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ECE 344 Lab Safety

One bad accident could conceivably bring an end to the ECE 344 lab. Its excellent 20+ year safety history depends largely upon student preparedness, so the best thing you can do in the interest of safety is understand what you will be doing BEFORE you come to lab.

Here is some information which should help you stay out of danger.


Laboratory Chemicals

The chemicals required for IC fabrication are hazardous. The student is well advised to develop a healthy respect (if not fear) for the chemicals in the lab. Below is a brief listing of most of the chemicals in the lab. More detailed safety information can be found in the safety and MSDS (Material Safety Data Sheet) files in the top drawer of the filing cabinet in the lab. Please take a look at them when you have a chance (e.g., during a diffusion furnace operation).

NOTE: When using acids or organic solvents, ALWAYS wear gloves, goggles, and a face shield. Work under a fume hood.

Chemicals	:	Acetone, Isopropyl alcohol (IPA), Ethyl alcohol,   
                        Methyl alcohol, Trichloroethane (TCA) 
Use		:	Cleaning, organic solvents.
Handling	:	The above chemicals will irritate the skin if
                        not washed off as soon as possible.  If you use
                        gloves (especially plastic gloves) in handling the
                        above solvents, check them for holes before
                        handling acids.  All the above liquids have low
                        boiling points and evaporate quickly when left
                        standing in the open.


Chemical	:	HF (Hydrofluoric acid) 
Use		:	Dissolve SiO2 (and other glasses).
Handling	:	ALWAYS USE GLOVES.  HF, unlike other acids, 
                        does not burn immediately. HF is absorbed through 
                        the skin and dissociates into H and F ions. The 
			F ions bind with Ca in the blood stream, which
			can cause cardiac fibrillation.
			After handling HF, always rinse your hands 
                        carefully (even if you use gloves).  Make a 
                        special effort to rinse underneath the fingernails 
                        - a burn here really smarts.  If you spill HF on 
                        yourself, rinse the affected part in water 
                        immediately (although there is controversy
			about washing).  Have someone report to your TA
                        immediately while you are rinsing. 


Chemical	:	HN03 (Nitric acid) 
Use		:	Oxidize silicon.
Handling	:	Use gloves.  Nitric acid leaves a tell-tale 
                        yellow mark when it contacts the skin.  If you see 
                        yellow marks developing, wash the affected area _ 
                        small burns are seldom painful.


Chemical	:	H2SO4 (Sulfuric acid) 
Use		:	Inorganic and metallic solvent.
Handling	:	USE GLOVES.  Concentrated sulfuric acid is a 
                        powerful acid.  Have respect for it.  If it 
                        contacts the skin, the affected part quickly 
                        blisters.


Chemical	:	H202 (Hydrogen peroxide) 
Use		:	Oxidizing agent, passivation.
Handling	:	Use gloves.  This is concentrated stuff, not 
                        the household variety.


Chemical	:	Deionized water 
Use		:	Solvent, rinsing.  Deionized water is used for 
                        rinsing such things as tweezers, beakers, and 
                        other lab equipment.  In high purity work it is 
                        often used in the cleaning of semiconductor 
                        wafers.  Please do not use it to clean your hands. 
                       (use tap water).

NOTE:	We call deionized water DI


Chemical	:	AZ 5214 Photoresist 
Use		:	Photomasking (positive type).
Handling	:	Use under gold light to avoid polymerization.  
                        Use adequate ventilation.  Avoid contact with 
                        skin.  


Chemical	:	MIF 327 Developer  
Use		:	Develops positive resists after exposure to UV.
Handling	:	Use adequate ventilation.  Avoid contact with 
                        skin.


Chemical	:	Phosphoric Acid, H3PO4, Mixed 1:1:1 with HNO3 
                        and DI for "aluminum etch"  
Use		:	Removes Al from Si in unmasked areas.
Handling	:	Use gloves and goggles; heat only under hood 
                        (70 C).


Chemical	:	"Hot Oxide Etch" [6NH4F(40%):  1 HF] 
Use		:	Etches unmasked oxide layer on Si wafer.
Handling	:	Same as HF.


Chemical	:	HMDS (Hexamethyldisilazane) 
Use		:	To improve the adherence of the photoresist to the 
                        oxidized wafer.
Handling	:	Avoid contact with skin.



The remaining chemicals on this list are available in the 
lab, but not used in the current experiments.


Chemical	:	"6/l/l ETCH," HNO3/HF/CH3COOH 
Use		:	Slow but high quality Si wafer preparation.


Chemical	:	"l3/l/l ETCH," HNO3/HF/CH3COOH  
Use		:	Very slow but excellent, chemical-mechanical Si 
                        etch.


