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--- nanotube_growth [2021/06/28 13:05] – [Paint-on catalysts] ethanminot
+++ nanotube_growth [2022/08/09 16:33] (current) – dublin
@@ Line 41: / Line 41: @@
 === Recipes ===
-*UPDATED 05/28/2012 by Heather*
+*UPDATED 2022 by Dublin
-(Click here for [[other recipes]])
+(Click here for [[other recipes]]) and [[old_recipes]]
-  *Check that the gas cylinders are all on and have plenty of gas (the pressure inside a full cylinders is about 1500 psi).
+==== 1" Furnace growth ====
-  *Open furnace lid. Open growth tube carefully.  Place sample within growth tube.  Use the quartz push rod to slide the sample to the center of the furnace.
-  *Close growth tube. Establish vacuum seals to the quartz tube.  Close furnace lid.
-  *Set purge parameters in automated program.
-  *Make sure furnace and power supplies are on.
-  *If you are doing alcohol growth add ice and water to the beakers that the bubblers are in.
-  *Press the start button on the automated growth display panel.
-  *Allow system to cycle.
-  *Set growth parameters in automated growth program.
-  *Press the start button on the automated growth display panel.
-  *Allow system to cycle.
-  *At 400C, safe to open furnace lid (speeds up cooling process)
-  *At 200C, safe to handle growth tube and retrieve sample.
-    * **Purge Parameters**
+__**Startup/Loading chips**__
-    -Anneal temperature = 100C
-    -Anneal time = 10 minutes
-    -Anneal gases (if alcohol growth is planned) = 0.45 SLM Hydrogen, 0.30 SLM Methanol, 0.15 SLM Ethanol, and 0.50 SLM Argon
-    -Anneal gases (if other recipe is planned) = growth gases and flow rates, and 0.5 SLM Argon
-    -Growth temperature = 0C
-    -Growth time = 0 minutes
-    -Growth gases = 0 and uncheck all gases (check “neither”)
-    * **Alcohol Growth Parameters**
-    -Anneal temperature = 800C
-    -Anneal time = 15 minutes
-    -Anneal gas = Atmosphere
-    -Growth temperature = 900C
-    -Growth time = 15 minutes
-    -Growth gases = 0.45 SLM Hydrogen, 0.30 SLM Methanol, and 0.15 SLM Ethanol
-    * **Methane Growth Parameters** (suggested by McEuen group)
-    -Anneal temperature = 550C
-    -Anneal time = 5 minutes
-    -Anneal gas = Atmosphere
-    -Growth temperature = 825C
-    -Growth time = 60 miniutes
-    -Growth gases = 1.9 SLM Methane, 0.3 SLM Hydrogen
+  - Keep chips ready for growth in furnace
+  - PNF are for Utah
+  - PNF - 2 micron trench
+  - PNR - 2.6 micron trench
+  - To pressurize:
+  - Connect hand pump to nipple
+  - Black button releases pressure
+  - Pump up to 25 in Hg
+Ethanol/methanol levels: Use around half as much Methanol as Ethanol. (In my experience, a 1:1 ratio produces more multi-tube sites and shorts, so this ratio is important. - Dublin)
+  - Fill out logbook
+  - Always run purge
+  - STD growth
+  - Humidity
+  - Turn on Dehumidifier
+  - Humidity should be around 30%
+  - Check end cap is secure
+  - Check Ar and H tanks
+  - 20PSI on both
+  - Lose around 5psi of argon tank pressure per hour of flowing
+  - Load in chips. (I have successfully grown 3 at a time, which is all you can fit on the boat. - Dublin)
+  - Unscrew the end part
+  - Careful not to drop it
+  - Attach magnet to end of tray and slide in chip
+  - Reattach end part
+  - Current tube 2022:  “Tristan”
+__**Growth Process**__
+Input purge parameters:
+Anneal:
+  * 30 C
+  * 3 min
+  * Hydrogen: 0.45 SLM
+  * Argon: 1SLM
+Transition:
+  * 0 min (no transition)
+Growth:
+  * 30 C
+  * 3 min
+  * Hydrogen 0.45 SLM
+  * Methanol 0.3 SLM
+  * Ethanol 0.15 SLM
+  - Set timer for 5 min and start purge. Will go through anneal and “growth” stages at 30 C
+  * When changing parameters, give the program a few seconds to get it
+  * After purge finishes, reinitialize parameters
+  * Wait until all flow rates show zero
+Growth Parameters:
+Anneal:
+  * 800 C
+  * Hydrogen: 0.45 SLM
+  * 1 min
+Transition:
+  * 0 min ramp time
+Growth:
+  * 800 C
+  * 5 min
+  * Hydrogen 0.45 SLM
+  * Methanol 0.3 SLM
+  * Ethanol 0.15 SLM
+  - Start growth and set a timer for 14:30. When the furnace reaches 798 C, slowly and deliberately slide in tubes
+  - Once anneal phase begins, set timer for 4:30 min
+  - To check if it’s working: Ethanol and methanol are bubbling.
+  - When PID controller clicks off (growth is finished):
+  - Pull chip to rim of insulating chamber and allow to sit until 790 C
+  - Pull chip fully out
+  - When temp is 500 C, open lid
+  - When temp is 200 C or lower, pull out chip
+  - The program flows argon before 200C
+  - Close lid
+  - Unscrew end connector
+  - Drag magnet as far to the left as possible
+  - Grab back end of sled and pull chip straight out
+  - Grab in center of rod
+  - Keep the chip level! It’s not connected
+  - Place chip on beta wipe
+  - Hold rod while grabbing chip and place chip in holder
+  - Store rod in quartz tube, cap it up
+  - Screw end cap back on and seal tube
+  - Once chamber is cooled back down to room temperature, ready for another growth
-=== Growth Success Table ===
-^Catalyst ^Evaporated Stain ^ Rinsed Stain ^ Tape ^ Photoresist ^Ink Jet ^Spin Coating ^Sputtered^
-| CuCl2/PVP | | | | | | N| |
-| CuCl2| N | N | | | | | |
-| FeMo| Y,N| N| | | | | |
-|Ferritin |Y,Y | N | | Y | | N | |
-| FeMo + alumina| Y| Y| | Y| | Y| |
-| Sputtered Iron| | | | | | |Y|
 ===== 4" Furnace growth =====