ANU Centre for Sustainable Energy Systems (CSES)

Lab Tool-book Checked date:April 2010 Checked by James

RCA Clean Full Procedure Protocol

1. Background
RCA cleans were developed by the RCA company in the US. They are a two-part cleaning process. The first part (RCA1) is an alkaline solution that removes organic residues. This tends to grow a thin oxide that consumes silicon and hopefully sequesters metal ions in the first few monolayers of silicon. This oxide can then be removed in HF thus improving the removal/cleaning process. The second part (RCA2) is an acidic solution that removes metal ions and inorganic residues. RCA cleaning is always done before wafers go into a furnace. Once wafers are clean, they can be stored in the laminar flow bench before loading in the furnace. Important Note: accreditation for RCA cleaning does not include accreditation for make-up and disposal of HF solutions. All RCA clean users should ideally be accredited for HF etching prior to RCA cleaning, or otherwise will require assistance for the HF parts of the process.

2. Hazards & Safety Gear

Traps for the Unwary
RCA solutions are hot. They can bubble or effervesce once you add a cassette of wafers. Leave the watch glass lids on beakers, when solution is not in use, to prevent evaporation.

Hydrochloric Acid (37% HCl) Hydrochloric acid solution and vapour causes painful burns. Read the MSDS before using this acid. Be aware of the handling and safety procedures and wear glasses, lab coat, plastic inner, and nitrile outer gloves at all times handling this acid. Ammonium Hydroxide (10-35% NH3) Ammonium Hydroxide solution and vapour causes painful burns. Read the MSDS before using this solution. Be aware of the handling and safety procedures and wear glasses, lab coat, plastic inner, and nitrile outer gloves at all times handling this acid. Hydrogen Peroxide (30% H2O2) Hydrogen peroxide solution and vapour causes burns. Concentrated H2O2 may burn paper. Dilute spills with water before wiping up. It is also highly flammable. Read the MSDS before using this solution. Be aware of the handling and safety procedures and wear glasses, lab coat, plastic inner, and nitrile outer gloves at all times handling this acid. Note: HCl and NH4OH are incompatible and NH4OH and H2O2 are incompatible

3. Equipment & Resources

RCA cleaning is done using designated cassettes and equipment. The RCA clean solutions are usually prepared using 4 glass 2L beakers marked A, B,C and D. These are

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ANU Centre for Sustainable Energy Systems (CSES)

Lab Tool-book Checked date:April 2010 Checked by James

rotated between RCA1, RCA 2 and rinse in accordance with the schedule on the wall adjacent to the fume hoods in the clean room E125 (where the gloves are hanging). There are larger containers suitable for RCA cleaning available. If you need to RCA clean larger items, discuss with staff to determine most suitable equipment and location. The post-RCA HF dip beaker also requires cleaning occasionally. This can be done by using the RCA solutions after sample cleaning has taken place. See instructions below. This step needs using/preparing HF solutions accredition. The RCA beakers sit atop their own dedicated hotplates. The handheld IR thermometer can usually be found on one of the tables alongside the RCA fume hood in the clean room. It is used to check solution temperature. DO NOT IMMERSE THIS THERMOMETER IN ANY SOLUTION, hold next to beaker (but not touching) to read temperature.

4. Procedures
RCA1 5:1:1 of H2O: Ammonia: H2O2 RCA2 5:1:1 of H2O: Hydrochloric acid: H2O2 For 2L beakers: RCA1 1000ml H2O : 200ml Ammonia: 200ml H2O2 RCA2 1000ml H2O : 200ml HCl: 200ml H2O2 In both beakers add required quantity of DI H2O. Add ammonia to RCA1, put ammonia away; add HCL to RCA2, put HCL away. (do not have more than one concentrated solution open in the fume hood at the same time; check section 2 Hazards & Safety Gear-Note) When RCA1 solution is above 65C and before immersing wafers in solution, add H2O2 to RCA1 beaker. Load wafers into designated Teflon cassette (non-RCA tweezers) or glass cradle and immerse in RCA1 solution for 10min. The solution should bubble gently. Fill Rinse bucket/beakers with DI water While wafers are in the RCA1 solution, add H2O2 to RCA2 (check the temp. first). After 10min in RCA1 solution rinse wafers twice in designated rinse container. OPTIONAL: Using a clean 10% HF dip place wafers in solution for approximately 10seconds until hydrophobic. Rinse in fresh DI rinse water three times after HF dip. Immerse wafers in RCA2 solution 10min. The solution should bubble gently. Refill rinse buckets After 10min in RCA2 solution, do three separate DI beaker rinses (alternating between fresh beakers of DI water) or a three minute overflow rinse. OPTIONAL: Using a clean 10% HF dip place wafers in solution for approximately 10seconds until hydrophobic. Rinse in DI water three times. Spin dry in spin rinser or dry using nitrogen gun

CLEANING THE HF DIP BEAKER:

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ANU Centre for Sustainable Energy Systems (CSES)

Lab Tool-book Checked date:April 2010 Checked by James

The simplest method is to re-heat the previous days RCA solutions. While they are heating up, lift a HF waste container into the fumehood and pour the clean HF solution into the HF waste carboy. Rinse the HF dip beaker three times with DI water. Use acetone on a Kimwipe to remove any label on the outside of the beaker. When RCA 1 solution is hot pour it into the HF dip beaker. It should be left for 10 minutes . After this time, decant the RCA 1 solution into a large upturned sink beaker , rotating the HF dip beaker to clean the inside rim as the solution is poured out. Rinse the HF dip beaker three times and pour the RCA 2 solution into it. Wait 10 minutes and repeat as before, adding the RCA 2 solution to the upturned sink beaker to cool. Rinse the HF dip beaker three times. Use a permanent marker to label the outside of the beaker Clean HF dip, beaker RCAd xx/xx/xx (date). Prepare a new solution by putting enough DI water to just cover the intended samples, then add a quantity of HF to make the solution approximately 5%. Place a label on /under the beaker to indicate the date of preparation/your name etc. When the old RCA solutions in the sink beaker are cool, pour them down the sink and flush with town water for 5-10minutes. DO NOT dispose of these solutions while they are hot.

*NOTE: For make-up and disposal of HF dip solutions refer to module on HF etching. If
you are NOT accredited to perform HF etches then you WILL require assistance for this part of the process.

5. Clean Up and Waste Disposal

Since a large volume of solution is necessary for cleaning cassette wafers, you may reuse the solution. Change it every day or more depending on use. Topping up with H2O2 can rejuvenate solution. Leave RCA solutions you intend to reuse on the hot plate with the lids on. To dispose of the RCA Solutions, allow them to cool then alternate the pouring of solutions down the sink with plenty of town water running. Leave the town water running for at least 5 minutes afterwards. The Clean HF solution should be put into waste containers as per the module for the HF etch process.

6. Troubleshooting
Provided that the instructions are followed, not a great deal can go wrong.

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