Chemicals	:	"4/l ETCH," HNO3/HF  
Use		:	Fast but imperfect etch (used for very thorough 
                        etch of alloyed device material where "wetting" is 
                        important but planar quality is not).
Handling	:	Quench all etches above with CH3COOH in a 
                        roughly equal volume; add half, decant, add 
                        remainder, decant, quench thoroughly (three times) 
                        with DI.  Always keep material submerged (all Si 
                        out of air) until ALL etch has been decanted in 
                        fifth quench.  As with any chemical containing HF, 
                        use gloves and goggles, care when swirling the 
                        beaker, and wash as per "HF Handling" above.  
                        Also, stir gently all pre-prepared etches before 
                        use to insure good mixing (GLOVES).  Fill the etch 
                        tubs with only enough etch to cover the wafers; 
                        they should never come anywhere near completely 
                        full unless specified in the text.

The Sinks and Fume Hoods

The fume hoods are designed for safety. Such materials as HF and trichloroethane give off fumes which are potentially dangerous. Always work with these chemicals at a fume hood - make sure the vent fan is ON. There are LED indicators and streamers to help you know if the proper fan is on. We have labeled waste containers for most of the chemicals used in ECE 344, but if chemicals must be dumped down the sink, always flush with plenty of tap water. This will keep the plumbers at home. Most drains are either plastic base or metallic base. You will be working with both organic and inorganic solvents and thus only sufficient flushing will keep the pipes intact. Used organic solvents are to be stored beneath the developer hood in bottles labeled with the contents and the word "waste", used acids go in the carbouy labeled "waste acids" in the acid hood (the lid must be left a bit lose except during transportation). Avoid pouring anything but water down the drain.

NOTE: Only expensive Teflon has no known solvent.

Furthermore:

  1. Always wear:
  2. Make use of the heavy acid gloves when handling acids or using the degreaser.
  3. All chemicals will be mixed by the instructor unless specified in the instructions. If you need something ask.
  4. Only the labeled beakers are allowed under the hoods, and only for use with the chemical so intended.
  5. Do not remove the labeled beakers from the acid hoods.
  6. Do not leave chemicals in unlabeled containers!

The following instructions will be posted as a sign at the ACID HOOD.

Etching (without etching yourself)

  1. PLACE WAFER(S) IN A POLYPROPYLENE WAFER CASSETTE.
  2. TURN ON THE RIGHT HAND FAUCET.
  3. PUT ON A PAIR OF HEAVY GLOVES.
  4. ARRANGE THE ACID(S) AND RINSES.
  5. WHILE FIRMLY HOLDING THE ACID CONTAINER WITH PALMS, USE INDEX FINGERS AND THUMBS TO SLOWLY RAISE THE FAR SIDE OF THE LID.
  6. PLACE ALL THE LIDS UPSIDE DOWN IN POSITIONS THAT KEEP THEM CLEAN AND EASY TO PICK UP.
  7. MOVE THE FIRST RINSE TANK(S) ALONG SIDE THE CORRESPONDING ACID TUB(S).
  8. GRIP WAFER CASSETTE HANDLE SUCH THAT DRIPS FROM THE GLOVE ARE UNLIKELY TO LAND ON THE WAFERS.
  9. SLOWLY IMMERSE THE WAFERS IN THE ACID AND BEGIN TIMING. ROTATE THE WAFERS SLOWLY BACK AND FORTH. DO NOT EVEN COME CLOSE TO SPLASHING!
  10. WHEN THE ETCH TIME HAS ELAPSED, TILT THE WAFER CASSETTE AND THEN SLOWLY RAISE IT OUT OF THE ACID.
  11. ALLOW FOR MOST OF THE ACID TO DRIP OFF FOR A FEW SECONDS, THEN QUENCH IN THE FIRST RINSE.
  12. AFTER AGITATING FOR 5-10 SECONDS, TRANSFER TO THE FINAL RINSE TANK FOR 20-30 SECONDS.
  13. RINSE A GLOVE UNDER THE FAUCET AND USE IT TO SPRAY THE WAFER CASSETTE WITH FRESH D.I. OVER THE SINK.
  14. IF NO OTHER ETCHES ARE NEEDED, SET THE WAFER CASSETTE ON A GLASS PLATE AND ONLY ON A GLASS PLATE.
  15. REPLACE THE LIDS AND SLOWLY PUSH THE TUBS TO THE BACK OF THE FUME HOOD.
  16. RINSE THE HEAVY GLOVES UNDER THE RUNNING FAUCET, TAKE THEM OFF AND LEAVE THEM TO DRY ON THE COUNTER.
  17. IF ACID DROPS ARE SUSPECTED, GENTLY SPRAY WITH D.I. AND N2 DRY OR ASK THE INSTRUCTOR FOR ASSISTANCE.
  18. TURN OFF THE FAUCET.

Furnaces

There are certain DO's and DON'TS, tips and tricks associated with working with furnaces. Some are obvious, some are not so obvious.

