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STANFORD NANO SHARED FACILITY

GENERAL CLEANROOM MANUAL

The Flexible Cleanroom (FCR)

Spilker Building

Rooms 131A-K

Stanford Nano Patterning Cleanroom (NPC)

Spilker Building

Rooms 005 and 006

Revised September, 2017

Table of Contents

Emergency Numbersii

Flexible Cleanroom (FCR)iii

Nano Patterning Cleanroom (NPC)iii

1. Lab Basics1

1.1 Tool Training1

1.2 Layout of the Lab2

1.3 Laboratory Access and Hours of Operation2

1.4 Equipment Responsibility3

1.5 Broken Equipment3

1.6 Gowning Procedure4

1.7 General Cleanroom Practices (both Labs)5

1.8 Laboratory Etiquette6

1.9 Visitors7

1.10 Personal Tools, Belongings and Equipment8

2. Lab Safety8

2.1 Cleanroom Staff Responsibilities8

2.2 Lab User Responsibilities8

2.3 General Cleanroom Safety8

2.4 Safety Considerations10

2.5 Appropriate Street Clothing and Shoes10

2.6 Eye Protection10

2.7 Personal Protective Equipment11

2.8 Buddy System11

2.9 Special Health Concerns11

3. Facility Hazards Overview11

3.1 Chemical Hazsards11

3.2 Electrical Hazards11

3.3 Other Hazards12

4. Chemical Safety Information12

4.1 Manufacturers Chemical Labels12

4.2 Secondary Use Labels12

4.3 Required Lab/Cleanroom Specific Labels12

4.4 Safety Data Sheets (SDS)13

5. Chemical Hazard Classes13

5.1 Liquid Chemical Hazard Categories13

5.1.1 Solvents13

5.1.2 Corrosives14

5.1.3 Oxidizers14

5.1.4 Water Reactive Chemicals14

5.1.5 Flammables15

5.1.6 Toxic/Poison15

5.1.7 Non-toxic15

5.2 Resists and Other Chemicals15

5.2.1 Other Chemicals in the Flexible Cleanroom16

5.3 Miscellaneous Materials16

6. Chemical Storage17

6.1 Background17

6.1.1 Flammables17

6.1.2 Corrosives17

6.1.3 Oxidizers17

6.2 General Use Chemicals17

6.3 Introducing New Chemicals18

6.4 Personal Chemical Storage18

7. Chemical Handling18

7.1 Personal Protective Equipment18

7.2 Safe Operating Procedures19

7.3. Chemical Exposure19

7.4 Transporting Chemicals to/in the Lab19

7.5 Chemical/Hazardous Waste Collection and Disposal19

7.6 Solid Hazardous Waste Disposal21

7.7 Chemical Spills21

8. Emergency Information22

8.1 Emergency Equipment22

8.2 Emergency Exit Information22

8.3 General Emergency Response23

8.4 Posted Emergency Response Procedures23

8.5 Life threatening medical emergency23

8.6 Evacuations23

8.6.1 Building Evacuation23

8.6.2 Laboratory Evacuation24

8.6.3 Wet Bench Room Evacuation and Isolation24

8.6.4 Odors in the Lab24

8.6.5 Lab Fire24

8.6.6 Fire Alarms25

8.6.7 Electrical Power Outage25

8.6.8 Major Earthquake25

8.6.9 Water on Floors25

9. Reporting Accidents25

9.1 Incident Reporting25

9.2 Follow-up26

10. Medical Providers or Work Related Injuries26

Appendix A: Working with Hydrofluoric Acid (HF)27

Appendix B: Chemicals in the Nano Patterning Cleanroom28

Appendix C: Flexible Cleanroom Map29

Appendix D: Nano Patterning Cleanroom Map30

Emergency Numbers

Emergency Phone NumbersFrom Campus PhoneFrom Cell Phone

Life Threatening Emergency9-911650-321-4433

EH&S Emergency Line (chemical spills)x5-9999650-725-9999

Health & Safety Info 24 hourx3-0448650-723-0448

Facilities Quick Response (broken pipe)x3-2281650-723-2281

Stanford Hospital Emergency Roomx3-5111650-723-5111

Vaden Student Health Centerx4-2273650-724-2273

California Poison Control 9-1-800-222-1222 800-222-1222

Flexible Cleanroom (FCR)

Room 131A 6507252292

Room 131C (yellow room) 6507252293

Room 131G (Microfab Shop)6507259183

Phone in hallway outside of lab 6507252283

Tom Carver (Lab Mgr.) office x31861 6507231861

Tom Carver cell (emergencies) 915107927691 5107927691

Anthony To (Building Manager) x2-8306 650-272-8306

Address of this Lab: Flexible Cleanroom,

Rooms 131 AK,

Spilker Building # 04040

348 Via Pueblo

Stanford, CA 94305

Nano Patterning Cleanroom (NPC)

CAD Computer Station 650-723-8584

JEOL Desk 650-723-8586

Nova Nano SEM650-723-8587

Cliff Knollenberg (Desk)cknollen@stanford.edu 650-723-1675

Shiva Bhaskaran (Desk) bshiva@stanford.edu 650-498-5653

Rich Tiberio (Desk)tiberio@stanford.edu 650-725-2299

Anthony To (Building Manager) anthony.to@stanford.edu 650-272-8306

Address of this Lab: Stanford Nano Shared Facilities Rooms 006 A-H (basement)

Spilker Building #04-040

348 Via Pueblo

Stanford, CA 94305

Stanford Nano Shared Facilities General Cleanroom Manual

iii

SNSF General Cleanroom Manual

Page 17

Ver. 1.1Sept. 2017

1. Lab Basics

Setting up a Badger Account at SNSF:

All users must have and maintain a valid SNSF Badger account. You must verify that your account is active before requesting training within the Flexible Cleanroom or the Nano Patterning Cleanroom. If you have not completed this step, refer to http://snsf.stanford.edu/about/join.html to join SNSF and create a Badger account.

SNF Users: Please note here that SNSF Badger is separate from SNF Badger!

All new users are required to review the Stanfords Chemical Hygiene Plan prior to working in the lab. https://ehs.stanford.edu/manual/chemical-hygiene-plan

1.1 Tool Training

Many of the pieces of equipment in the lab require additional handson training. Many of the machines have a person in charge or staff member whom is the first person you should talk to. Never use a machine that you have not been trained on even if you think you know how to use it already, because each machine has its own little quirks and special problems you will need to learn about.

