How to use a glovebox (spin coating)

Preparation

1. Put on your lab coat, gloves, shoe covers, and head cover before entering the clean room.
2. Make sure that the glove box is in default "initial condition": the gloves on the glove box are blown onward. It indicates that the pressure is quite high inside the glove box. We do it to prevent any oxygen from entering the glovebox during the idle condition.

Start using the glovebox

1. Reduce the pressure
   1. In the control panel, press END (menu on the left side)
   2. Press the box containing Press, H20, O2
   3. Change the pressure
      Change the from the default (High: 5 mbar, Low: 3 mbar) to (High: ?, low: 1 mbar)
      It immediately changed, no need to press back.
2. Transfer the stuff into the glovebox
   1. Rotate the black valve under the chamber clockwise direction to let the Ar gas come in.
   2. Open the chamber's lever
   3. Put the stuff in
   4. Close the chamber's lever
   5. Rotate the black valve under the chamber counterclockwise direction (point toward glove box)
   6. Cycle 3 times (black valve (point up>point left)x3, at least in total 10-15 minutes before transferring the stuff inside the glovebox)
   7. Open the inner door, and transfer the stuff in.

When about to use spin coater

1. Turn off the circulation
   1. Press Function in the left menu
   2. Press the "Circulation Reactor 1". It will turn from green to grey. Listen to the change of sound as well.
2. Bypass route in the solvent trap
   During circulation, the air is going inside the solvent trap.
   Now that we want to spin coating, a lot of residual gas will come from the glove box. We need to bypass so that the gas does not go inside the solvent trap.
   • Bypass when:
     • Spin coating
     • Purging
   1. Open the top route, one lever (vertical -> horizontal)
   2. Close the bottom route, two levers (vertical -> horizontal)
3. Now you can:
   1. Start the spin coating
   2. Purging. (make O2 below 5 ppm during spin coating)

Use spin coating

1. Prepare the aluminum foil to wrap around the side of the spin coater
   1. Prepare around 0.5 m
   2. Fold the long side twice (about 5 cm)
   3. Fold it round
   4. Tape it to maintain the shape
   5. Put it in the transfer chamber
   6. Also put samples and XL gloves
   7. Leave it under vacuum (lever to the left direction)
2. Start purge. Always purge the glovebox before and after use
3. Additional vacuum pump (to suck the sample)
   1. Turn on the vacuum switch on the wall
   2. Open the valve behind the glovebox (there are 2 pipes that go to the spin coater, the left one is for the vacuum)
4. Additional argon (to prevent the solvent to go deep insight the spin coater)
   1. It is already open in the tank. Keep it like that.
   2. Open the valve behind the glovebox (the right one of the two mentioned)
5. Start spin coating
   *if the additional argon and vacuum are off, the spin coater will show "need CDA"
   1. Cover the surrounding with aluminum sheets
   2. Press "SELECT PROCESS"
   3. Chose any program
   4. Press "EDIT MODE"
   5. Edit: by pressing "tab>" then the cursor blinking
      1. Step: how many steps, which steps we are in (ex 1/2 means we have two steps, now in the first step setting)
      2. Time: time for the current step
      3. Rpm
      4. Acel: acceleration (usually 2000)
      5. Goto: 001
   6. Press "RUN MODE"
   7. Put the sample in the middle
   8. Press the vacuum button, the one that is most damaged. (now it said "ready")
   9. Blow the sample surface to make it clean from dust
   10. Drip the perovskite solvent
   11. Press the start
   12. Drip the antisolvent at your timing
   13. Press the vacuum button to turn off
   14. Take out the sample (put it on the top of heat plate)
   15. To make another, you need to open and close the spin coater top part first. Use your hand to hold. It will jump.
   16. Clean the top part of the spin coater with ethanol if needed
6. Annealing
   1. Turn it on by pressing the green switch under the red knob. It will start to heat up
   2. Press set to see what the temperature setting is.
   3. To change the temperature: press the "set" while also pressing the up or down
   4. The red knob is to set the power that will affect the heating speed. Usually, we don't touch it
7. Turn off the vacuum after finished. A MUST
   1. Close the valve behind the glovebox
   2. Turn off the switch on the wall
8. Turn off the additional argon. A MUST
   1. Close the valve behind the glovebox

After finishing spin coating

We can take our sample out, or just leave it inside.
Then do:

1. Turn off the vacuum after finished. A MUST
   1. Close the valve behind the glovebox
   2. Turn off the switch on the wall
2. Turn off the additional argon. A MUST
   1. Close the valve behind the glovebox
3. Purge it for at least 10 minutes
4. Turn off the purge
5. Change the route in the solvent trap
   1. Open the two levers (bottom) (horizontal -> vertical)
   2. Close one lever (top) (horizontal -> vertical)
6. Start the circulation by pressing it in the control panel (grey>green)

After finish all

1. Change the pressure value to the default
2. Clean the gloves using ethanol/IPA if needed
3. Make sure the vacuum and additional argon are turned off
4. Fill in the record

Else

About the gas tank

• The main tank powering the glove box is the left one.
  • For purging, 1 tank probably lasts for 30 minutes. Need to consider bringing backup.
  • Usually, bring 1 tank if we do the spin coating.
• The right one is for a spin coater.
  • Not so many are needed. Lasts long.
• How to change the gas (left)
  • If still gas inside. We want to finish them first. How? Use it for purge:
    • Turn off the circulation
    • Change the route: bypass (top open, 2 bottom close)
    • Press purge
    • You will hear the sound of gas flow/stop when the gas is low enough
    • When the gas pressure in the panel hit 1.5 mbar (in the tank it's around 5 bar), turn off the purge
    • Turn off the purge
    • Wait for the pressure in the tank to stabilize (go back to the black line mark)
  • Close the valve (that connect the glovebox and tank) by turning the black knob counterclockwise (all the way)
  • Close the valve on the top of the tank, clockwise
  • Now we can open the connector using a wrench
  • Make sure that the black knob is not opened by your hand
  • Tear the paper in the tank
  • Change the tank to the new one
  • Tighten using wrench
  • Open the valve on the top of the tank slowly until seeing the pressure rise. Then open it all the way.
  • Before opening the black valve, turn on the purge so that the needle goes down.
  • Open the valve (that connects the glovebox and tank) by turning the black knob clockwise slowly until the pressure is slightly below the black mark (the pink mark).
  • Turn off the purge.
    Done, now put the empty tank in the storage room.

Linked notes

013_Notes_Research
How to use a glovebox (weighing)