Hone Group

Graphene Growth Furnace

The Graphene Growth Furnace is used to grow CVD graphene on copper substrate. Currently, the furnace can grow on standard, pita copper substrates.

Location

The tool is located in room 705E on the 7th Floor of Northwest Science Building.

Notices

6/10/11: Scroll Pump O-ring installed. Will be replaced every 6 months.

6/28/11: RF Plasma Cleaner attachment was installed on the left end valve of chamber. Removed 8/17/11.

7/21/11: Discolored middle stripe on the copper strip was first observed on standard growth.

8/2/11: Low CH_4 flow and High CH_4 flow controllers installed. Problem with Low CH_4 flow control. Fixed 8/25/11.

8/17/11: Acetic acid pre-treatment of copper strip. 9/10/11: Use Copper Roll Lot #H18W014 first! (Chromium Oxide deficiency)

8/31/11: New Hydrogen, Methane and two Argon tanks, all bled for 2 hrs.

Training and Maintenance

For training on this tool or if there is a problem, contact Nick Petrone at nwp2105@columbia.edu

Scheduling

For CVD graphene growth requests, contact Steven Yoon at sy2272@columbia.edu

The use of the Graphene Growth Furnace is limited to those that are both trained in proper usage and approved by Nick.

Tool use

Resources

Are there any websites, or papers with good discussions on how this tool works? Add them here.

Standard operating procedure

Standard Growth procedure is shown here; Pita Growth procedure has several important modifications.

Preparation of Sample

1. Liberally lay down large Texwipes on CVD bench area.

2. Place Copper Substrate on Quartz Substrate Holder.

3. Use Ar gun to clean the substrate holder surface and both sides of copper substrate.

4. Place “back” side of copper substrate on substrate holder, and fold over one end.

Load Sample

1. Release both end valves by unscrewing the cuffs and disassembling the cuff, cap and O-ring onto clean Texwipes.

2. Using the clean quartz rod, gently push sample until it is centered on the oven’s thermocouple.

3. Seal both end valves.

4. Make sure that the proper exhaust valves are open/ closed and the proper power plug is being used for the pump.

Exhaust Valves for Standard: Valve 1 Closed, Valve 2 Closed, Valve 3 Open

Power Plug for Standard: Orange Tag

Preparation for Growth

1. Start Labview Program: Flow and Temp Control.vi

2. Click “Run” Command on Control Bar.

3. Click “Pump” Button on Dashboard.

4. Wait until desired P_Air value is reached.

5. Turn off program using the Stop button on Dashboard.

Growth

1. Start Labview Program: Graphene Growth Interface_Cu Growth_v2.vi

2. Click “Run Continuously” Command on Control Bar.

3. Make sure proper values are being used for the recipe: Check Ar, H_2, CH_4, Growth Temperature and Time.

4. Click “Start” Button on Dashboard.

Unload Sample

1. Make sure the program has finished: oven is fully retracted, chamber has been vented to air pressure.

(If aborting program during cooling: Press “Cancel” Button on Dashboard; Select “Yes” for Vent to Atmosphere prompt.)

2. Release both end valves by unscrewing the cuffs and disassembling the cuff, cap and O-ring onto clean Texwipes.

3. Using the clean quartz rod, gently push finished sample out of the chamber.

4. Place finished sample on clean Texwipes on CVD bench area.

Storage of Sample

1. Using clean tweezers from “Copper” bin, carefully separate copper substrate from the substrate holder.

2. Using tweezers, “Drag” the copper substrate onto a glass slide.

3. Lay substrate flat on slide, fold over both ends.

4. Place slide in a petri dish, and mark tampered portion on the lid of the dish.

5. Mark Date, Name, and important parameters: H_2, CH_4 flow, Growth Temperature and Time.

Tool Recipes

Standard Growth

A typical growth will have the following parameters:

Anneal: H_2: 2 sccm, 1000 deg Celsius, 900 sec (15 min.)

Growth: H_2: 2 sccm, CH_4: 35 sccm, 1000 deg Celsius, 1800 sec (30 min.)

Pita Pocket Growth

A typical growth will have the following parameters:

Anneal: H_2: 2 sccm, 1000 deg Celsius, 900 sec (15 min.)

Growth: H_2: 2 sccm, CH_4: 3 sccm, 1035 deg Celsius, 3600 sec (1 hr.)

Purchasing Information

Scroll Pump Replacement O-rings

Within the pump body, each scroll is protected by a spiraling Teflon O-ring. These O-rings should be replaced every 6 months. A new kit is purchased from ( )

Link: ( )

Pressure Gage O-rings

Two O-rings are needed for one pressure gage, which is located on both ends of the growth chamber. O-rings can be ordered in bulk at Marco Rubber. Dimensions: AS568A-21

Link: http://www.marcorubber.com/viton.htm

Quartz Tubing

During times of heavy use, changing the growth chamber once a week is recommended. Dimensions: I.D. 22 mm (0.86 in) O.D. 25mm (1 in) Length: 48 inches (4 ft) Model #: FQ-T-25-22-4

Link: http://www.advaluetech.com/clear_fused_quartz_tubing.html