In the Flexible Cleanroom

You will need to be checked off by the person in charge on the operation of a machine before you can use it. At the discretion of the person in charge of that machine (or of the Lab Supervisor), you may be checked off on that machine by another person familiar with the machine or by demonstrating prior experience and knowledge of that particular machine. If you have been checked out on one machine, it doesn't necessarily give you the right to check someone else out on that machine. Check first with the person in charge before training anyone new yourself.

The Ion Milling Machine, Oerlikon Leybold Univex Sputter, and possibly other new machines, are reserved and monitored via the Badger user interface. Most other machines are first come, first serve.

On the following page is a list of who is in charge of some of the major pieces of equipment in the Flexible Cleanroom:

Oerlikon Leybold Univex Sputter: Tom Carver, carver@stanford.edu 650 7231861

Intlvac Ion Milling Machine: Cliff Knollenberg, cknollen@stanford.edu 650-7231675

Quintel Mask Aligner: Carsten Langrock, langrock@stanford.edu 7230464

Karl Suss Mask Aligner: John Bartel, jbartel@stanford.edu 650 7252407

Plasma Etcher: Tom Carver, John Bartel

Knowledgeable users: John Bartel , jbartel@stanford.edu 650 7252407

Olympus Microscope (in yellow room): Volunteers?

Knowledgeable users: Carsten Langrock, langrock@stanford.edu

Rapid Thermal Annealer: Volunteers?

Everything else: Check with Tom Carver carver@stanford.edu 650 7231861

In the Nano Patterning Cleanroom

The Person In Charge is usually a staff member who provides maintenance and trainings on the tool. Contact them regarding tool training for the Badger interlocked tools below. On some of the smaller and simpler tools, a written list of instructions is available for user to review. If after reviewing these directions they do not feel comfortable on a machine, they may contact a staff member for additional training.

JEOL e-beam writer: Rich Tiberio tiberio@stanford.edu

Nova SEM: Cliff Knollenberg cknollen@stanford.edu

KJ Lesker e-beam Evaporator: Shiva Bhaskaran bshiva@stanford.edu

Keyence 3D Lase Confocal Microscope: Shiva Bhaskaran bshiva@stanford.edu

Oxford RIE: Usha Raghuram usha@stanford.edu or Cliff Knollenberg cknollen@stanford.edu

Cressington Sputter Coater: Cliff Knollenberg cknollen@stanford.edu

1.2 Layout of the Lab

The cleanrooms are accessible only from their respective gowning rooms.

In the Flexible Cleanroom:

You will see four doors which lead from the cleanroom to narrow service chases. These service chases are not clean. They act as the return path of laminar flow air which circulates through the lab. Do not enter these service chases from the cleanroom, because the dirty floors in them will contaminate your booties. When its necessary to move chemicals from the storage cabinets in the service chases to the cleanroom, please see Tom Carver. There are pass-throughs to use for passing chemicals or other things back and forth between the service chases and the cleanroom. There is also a passthrough to pass things into the cleanroom from the gowning room without having to completely gown up. The yellow room is where all photolithography is done, as well as all chemical processing. Please keep the door to the yellow room closed to avoid white light from exposing photoresist that people may be working with. Due to the high return ducts, there is a small amount of white light that is unavoidable, so keep any unexposed photoresistcoated samples in a dark container or wrapped up in aluminum foil if they need to stay in that room for extended periods of time. Keep in mind when working with chemicals in the yellow room that there may be people trying to do very critical lithography. Avoid stirring up dust and keep the door shut. At the far end of the lab is the Lab Supervisors work area, including two evaporation stations, and four workbenches. Please do not use any of these machines or work areas and do not use any of the tools or fixtures on those benches because they are cleaned for ultra-high vacuum.

In the Nano Patterning Cleanroom:

The Nano Patterning Cleanroom (006 Suite in the Spilker Building) is accessed by swiping your access card outside the gowning room on the right of the lab. 005 Spilker which is used primarily for storing chemicals and cleanroom supplies is the next door to the right. Upon entering the gowning room users may store backpacks in the lockers and don cleanroom attire. Note that all lab users are required to wear nitrile gloves and safety glasses (required PPE) while working inside the lab. The only exception to this is that lab users are not required to wear safety glasses while sitting directly in front of a microscope. Failure to wear the required PPE may result in the loss of access to SNSF facilities. Additional Personal Protective Equipment maybe necessary when working with chemicals in the wet bench room. After donning the required cleanroom attire, the white light rooms may be entered through the door to the left. The white light rooms hold tools for processing steps where the filtered (yellow) light is not necessary to prevent accidental exposure of resist. These tools currently include the KJ Lesker e-beam evaporator, Oxford Reactive Ion Etcher (RIE), the Keyence 3D scanning confocal laser microscope, and the CAD computer station with the Genisys software package. Behind the white light rooms are the filtered light (yellow light) rooms which help prevent the accidental exposure of undeveloped resist before and after exposure in the writing tools. Unfortunately, a small amount of white light is unavoidable, so keep any unexposed photoresistcoated samples in a dark container or wrapped up in aluminum foil. The tools in the yellow rooms include the JEOL e-beam writing tool, the Nova SEM (with Nabity e-beam writing package), the Cressington Sputter Coater, the optical inspection microscope, Dektak stylus profiler, FilmSense Ellipsometer, and the wet benches for wet chemical processing. The JEOL and Nova SEM tools are located in the rooms at the back of the lab furthest from the entry hallway and the JEOL has an operator station located immediately in front of its room. The wet benches are located in a room on the right of the lab which is immediately behind (and visible from) the gowning room and is connected by a door to 005 Spilker.

1.3 Laboratory Access and Hours of Operation

All users must fully understand the rules and regulations pertaining to the lab and its use. Access will be granted to all new users who have:

1. Been issued a Badger Account and have set it up,

2. Read and have a working understanding of the Cleanroom Manual

3. Filled out the Access Authorization Form for the Flexible Cleanroom or the Lab Safety Protocol Checklist for the Nano Patterning Cleanroom,

4. Completed all necessary online and handson safety training,

5. Keep their Badger account current with an active PTA.

New users may be required to take a short quiz covering the areas of laboratory conduct, laboratory safety, and hazardous waste storage and labeling. It is very important that all new users read and understand the contents of this manual.

Once your I.D. card has been activated to access the lab, your I.D. card is for YOUR USE ONLY. Every time you use your I.D. card to access the lab, you are entered into the Badger accounting system as a user for that particular day, and you will be billed for each day that you use the lab. Never loan your card to someone else, because YOU will be held accountable for what that person does in the lab. If you loan your cardkey to someone else, this may become grounds for revocation of your access and possible disciplinary action.

