-based resists (i.e. PMMA, HSQ)
3. Small levels of Alcohols, Ketones, Ethers.
Special instructions (circulation isolation, purging) are required to protect the box during solvent use.
Startup
Reserve and enable the side(s) of the glovebox you’ll be using on Badger.
Sign-in into the log-book and note starting O2, H2O levels, as well as any chemicals you’ll spin or use.
Sample Loading
Each glovebox side has a smaller loadlock, and a large ante-chamber for transfer between boxes and loading of larger equipment. Generally, only the smaller loadlock should be used since it takes much less time to pump down. Both loadlocks should be pumped down when not in use. Use of the ante-chamber requires prior approval from staff.
1. Check that the glovebox environment is nominal.
Pressure : 5 – 6 mBar
O2 : < 0.5 ppm
H2O : < 1 ppm
If these are not within the range stated, please report this in Badger so that the staff can evaluate the problem and determine the source of this issue.
2. Push the Refill lever to the Open position to vent the loadlock.
3. Push the Refill lever to “Closed”. Otherwise, the loadlock door will not open. This is a safety feature to ensure that the door does not fly open and injure the user since gas is being pumped into the loadlock chamber.
4. Open the loadlock door, load samples (using clean gloves), and close the door.
a. It is hard to reach inside the LL once you have the gloves on, so place objects at the far end.
b. Everything you place in the loadlock must be capable of surviving a vacuum, and cannot contain any air pockets as they will contaminate the glove box. Any plastic bags should be left open. Any bottles or chemicals should have their caps loosened. If this presents a chemical hazard for any reason, consult with staff on best practices.
c. For volatile solvents or full bottles, use a sealed pinhole Solvent-Transfer Box.
5. Pump / Purge the loadlock a total of 10 times (to prevent contamination of glovebox)
a. Push Evacuation lever Open to evacuate the loadlock.
b. Wait until the pressure drops to <-30 inHg
c. Push Refill lever Open.
d. Repeat steps a-c 10 times.
6. Open the Evacuation Lever, let the chamber pump all the way down to -30 inHg (full vacuum), close it, and then Open the Refill Lever to bring the chamber back up to atmospheric pressure.
7. Close the Refill lever.
8. OPTIONAL: Adjust the glovebox pressure using the foot pedals. The nominal operating pressure is 5 mBar, but you will want a slightly lower pressure when pushing your hands into the gloves. Be attentive: the glovebox pressure will change as you push the gloves into the glovebox!
9. Put your hands in the glovebox gloves, and add secondary latex gloves.
a. Remove ALL JEWELRY, watches, arm-bands etc. to prevent tears.
b. Make sure you’re wearing gloves and long-sleeves, to protect the main gloves from your fingernails and avoid build-up of sweat.
c. It is very important that you always have secondary latex gloves on when working in the glovebox. While the glovebox gloves provide protection, damaging those would result in a lengthy shutdown of the tool and high repair costs. Thus it is best to put on secondary latex gloves.
10. Open the door from inside the glovebox, retrieve your items from the boat, and close the loadlock door.
11. Pump down the loadlock by opening the Evacuation lever.
12. Leave both levers closed (or Evacuation open) while processing.
Unloading
When finished working, unload your samples through a similar procedure as Loading.
Volatile solvents should be kept in the pinhole Solvent-Transfer Box.
1. Open the Refill lever to return the system to vent the chamber to atmosphere.
Close it when finished.
2. Open the door inside the glovebox, load your samples, and re-seal the loadlock.
3. Pump / Purge the loadlock at least once to protect yourself from noxious fumes. Leave the chamber at atmosphere and Close both levers.
4. Open the external chamber doors and retrieve your materials.
5. Close all doors and Pump the loadlock down to base-pressure. Leave the Evacuation lever Open when finished.
Record final O2 and H2O concentrations in the log-book, turn-off all lights and disable the tool when finished.
Transfer Station Operation
The micromanipulator is capable of aligning samples with approximately 5um precision.
Materials:
1. Microscope with light source
2. Heated stage
3. Micromanipulator
Operating procedure:
1. Wear appropriate personal protective equipment (PPE).
2. Load all solvents and materials into glovebox in a pinhole-lid solvent transfer box through the small load-lock. Pump-and-purge load-lock 10x and introduce into glovebox using the same procedure as outlined for the left side of the glovebox.
3. Close circulation for glovebox half in use (rear two valves), open solvent bottles and load chips for PMMA removal; leave for 30 min – 1 hour in Acetone (with 2-Propanol dip) and let chips dry in glovebox ambient.
4. Perform transfer of material using transfer stamp. For more detailed instructions on how to perform the transfer, click here. Set heated stage to ~40⁰ C for “pick-up” of material and then ~110⁰ C for “put-down” of material on new substrate.
5. Soak chips for 30 min – 1 hour in Acetone (with 2-Propanol dip) to remove any residue from the stamp during transfer. Let chips dry in glovebox ambient.
6. Seal all solvents and purge glovebox for 5-15 minutes (open valve) before recommencing circulation.
7. Dispose of hazardous solvents, solutions, mixtures, and reaction residues as hazardous waste. Place in sealed plastic bags and extract in pinhole lid container with solvent bottles; pump-purge load-lock once.
8. Clean up work area and lab equipment. Wipe down any spilled solvents and similarly extract in sealed plastic waste-bag,
9. Remove PPE and wash hands.