  1. The furnace tubes and pushrods are made of quartz, not glass. This enables them to withstand the high temperatures inside the furnace without melting. It also means that they are not cheap. Always handle the quartz with care. It is extremely fragile, especially the pushrod. Try not to exert a torque on any quartz part.
  2. Never touch the quartz furnace parts with your bare hands. There is the danger of getting yourself burned, and in addition, you will contaminate the furnace. Contaminants on your hands, particularly sodium, can be very detrimental to the experiment. Contamination will result even if you have just washed your hands, so always wear the zetex gloves provided. (Remember it is 1000 to 1200C inside the furnace.)
  3. If the furnace tube end cap does not come off easily (this often happens after wet oxidations) hold the tube steady with one hand (wear gloves) while removing the end cap with the other. It may help to tap the end lightly with a pen or some other blunt instrument. When replacing the end cap, put it on loosely; a tight fit is not necessary.
  4. Always return the pushrods to the labeled storage tubes provided along side the furnaces. It is essential that the proper rod be used in each furnace.
  5. Always store the empty boats in the front end of the furnace tubes. Do not exchange the boats between furnaces.
  6. Not all of the furnace is at the same temperature; only the center is at the desired temperature. So, when putting the boat into the furnace, try to make sure the boat center is within an inch of the furnace center.
  7. Do not adjust the furnace controls. They will be set at the temperature needed. Do not be fooled by the controller settings, they are sometimes different than the actual temperature used in the experiment. The thermocouple used in the control is outside the mullite tube; the temperature pertinent to the experiment is inside the quartz tube. Before the semester began a calibration was performed using a thermocouple placed inside each quartz tube to determine the controller settings. The electrical and gas controls associated with the furnaces are described in Appendix F. However, your instructor must make these adjustments.

A Final Word of Caution

Use care at all times (both for your sake and the sake of your wafer). If you move a wafer, carry it in your wafer carrier with the lid ON. If you MUST carry it in tweezers, cup your other hand under the wafer. In the event that it slips from the tweezers, it will fall into your hand rather than onto the floor. Two inch wafers are fragile! Previous students have broken their wafers by swishing them in a rinse tank or even simply squeezing too hard with their tweezers.

THINK SAFETY - Eyes and fingers must be protected. They cannot be (easily) replaced.

Cleanliness is of great importance in the fabrication process. Contaminants introduced during the process can degrade or destroy device performance. Therefore, it is important that processing equipment or chemicals are never touched with the bare hands, (i.e., diffusion furnaces, push rods, boats, etc.) Not only do the bare hands contain dirt and oils, but also sodium which can easily destroy FETs. Always handle the wafer with clean tweezers. A good rule to remember is to never touch anything with your bare hands that will come in contact with the wafer. Always consult the instructor if any mistakes are made in processing. Always consult your instructor at the beginning of the period for any special processing instructions. Often the instructor will call a short meeting at the beginning to make such announcements to everyone at once.

Photoresist should not be left on wafers overnight. Do not begin a photoresist operation unless you are confident you can finish it. At the beginning of the semester a PR patterning process will take a little over an hour. Later, it will go more quickly.

Always wipe your feet well on each rug as you enter the complex. Leave most of your stuff outside the cleanroom. Bring only your lab manual, notebook, and a pen into the lab. Use the shoe cleaner before entering the gownroom. Wait outside if there are already three persons in the gownroom. Don your tyvek coveralls and cap while on the "dirty" side of the bench. If you do not wear glasses, put on a pair of safety glasses or goggles. Contact lenses are unnecessarily risky because they can hold chemicals against your eye. Please do not use them when you come to lab. Put on the booties as you step onto the "clean" side of the bench. Never step on the dirty side of the gownroom with booties on. As you enter the cleanroom, take a couple of steps on the tacky mat to remove lint from the booties. Never ever enter the wet lab without gloves and a face shield (and glasses).

It is of the utmost importance that processing instructions be performed carefully, step by step, as outlined. Of equal importance is the requirement of absolute cleanliness. Industrial fab labs often spend as much or more on "clean" as on the equipment in the lab. In this laboratory, however, we must be satisfied with observing basic precautions. Always clean tweezers in the vapor degreaser before use. When a rinse with DI water is called for, rinse thoroughly with copious quantities of water. Any strange stains or spots which may develop on the wafer should be called to the attention of the lab instructor for analysis and treatment.

To fight pollution and cost overruns, use all chemicals sparingly; i.e., never scrimp on cleanliness, but avoid excess.

Read instructions carefully, think about what must be done, and then do it with care. It is imperative that you read the instructions through completely before coming to lab. Watch for changes, corrections, or addenda. These will normally be posted in the Network Newsgroup: uiuc.class.ece344. This manual is revised frequently, but last minute changes may be added during the course of the semester. This is particularly true now that the manual is available on the World Wide Web.


ECE 344 home page.

This screen was created by Mike Fitzimmons - U of Illinois ECE Dept. - mikef@uiuc.edu,
and is maintained by Dane Sievers - U of Illinois ECE Dept. - dsievers@uiuc.edu
E-mail comments and suggestions to ece344@uiuc.edu or use the FEEDBACK FORM.
safety.html updated 05/5/98

Warning! This is the archived 1999 Fabweb site! Here is the latest site