Besides gaining access to the lab, you will also need to be checked out or trained on each individual piece of equipment that you want to use by the person responsible for that piece of equipment.

Good communication is essential to the operation of the lab. Please read your email routinely for messages pertaining to the lab, check the bulletin board next to the lab entrance, and read notices posted on pieces of equipment.

The lab is open 24 hours a day to qualified users, subject to the provision that at least one other person who is also a lab user is present outside of normal weekday working hours. Some temporary users may be restricted to normal business hours.

1.4 Equipment Responsibility

Check out: Most major pieces of equipment will have one designated person or staff member whose responsibility it will be to instruct and train others in the use of that equipment. A person will be considered "checked out" or trained when the person responsible is satisfied that the user understands the proper operation and has demonstrated competence in its use. Competence means that the user:

1. Logs in before using equipment by entering the time and date, and also indicates problems experienced in operation (either in the provided log in sheets or by using Badger).

2. Can operate equipment safely without supervision.

3. Knows what to do in case of an emergency.

4. Knows how to clean up and how to leave the equipment when he/she is finished (default settings for switches, etc.).

5. Reads and understands the "how to" or Safe Operating Procedures card posted on equipment.

1.5 Broken Equipment

When equipment fails to operate properly, whether through natural causes or improper use, the current user will IMMEDIATELY notify the person responsible for the equipment and/or the lab supervisor or the supervising staff member, then either repair it him/herself if its a simple fix and if competent to do so, or work out a way to repair it with the person responsible. If it's impossible to reach the responsible person or the lab supervisor, the equipment must be plainly signed indicating that it is temporarily inoperative (or by emailing the user list and posting a Problem or Shutdown on Badger) and messages should be left for early notification of the responsible individuals.

When to Shutdown a broken tool on Badger:

1. If the issue is dangerous to lab users.

2. If the issue is dangerous to the tool.

3. The tool is doing something that could ruin users samples.

4. Something is so wrong that no one should use the machine.

When to enter a Problem on Badger:

1. Some aspect is not working correctly, but some users may be able to use other aspects without a problem.

2. The tool is working, but not in the normal way and this could affect the results users see on their samples.

Important note: It should be understood that research advisors shall pay for repairs of any equipment broken by a member of his/her group if the damage is due to improper or careless usage. In shared negligence, there will be a fractional analysis of responsibility and the cost will be split accordingly.

1.6 Gowning Procedure

Class 100 Gowning Procedure for the Flexible Cleanroom

1. Leave your belongings in a locker and keep the key in your pocket.

2. Before entering the gowning room, please make sure there is no mud, grass, or sand on your shoes. If your shoes are messed up, please leave your shoes in a locker. Do not take any paper, pencils, cardboard, food, wood, etc. into the cleanroom (cleanroom paper is okay).

3. Use air hose by door to dust off anything you need to carry into the lab, including laptop computers.

4. Enter the gowning room and step onto the sticky mat. Get a pair of the First Booties. Take your pick of whichever style light blue bootie fits over your shoes. You can sit down on the bench while you put your first booties on. Your street shoes should only touch the first sticky mat and the floor just in front of the first bench. Do not step onto the dirty sticky mat with your First Booties.

5. Walk around the bench and put on a hood or a hat. The hood is recommended if you are doing lithography or anything critical. The hats are okay for most other things and much cooler to wear. Tuck all of your hair into the hat.

6. Put on your Tyvek coverall (write your name on your jumpsuit so you can wear it multiple times). If you have a hood on, the jumpsuit should go over the base of the hood.

7. Put on either the medium or large white Tyvek booties and tie the ankles. There are new booties in bins on the shelf, but we can reuse booties several times if theyre in decent condition. The used booties will be in the shelves under the other bench (against the rear wall). Sit down on the other bench (the bench against the wall) while you tie your booties.

8. Put on your gloves from the glove bins near the door to the lab.

9. Use your knuckles or elbow to turn the door handle and enter the lab.

10. If you are going to be working around any chemicals, put on a pair of safety glasses and/or a safety face shield. The safety glasses are in a rack on the wall just inside of the cleanroom.

11. Use the passthrough if you need to carry any stuff into the lab or if you need to pass something to someone in the lab without gowning up.

Note: Do not step on the sticky mat that leads into the lab from the gowning room unless you already have the white (second pair) booties on. And once you have your white booties on, do not step on the dirty sticky mat by the gowning room entrance.

Procedure for UnGowning and Leaving the Flexible Cleanroom

1. Sit down on the bench where the booties are stored and take off your booties. If they are clean, you can put them in the shelf under that bench to be reused. Keep large booties on the upper shelf, and medium booties on the lower shelf. If they are dirty or ripped, throw them away.

2. Take off your coverall and put it on a hanger; your coverall should have your name on it, but if its ripped or ruined, throw it in the garbage. The coveralls are organized alphabetically by last name. Please write your full name on the back of your coveralls. You can save your hood or hat for reuse by hanging it on the lower bar of the hanger inside your coverall.

3. Move to the other bench, and remove your blue first booties BEFORE stepping on the dirty sticky mat. If they are pretty clean still, save them for reuse in the bin under that bench. If they are dirty, throw them away. Please do not turn your booties inside-out, otherwise the next person will have them dirty side out.

4. Exit the lab.

Note: please make sure you have picked up everything. Dont leave booties, hats, etc. on the floor. If any garbage like dirt clods falls out of your booties onto the floor, please use the cleanroom vacuum to clean up the mess.

Note: Cleanroom apparel is expensive, so please try to reuse anything that you can. By reusing things until they are ruined or dirty, you can keep the overhead costs down, which will also keep your lab user access fee down. This will also cut down on landfill waste.

Gowning Procedure Nano Patterning Cleanroom

1. Leave your belongings in a locker on the floor by the lockers.

2. Before entering the gowning room, please make sure there is no mud, grass, or sand on your shoes. Use the shoe cleaner outside if necessary. If your shoes are messed up, please leave your shoes in a locker.

3. Do not take any paper, pencils, cardboard, food, wood, etc. into the cleanroom (cleanroom paper is okay).

4. Use air hose by door to dust off anything you need to carry into the lab, including laptop computers.

5. Enter the gowning room and step onto the sticky mat. Get a pair of the blue First Booties. You can sit down on the bench while you put your first booties on. Do not step onto the dirty sticky mat with your First Booties.

6. Put on a First Hood or bouffant hat. Tuck all of your hair into the hat.

7. Put on an appropriately sized polyester hood from the containers to the right of the entry. Be warned that hood size seems to correlate with volume of hair more strongly than head size.

