ANU Centre for Sustainable Energy Systems (CSES)

Lab Tool-book checked date: Feb 2009 by Andrew Li

NaOH Etch Full Procedure

1. Background

NaOH is an alkaline solution used to etch silicon wafers. Depending on the processing conditions, it can be used for polishing or for texturing. The general etch reaction proceeds according to the equation: Si + 4NaOH [SiO4]4- + 4Na+ + 2H2 RCA2 is usually done after the NaOH etch to remove the sodium ions and other impurities from the NaOH etching process. HF dips may also be done as part of the whole cleaning process. Please refer to Risk Assessment documents for RCA2 cleaning and HF etching, as well as for NaOH etching.

2.

Hazards & Safety Gear

Traps for the Unwary The etch rates of silicon dioxide in alkaline etches is VERY slow (up to 1000 times slower than bare silicon). Make sure your sample has been HF dipped immediately before immersion in an alkaline solution, or you may wait a very long time to begin etching the silicon. Texture and polish solutions need to be heated for consistent function and reaction rate. The solutions used in this process are hot (up to 90 C). 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. Sodium Hydroxide (NaOH) Exposure to NaOH can result in intense burning of the eyes, nose, throat, lungs, and skin. Read and understand the MSDS and hazard reports BEFORE you begin to use this compound. Be aware of the handling and safety procedures and wear glasses, lab coat, plastic inner, and nitrile outer gloves at all times handling this alkaline. Hydrochloric Acid (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. Hydrogen Peroxide (H2O2) Hydrogen peroxide solution and vapour causes burns. 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. Hydrofluoric Acid (HF) Hydrofluoric acid solution and vapour causes SEVERE and NOT IMMEDIATELY APPARENT BURNS. Read the MSDS and Medical Treatment & Chemical Properties manuals before using this acid. Be aware of the handling and safety procedures and wear

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ANU Centre for Sustainable Energy Systems (CSES)

Lab Tool-book checked date: Feb 2009 by Andrew Li

glasses, lab coat, plastic inner, yellow apron, and nitrile outer gloves at all times when handling this acid.

3.

Equipment & Resources

Use dedicated equipment for the NaOH etch processes, as it may have impurities that affect other chemical processes. The scale for weighing NaOH pellets should be kept in lab E122. Avoid using a fumehood that is used for other clean processing

4.

Procedure

The complete NaOH etch procedure will usually consist of the following (in typical order): 1. Prepare NaOH solution 2. HF dip (optional) 3. NaOH etch 4. Dirty RCA2 clean 5. HF dip (optional) 6. Final rinse

4.1.

NaOH Solution Preparation

The NaOH solution can be prepared using NaOH pellets, or from a pre-made NaOH solution. NaOH solution: o Add the required quantity of DI H2O o Add the required quantity of NaOH to the solution beaker. NaOH pellets: o In a fumehood, weigh out the NaOH pellets in a dry beaker on the weighing instrument o Add the NaOH pellets until you have the required weight o In another beaker, add the required quantity of DI H2O o Slowly add the NaOH pellets into the beaker of DI H2O o Use a pair of tweezers to slowly stir and dissolve the pellets

4.2.

HF Dip (optional - usually done prior to NaOH etch)

Note: User must be accredited in HF etching to be able to perform this pre-NaOH HF dip! Fill a plastic beaker with the required volume of DI H2O Measure the required volume of HF in a measuring cylinder and add to water; rinse measuring cylinder thoroughly using DI water. Remove the cradle and wafers from rinsing beaker and dip in solution for approximately 10 seconds until hydrophobic (the quartz cradle may be used here since it is only for a very short time period). BE CAREFUL NOT TO SPLASH THE SOLUTION Rinse cradle and wafers in the rinse bucket/beaker

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ANU Centre for Sustainable Energy Systems (CSES)

Lab Tool-book checked date: Feb 2009 by Andrew Li

4.3.

NaOH Etching
Place the NaOH solution beaker on the hotplate. Turn on the hotplate and heat the NaOH solution to the required temperature (up to 90 C). Do not allow it to boil rigorously. Fill rinse bucket/beaker with DI water Load wafers into designated glass cradle and immerse in NaOH solution for the required time. Rinse cradle and wafers in the rinse bucket/beaker.

4.4.

Dirty RCA2 Clean

The RCA2 solution is in the ratio of 5:1:1 of H2O: HCl: H2O2. Solutions may be measured approximately by pouring straight into a glass beaker with graduation markings, that is to used to perform the RCA2 clean. In a suitably sized glass beaker add required quantity of DI H2O and HCl in that order. Place RCA2 solution on the hotplate. When RCA2 solution is above 65C and before immersing wafers in solution, add required quantity of H2O2 to RCA2 beaker. Remove the cradle and wafers from rinsing beaker and immerse in RCA2 solution for 10min. The solution should bubble gently. Empty and refill the rinse bucket/beaker with DI water Rinse cradle and wafers in the rinse bucket/beaker.

4.5.

Final Rinse
Fill the required number of rinse buckets/beakers with DI water Do three separate DI beaker rinses (alternating between fresh beakers of DI water) or a three minute overflow rinse To dry the wafers, pull-dry from the water and/or dry using nitrogen gun

5.

Clean Up and Waste Disposal

A used NaOH solution may be store in a plastic container in a cool, dry, well-ventilated area. Keep containers securely sealed. DO NOT use aluminium, galvanised or tin-plated containers. DO NOT store near acids, or oxidising agents. To dispose of the NaOH solution, allow to cool then poured into a clearly marked NaOH waste bottle and set aside for collection by waste disposal contractors. To dispose of the RCA2 solution, allow to cool then pouring solution down the sink with plenty of town water running. Leave the town water running for at least 5 minutes afterwards. The HF solution should be put into waste containers as per the module for the HF etch process. Rinse all the process vessels thoroughly with DI water.

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ANU Centre for Sustainable Energy Systems (CSES)

Lab Tool-book checked date: Feb 2009 by Andrew Li

6.

Troubleshooting

If etching does not occur it is possible that an oxide is present on the wafer. HF dip the wafer to ensure the wafer is hydrophobic & try etching in NaOH solution again.

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