8. Select an appropriate sized polyester coverall from the lab user labeled hangers or the visitor hangers. Fresh coveralls of various sizes are kept in labeled containers on the racks about/above eye level. Lab user hangers are for the users who find themselves using the lab more than once a week. The cloth garments are swapped out and sent to cleaners once a week, and for lab users that use the lab less than once a week we recommend using the garments on the visitor hangers.

9. Sit on the stainless steel bench in front of the cleanroom entry door and select an appropriately sized polyester boot. Put it on over your blue shoe cover, tighten the bottom adjustments around your shoe and then snap the calf adjustment strap at the top.

10. Put on a pair of nitrile gloves from the glove bins near the door to the lab.

11. Safety Glasses are mandatory inside the lab and are provided in racks just before the entry door to the cleanroom. Face shields are available inside the wet bench room for working with especially dangerous chemicals (Hydrofluoric Acid, Sulfuric Acid or Piranha, and 25% TMAH).

12. Use your knuckles or elbow to turn the door handle and enter the lab.

13. Use the passthrough if you need to transfer items into the lab or if you need to pass something to someone in the lab without gowning up.

Note: Do not step on the sticky mat that leads into the lab from the gowning room unless you already have the white (second pair) booties on. Once you have your white booties on, do not step on the dirty sticky mat by the gowning room entrance.

Procedure for UnGowning and Leaving the Nano Patterning Cleanroom

1. Sit down on the bench where the booties are stored and take off your booties. If they are clean, you can put them in the shelf under that bench to be reused. Put booties in the slots appropriate for their size. Do not throw away booties in the trash! Put dirty booties in the blue cloth bag by the coverall hangers.

2. Take off your coverall and put it on a hanger with your name on it. If you are an infrequent user (less than once a week), put it on a visitor hook. Snap the hood to the collar.

3. Move to the other bench, and remove your blue first booties BEFORE stepping on the dirty sticky mat. If they are pretty clean still, save them for reuse in the bin next to that bench. If they are dirty, throw them away in the trash.

4. Exit the lab.

Note: please make sure you have picked up everything. Dont leave booties, hats, etc. on the floor. If any garbage like dirt clods fall out of your booties onto the floor, please use the cleanroom vacuum to clean up the mess.

1.7 General Cleanroom Practices (both Labs)

The Flexible Cleanroom and Nano Patterning Cleanroom are "Class 100" (ISO Class 5) cleanrooms. To maintain this level of cleanliness, it is important to follow these general cleanroom practices:

The user should gown and ungown using the procedures above, making sure to remember that the dirty street shoes only touch the first sticky mat. The first set of blue booties are only for walking in to the gowning area. Do not walk on the first dirty sticky mat with the blue booties.

Anything brought into the cleanroom should be dustfree or cleanroom compatible. An air hose by the door to the lab is helpful for blowing dust off equipment, bottles, and dusty clothes. Some items, like old equipment, may require a thorough wipedown with damp wipers. Only cleanroom paper should be brought into the cleanroom. Pens (ballpoint or felt tip) are okay. Pencils are not allowed.

Laptop and tablet computers are allowed, but must be wiped down or blown off with N2 prior to entering the clean room.

Food, cigarettes, gum, paper bags, and cardboard boxes are prohibited.

People are the main source of dust in the lab, so try to avoid making unnecessary trips into the lab whenever possible. For instance, if you need something from the lab, it would be better to call into the lab and ask someone to hand it out to you, rather than gowning up and going in and out. Avoid taking visitors into the lab if it's not absolutely necessary.

The countertops should always be spotless. They should be wiped down thoroughly after use.

Anything left unattended without a written explanation shall be considered trash and either be put in the lost and found shelf or thrown out.

When pouring from bottles, care should be taken to wipe any residue or dribbles from the neck and side of the bottle.

Great care should be taken to make sure that acids, photoresists, developers, and other chemicals don't get spread around by touching things with contaminated gloves. Do not touch switches, phones, splash shields, etc. with chemical soaked gloves. One drop of hydrofluoric acid, for example, if transferred onto the phone receiver or a doorknob could give somebody a severe burn. Small drops of photoresist or powerful solvents can permanently stain or destroy things like spinner control digital display panels and acrylic plastic splash shields. One smudge of uncured PDMS or silicone oil can ruin other lab users processes by making surfaces hydrophobic.

In the Flexible Cleanroom: Whenever a wastebasket is near full, it is the user's responsibility to tie up the liner full of trash, replace the liner with a fresh one from the supply cabinet, and take the bag of trash outside when through using the lab.

Powders should be avoided (purchase chemicals in granular form, rather than powder).

When boiling liquids, always place a watch glass over the beaker to avoid having excess amounts of vapor come off, which may condense all over everything in the wetbench.

Avoid unnecessarily wandering around the lab. Whenever possible, stay clear of areas where other users may be doing highly critical work. Just walking by can ruin some operations such as optical bonding or spinning resist on a pyroelectric substrate.

While your own work may not require class 100 cleanliness, be sensitive to the fact that other users may need things as clean as possible.

To facilitate unobstructed laminar flow of air in wetbenches, do not leave any unnecessary items out on the countertops.

When you are through using glassware, wipe it dry and put it away. Do not leave glassware to dry on the countertop, because that usually results in it sitting there forever, and in other lab users way.

1.8 Laboratory Etiquette

These are the rules of conduct for the lab, which are necessary to keep the numerous lab users from annoying, injuring, or killing each other.

1. Turn off equipment when you're finished using it.

2. Don't take up any more space than necessary when working at the wetbenches.

3. Put EVERYTHING away when you're finished.

4. Don't leave glassware drying FOREVER.

5. Wipe down everything when you're finished.

6. Your work area should be DRY when finished.

7. Don't tie up equipment any longer than necessary.

8. Don't bring in visitors without checking with the lab supervisor first.

9. Don't allow visitors to touch ANYTHING, especially chemicals.

10. Don't touch the personal property of someone else.

11. Don't touch anything in the sputter/evaporation stations, or the lab supervisor's work areas in the Flexible Cleanroom (these have vacuumclean tools and parts).

12. Do not borrow anything without the owner's permission.

13. Bring in your own pen(s) and/or cleanroom notebooks if you know you'll need them.

14. Don't use equipment that you haven't been trained on!!!!!

15. Purchase your own tweezers and glassware.

16. Leave equipment exactly like you found it (clean, switches, and adjustments in the normal positions/settings).

17. Read notes on bulletin boards, posted signs, email, and on individual pieces of equipment.

18. Leave notes in equipment logbooks or on Badger if anything strange happens.

19. Remember to log into equipment logs or by using Badger

20. Immediately notify the responsible people for any equipment failures or problems.

21. Peel up sticky mat top sheets when they get particularly dirty.

22. Notify lab supervisor of: chemical shortages, poor D.I. purity, supply shortages, leaks, disasters, spills, etc.

23. Refill dispensers of gloves, wipers, solvents, Micro detergent, Qtips whenever you empty or nearempty them. Solvent squeeze bottles should be considered empty when less than half full.

24. Notify lab staff if acid, base, or solvent dumps are near full.

25. If a waste carboy alarm goes off, hit the button to silence alarm and put a note over cupsink to let the next user know that the carboy is full.

26. Label all chemicals properly (see sections on chemical storage and labeling).

27. If you must leave anything out on the bench unattended, leave a note describing what it is, what the chemicals are, your name, and when you'll be back (in the Nano Patterning Cleanroom leave a blue Chemical-In-Use tag with this information). You also need to describe what the hazards are, if any. (flammable, corrosive, toxic, etc.)

28. Before you start working with any chemicals, you should know how you're going to dispose of them first. See the lab supervisor anytime you're unsure.

29. Don't ever pour anything but the acids we supply in the acid waste cupsink.

30. Dont ever pour anything but bases in the base waste cupsink.

31. Don't ever pour anything but the solvents we supply in the solvent cupsinks.

32. In the Flexible Cleanroom: DON'T EVER POUR DEVELOPER IN THE SOLVENT DRAIN!

Note: In the Nano Patterning Cleanroom: some of the developers for e-beam resist are solvents, so this rule is relaxed.

33. Never use chemical abbreviations on labels always spell them out. (example: instead of "HF", it must say "hydrofluoric acid", or instead of "H2O", it has to say "water".

34. Always label waste containers properly. If the waste is hazardous it must say "HAZARDOUS WASTE", list the hazards, show your name, show the accumulation start date, list the contents, and specify the physical state of the chemical (solid, liquid, sludge etc.)

35. Never leave any hazardous waste in the lab for more than 9 months.

36. Don't turn on the safety shower or eyewashes unless it's a real emergency. (they pour onto the floor)

37. Don't do any wet processing at night or on the weekends without another qualified user in the lab with you.

38. Don't bring food, gum, cigarettes, paper bags, cardboard boxes, animals, plants, drugs, liquor or dust bunnies into the lab.

39. Be courteous, kind, helpful, polite, and respectful to your fellow lab users.

40. See a lab supervisor or staff member whenever you need help, don't understand something, have a question, or have a complaint about another user.

41. Feel free to make suggestions that will improve the lab.

42. Make sure items are labeled with an active lab users name, not group name. We want to know who to contact when an issue arises.

1.9 Visitors

If you have someone you would like to bring into the lab (a friend, colleague, brother, etc.), please check first with the lab supervisor. Any visitors brought into the lab must be shown how to gown correctly, be informed not to touch anything, and not be left unsupervised. It is NOT OK to bring in a visitor for the purposes of allowing the visitor to use equipment in the lab. The lab is only for the use of trained, qualified, legitimate users. Loaning your cardkey to an unauthorized person will be grounds for having your cardkey disabled.

1.10 Personal Tools, Belongings and Equipment

There is a limited amount of storage space available in the lab for personal items like tweezers, glassware and masks.

Do not touch, borrow, or steal things from other user's personal storage.

Large pieces of equipment such as signal generators should have a responsible persons name on it (not a group name).

All Chemicals must be stored in designated chemical storage areas as indicated in Section 6: Chemical Storage.

In the Flexible Cleanroom: Please keep your belongings in some type of container that has your name on it. A small plastic toolbox or a clear plastic tote works well for this purpose. If there is anything too large to fit in a box, please write your name on it. Do not touch anything in the vacuum station work areas or the lab supervisor's workbenches. These items are vacuum clean. Do not borrow any of the lab supervisor's glassware, tweezers, tools, etc. There is a small, orange toolbox full of tools for common use. If you use one of these tools, please return it when you are through using it.

In the Nano Patterning Cleanroom: Drawers, boxes, and shelf space within the cleanroom are numbered and assigned to active lab users on a yearly basis. Once a year the assignments must be renewed. Un-renewed space will be cleaned out and released to users on the waiting list. New users may request space by emailing lab staff at nano-snpcleanroom-staff@lists.stanford.edu. You must label your storage space and all items with your name or user name.

2. Lab Safety

The primary goal of safety programs is the prevention of accidents through the education of the lab user community. This is achievable through the understanding of safety hazards, the adherence to the safety policies, and the expectation of self-policing between our lab user and the lab user community. The secondary goal of a safety program is learning and applying the correct response in a safety or emergency event.

2.1 Cleanroom Staff Responsibilities

The responsibility of the Staff within the facility regarding safety is to:

1. Inform the lab member community of potential safety hazards within the facility

2. Provide the appropriate personal protective equipment (PPE)

3. Maintain a current SDS binder

4. Verify the safe operation of all facility equipment.

2.2 Lab User Responsibilities

The responsibility of the lab user within the facility regarding safety is to:

1. Follow the safety guidelines of the facility at all times

2. Operate in a safe and professional manner at all times

3. Take responsibility for your own and other lab members safety at all times

4. Report any unsafe conditions, or unsafe practices of their fellow lab users to the facility staff

5. Submit any suggestion for improving safety to the facility staff.

WARNING: Any lab member not adhering to the SNSF Code of Conduct or the safety rules set down by this manual, either intentionally or unintentionally will be subject to administrative action and this may result in a loss of lab privileges. See SNSF general policies at: http://snsf.stanford.edu/labmembers/policies.html

2.3 General Cleanroom Safety

Personal safety and the safety of other lab users should always be the top consideration when working in the lab.

The required lab coveralls, booties and gloves offer limited protection against chemical spills, but protective eyewear, face shields, aprons, and appropriate gloves should always be used when working with hazardous chemicals.

Contact lens wearers should be aware that solvents and other chemicals can become trapped between the lens and the eye causing severe eye damage. All lab users should always wear eye protection when working anywhere near chemicals.

The airflow characteristics of the fume hoods should be well understood to avoid bringing hazardous fumes into the work area. Always keep hazardous chemicals toward the back of the bench when possible. Use watch glasses over open containers to minimize volatile fumes. Don't block the path of air to the exhaust of the fume hoods. Don't wave arms around or do anything that would bring fumes out into the room.

Be aware of the flammability of most solvents, acetic acid, photoresists and other chemicals. Watch temperatures of solvents diligently when using hotplates to avoid boil overs or reaching flashpoints. Never leave a solvent or anything flammable on a hotplate unattended.

No chemicals shall be left unlabeled and unattended on the work surfaces. All chemicals in the lab must be labeled properly (see the sections of this manual on chemical labeling and storage), be placed on the chemical inventory, and must have an MSDS on file.

If a long process requires leaving any chemicals out on the wetbench unattended for any time at all, it is the user's responsibility to post a sign stating what the chemicals are, what the hazards of the chemicals are, the user's name, and the time when the user will be returning to the lab (In the Nano Patterning Cleanroom leave a Chemical-In-Use tag with this information).

Do not assume that other users will know what your chemicals are. If some of the chemical were to splash on another user, it is imperative for emergency personnel that the identity of the chemical be known immediately (so label your chemicals).

The work area should be thoroughly cleaned and wiped down whenever you're through using the lab.

When pouring from bottles, the neck and side of the bottle should be wiped clean. Any spills or dribbles, no matter how small, shall be cleaned up thoroughly.

Any dribbles on the waste containers or secondary containment trays must be cleaned immediately.

Do not touch anything (phones, switches, splashshields, door knobs, nitrogen guns) with chemical laden gloves. Always check gloves thoroughly before touching anything. Rinse and dry gloves if any chemicals get on them. The gloves are there to protect your skin in case of an accident, NOT to make it OK to be sloppy while working with chemicals.

You should always use tweezers or other tools to take samples out of dangerous etchants, rather than your gloved hands.

Gloves may often have unnoticeable small holes or tears. To test a glove, you can blow nitrogen in it while submerging it in water and looking for bubbles.

To minimize the hazards, always work with the smallest quantities of chemicals necessary. When ordering chemicals always order the smallest amount necessary.

Before ordering chemicals always check with the lab supervisor first. Certain chemicals are too dangerous to use in this lab.

No toxic gases are allowed in the lab (Silane, Cyanide, Arsene, etc.)

The waste acid, base, and solvent cupsinks are intended for the disposal of small quantities of liquids. If you need to dispose of large quantities of waste, please discuss this with the lab supervisor.

The acid, base, and solvent cupsinks lead to 5 gallon carboys in cabinets behind the wet benches. When these carboys are full, an alarm will sound on the wetbenchs headcasing. Please notify the lab supervisor if the carboy is full, after silencing the alarm with the switch and leaving a note near the cupsink that the carboy is full.

The one gallon sulfuric and hydrogen peroxide mixture (piranha) dump provided is for small quantities of COOL liquid only. Do not pour hot/boiling sulfuric/peroxide into any container. Allow it ample time to cool down. Use a funnel, and be very careful to wipe up any drips from the neck of the bottle.

Wipers that may have small dribbles of acid on them must be rinsed and wrung out before disposal. Acid contaminated Q tips must also be rinsed before disposal.

In the Flexible Cleanroom: In the yellow room and in the two service chases on either side of the yellow room, there are safety showers and safety eyewash fountains. In the event of a chemical splash on your skin or eyes, immediately use the shower and/or eye wash fountain. Remove all contaminated clothing.

In the Nano Patterning Cleanroom: The safety shower and eye wash fountain is located through the one way door to 005 Spilker and just to the right. In the event of a chemical splash on your skin or eyes, immediately use the shower and/or eye wash fountain. Remove all contaminated clothing.

Use the eye wash fountain to flush chemicals from your eyes for at least 15 minutes, using your fingers to keep your eyelids open, then seek medical attention. Note, the safety showers and eye wash fountains pour onto the floor of the lab, so please don't "test" them or use them as drinking fountains.

There is HF burn cream available on top of the acid bench, which should be used for any suspected HF skin exposure, prior to receiving immediate medical help. There are also pH neutral eye wash solution bottles on the acid bench to rinse any suspected acids or bases out of eyes.

In the event of a fire or massive chemical spill, evacuate lab and call 9911 to let the Fire Department handle it. In a minor incident, seek the assistance of the Lab Supervisor.

Emergency and afterhours phone numbers are listed in the front of this manual and on plaques near every phone in the lab.

2.4 Safety Considerations

Users must understand the safety considerations of the equipment they are using. This means they know of the radiation, contamination, health, and fire hazards associated with what they are using, and operate in the lab in such a way as to minimize these hazards for themselves and others.

1. Users will know about the location of, and be briefed in the use of, safety showers, eye washes, fire extinguishers, etc.

2. Users will wear protective gear when handling and transporting hazardous materials.

3. Safety Data Sheets (SDS) are on file for all chemicals in the lab and are also widely available on the internet. Each user is responsible for familiarizing him/herself with the hazards of each chemical he/she uses.

4. Any new chemicals brought into the lab must be approved by the lab supervisor (in the Nano Patterning Cleanroom email: nano-snpcleanroom-staff@lists.stanford.edu). A new SDS for the chemical must be provided, and the chemical must be labeled properly. Certain chemicals may be deemed too hazardous, and will not be allowed in the lab. The quantity of all chemicals should be minimized.

5. All users will participate in all of the University and state mandated hazardous chemical and hazardous waste management training programs.

6. All users will follow the University, local, county and state guidelines, rules and regulations on chemical and hazardous waste labeling and storage. All users will understand the procedure for disposing of hazardous waste BEFORE generating it.

2.5 Appropriate Street Clothing and Shoes

You are required to wear clean room gowns over your street cloths. To be most comfortable, street clothing should be worn that is light weight, comfortable and allows for free movement.

Required street clothing:

1. Long pants (or the equivalent) that cover the legs and ankles.

2. Non-perforated closed-toed shoes that completely cover feet. Avoid shoes with sharp or pointed heels that could jam in the perforated floor in some regions of the Nano Patterning Cleanroom.

2.6 Eye Protection

In the Flexible Cleanroom: Users shall wear safety glasses with side shields at all times while working in the photolithography/chemistry room, and a full face-shield when working with or transporting any hazardous chemicals or materials anywhere in the facility. Safety glasses are located just inside the main entrance door into the lab.

In the Nano Patterning Cleanroom: Safety glasses are required at all times in the facility. Safety glasses must be of type B, C, D, G, or H (with side shields or offer side protection) and conform to ANSI standard (marked "Z87"). Safety glasses must be worn over all prescription glasses which are not safety glasses. Anyone wearing contact lenses must wear safety glasses. Standard safety glasses are designed to protect against flying fragments, but, not chemical splash hazards.

Full face shields must be worn in addition to the lab members safety glasses when handling hazardous chemicals or working at chemical wet benches.

2.7 Personal Protective Equipment

Complete Personal Protective Equipment (PPE) must be worn while using any wet bench or during the transportation of any chemical. See appendix D for required and recommended PPE when working at the wet benches in the Nano Patterning Cleanroom.

2.8 Buddy System

Safetyis a critical concern and we do not want users working in isolation. We are concerned about injuries being reported and responded to in a timely fashion. The following Buddy System is especially important when working late hours, weekends, and holidays, when there is likely nobody within ear-shot of you if have an emergency.

While working in any lab alone, use the following methods to decrease the response time to any injuries that might occur (in descending order of preference):

1. Have a lab "buddy" who is working in the cleanroom at the same time and is aware of your presence and wellbeing.

2. Have a friend within Spilker check on you periodically (to make sure youre not incapacitated). Have them walk by the windows every hour or so and look to see if youre OK.

3. Make sure a friend or family member is aware of your plan for working in the Cleanroom. Call, or text every couple of hours to let them know youre OK. Also, prepare them to call the Stanford Emergency Dispatch Office at: 650-329-2412 if you stop responding to calls or texts, or do not return from the lab after a reasonable time.

2.9 Special Health Concerns

Pregnancy: Lab members who are concerned should consult the EH &S website at: https://ehs.stanford.edu/topic/health-wellness/reproductive-and-developmental-health-protection

Pacemakers: Equipment in the lab may serve as sources of high voltage, ionizing radiation, ultrasonic interference or electromagnetic interference, which may affect normal operation of a pacemaker. If you have such a device, you should consult your physician before working in the lab.

3. Facility Hazards Overview3.1 Chemical Hazsards

The key to safe use of any chemical is the understanding the hazards presented by each specific chemical and knowing and using the appropriate precautionary measures to minimize these hazards. Knowing the main hazards and general rules for how to safely transport, pour, use, and dispose of these chemicals is every lab member's responsibility. Detailed hazard information is provided in the Safety Data Sheet (SDS) located in the entry to the lab and online.

3.2 Electrical Hazards

The danger of injury due to electrical shock is present in any electrical component. To prevent electrical exposure all equipment is interlocked and must have the protective covers in place while being used. If you feel the equipment is unsafe or a potential electrical hazard exists, stop using the tool and immediately notify the staff.

Notice: With the exception of personal electronics devices, any electrical equipment brought into the facility must have prior approval by the facility staff.

3.3 Other Hazards

Many tools in the lab use or generate high voltages, ultraviolet, or electromagnetic radiation. Safety interlocks are built into each tool, which prevent direct contact with high voltage sources or exposure to radiation sources during normal operation. However, no system is absolutely foolproof. It is absolutely essential that you, as a lab user, learn and are always aware of the potential hazards, follow the procedures for safe operation of each tool you are qualified to use, and refrain from using tools you are not qualified/trained to use.

1. Ultraviolet Radiation: UV exposure is a potential risk in mask aligners, UV sources, plasma etch, UV Ozone, and sputter tools, where highly energized species are generated. Avoid looking directly at a UV source and always wear protective glasses. Standard safety glasses are made from polycarbonate plastic which is highly absorbent of UV light (though they are not specifically designed for this).

2. Electromagnetic Radiation: Electromagnetic radiation may be generated by equipment using RF (primarily plasma etch and plasma deposition tools.) If you have a pacemaker, be aware that RF sources are present in the lab. All equipment is shielded to prevent exposure; report any damage to shielding on the equipment or cables.

4. Chemical Safety Information4.1 Manufacturers Chemical Labels

All chemical containers from the manufacture are required to have a label identifying the contents and containing the following precautionary information:

1. A signal word to define the hazard potential. These words include one of the following: Caution, Warning or Danger, in order of increasing potential hazard.

2. One or more Statements of Hazard, which describe in more detail the hazard presented.

3. Precautionary Measures.

4. First Aid or other information (this may not always be present on the label.)

4.2 Secondary Use Labels

Chemicals that have been dispensed for use or divided into secondary containers must have an updated label listing the following information.

1. Common Chemical Name (not an abbreviation or chemical formula)

2. Hazard Potential or Potentials (fill in the values of the NFPA hazard diamonds)

3. Name and email address of person creating the secondary container

4. Date when the secondary container was created

IMPROPERLY LABELED CHEMICALS ARE IN VIOLATION OF COUNTY ORDINANCES, AND SUBJECT TO CITATIONS.

4.3 Required Lab/Cleanroom Specific Labels

In addition to the labeling requirements above (which are mandated by state laws and county ordinances), certain facility or lab information is also required to help us with lab organization. All bottles of chemicals must be clearly labeled with the following information (if not included in the labels above):

1. The user's name (an individual's name not a group's name)

2. The name of the chemical, no abbreviations! (for example: Potassium Hydroxide, rather than KOH).

3. The date the chemical was brought into the lab.

4. The known hazards of the chemical (flammable, acid, toxic, etc.)

In the Nano Patterning Cleanroom: there are yellow facility tags on the yellow solvent cabinet which you need to fill out with the above information and place on all bottles of personal use chemicals.

AS A QUALIFIED LAB USER, IT IS YOUR RESPONSIBILITY TO HAVE ALL THE CHEMICALS IN USE AT YOUR STATION PROPERLY LABELED AS DEFINED ABOVE.

4.4 Safety Data Sheets (SDS)

Chemical manufacturers and distributors are required by federal law to provide Safety Data Sheets (SDS) for each product they sell. The Safety Data Sheet (SDS) contains information on general composition, physical and chemical properties, toxicology, and storage and handling recommendations. The SDS sheets for all the chemicals in the Flexible Cleanroom are located in a binder in the gowning room. In the Nano Patterning Cleanroom there is a binder in the gowning room for chemicals stored in the cleanroom area and another binder in 005 Spilker by the door for chemicals stored in that room. SDS information for many chemicals/chemical mixtures is available through the Stanford University Environmental Health and Safety group (EH&S) website at: http://www.stanford.edu/dept/EHS.

You are required to read the SDS information and Safe Operating Procedures for all the chemicals that you use in the lab. You are expected to know the main hazards, handling requirements, and disposal methods for all chemicals used by you in the facility.

5. Chemical Hazard Classes5.1 Liquid Chemical Hazard Categories

Liquid chemicals can be divided into different hazard categories with many chemicals falling into more than one hazardous class. It is your responsibility to recognize the chemical hazards of all the chemicals you are using and understand the appropriate precautionary measures required for safe use.

The following are typical safety measures for handling any liquid chemical:

1. Knowledge of the main hazards.

2. Use of required personal protective equipment (PPE).

3. Working only in an approved exhausted bench.

4. Knowledge of the approved disposal method.

5.1.1 Solvents

Most solvents are flammable chemicals with low flash points that attack plastics and polymers. At sufficiently high vapor concentrations, they can be easily ignited at room temperature and pose a significant fire hazard. Great care is required when using solvents near ignitions sources such as hot plates or any electrical systems. Solvents may ignite or explode when brought into contact with chemical oxidizers, such as acids. Prolonged exposure to solvents can cause tissue and organ damage. Solvents must be double contained and stored in the designated flammables cabinet. Solvents may be used only in designated solvent hoods (with the exception of isopropyl alcohol).

Solvents Supplied by the Flexible Cleanroom:

1. Acetone Strong solvent used for minor degreasing and dissolving photoresist. Dissolves or crazes acrylic (Plexiglass) and polycarbonate (Lexan).

2. Isopropyl Alcohol Weaker solvent, general cleaning and wiping. Displaces water. Harmless to most plastics. Good for cleaning oxide off of rubber.

3. Methyl Alcohol Removes many inks and dyes. Good cleaner. Displaces water, low viscosity, dries fast.

4. Ensolv/Lexol (npropyl bromide with a stabilizer package) Powerful degreaser solvent, behaves very similar to 111 Trichloroethane. Attacks many plastics such as acrylic, styrene, and polycarbonate. Dissolves waxes and greases, non watersoluble, nonflammable, fast drying.

5. Cyclohexanone Dissolves waxes and greases, very slow drying, non water soluble, flammable. Strong odor.

6. Shipley 1165 Remover (NMP or n-methyl-pyrrolidone) Must be disposed of separately as HAZARDOUS WASTE

Solvents Supplied by the Nano Patterning Cleanroom:

1. Acetone Strong solvent used for minor degreasing and dissolving photoresist. Dissolves or crazes acrylic (Plexiglass) and polycarbonate (Lexan). Rinse with alcohol to leave a clean surface.

2. Isopropyl Alcohol or 2-propanol Weaker solvent, used for general cleaning and wiping. Displaces water -leaves clean surface. Harmless to most plastics. Good for cleaning oxide off of rubber.

3. Methyl Alcohol Removes many inks and dyes. Good cleaner. Displaces water, low viscosity, dries fast leaves a clean surface.

4. Remover PG (NMP or n-methyl-pyrrolidone)- strong solvent used for dissolving and removing photoresist.

5. Anisole- common solvent for dilution of e-beam resist.

6. Xylenes- solvent used in developing ZEP 520 or CSAR 62 resists

7. Methyl isobutyl ketone (MIKB)- solvent used in developing PMMA resists.

5.1.2 Corrosives

Corrosives include bases and acids. A corrosive (or "caustic") chemical destroys or permanently damage living tissue such as skin and underlying tissues resulting from an exposure. Splashes in the eyes can cause blindness and inhalation of vapors can destroy lung tissue.

Acids Supplied by the Flexible and Nano Patterning Cleanroom:

1. Acetic Acid Considered flammable, stored in solvent cabinet. Used in several etchant recipes.

2. Hydrochloric Acid Strong acid, used to etch metals alone or mixed with other acids. HCl and Nitric makes "Aqua Regia", which etches gold.

3. Hydrofluoric Acid Strong acid. Very dangerous. Used to etch glass, and silicon dioxide. Eats titanium like crazy.

4. Phosphoric Acid Used to etch iron oxide, and is an ingredient of many etch recipes.

5. Nitric Acid Strong acid, etches metals, eats cellulose, strong oxidizer, extremely dangerous if mixed with many organic materials.

6. Buffered HF Hydrofluoric acid buffered with ammonium bifluoride. Used to etch oxide on silicon and gallium arsenide wafers. Comes in 6:1, 20:1, and 50:1 ratios to allow controlled etch rates of SiO2. Also commonly called buffered oxide etch or BOE. 6:1 BOE etches Si02 at around 1000 Angstroms per minute at room temp.

Bases Supplied by the Flexible and Nano Patterning Cleanroom:

1. Ammonium Hydroxide Used in various etch formulas.

2. Sodium Hydroxide Lye, strong base, eats aluminum.

3. MF-319 Developer 2% TMAH solution + a surfactant -general purpose positive resist developer, used as is.

4. 25% TMAH (tetramethylammonium hydroxide) dangerous base used in developing HSQ resists.

5. Mirco (Brand) Detergent High quality concentrated detergent. Mixed with water to make an excellent cleaner for glass and stainless steel. Etches aluminum slightly, stains copper and brass slightly.

5.1.3 Oxidizers

An oxidizer is any substance which will react chemically either by supplying oxygen or removing electrons. Oxidizers must not be stored near flammable or reactive materials. Oxidizers should not be stored or mixed with solvents. When oxidizers are mixed with compounds that can act as reducing agents, the result is often a violent reaction and possibly an explosion.

Common Oxidizers:

1. Hydrogen Peroxide Strong oxidizer, used in cleaning and etching mixes.

2. Nitric Acid Strong acid, etches metals, eats cellulose, strong oxidizer, extremely dangerous if mixed with many organic materials.

5.1.4 Water Reactive Chemicals

A water reactive substance spontaneously undergoes a chemical reaction when in contact with water, very quickly generating heat and/or gas upon mixing. Water reactive mixtures should never be poured directly into a sink drain.

Common Water Reactives: Concentrated sulfuric acid and piranha

5.1.5 Flammables

Vapors from a flammable liquid can ignite and explode above a critical concentration called the flash point and in the presence of ignition source. To minimize hazards, always work well within the exhausted area of the appropriate bench and minimize the quantities of flammables in use.

Common Flammables: acetone, isopropanol, methanol, xylenes, n-methyl-2-pyrrolidone (NMP) and methyl isobutyl ketone (MIKB).

WARNING: HEATING OF ACETONE ON LAB HOT PLATES IS NOT ALLOWED IN EITHER FACILITY. ACETONE HAS A LOW IGNITION TEMPERATURE AND THE LIKELY HOOD OF IGNITION AND EXPLOSION IS HIGH.

5.1.6 Toxic/Poison

A toxic material is one which has poisonous or harmful effects. All materials can be toxic depending on the level of exposure. There are formal, quantifiable definitions as to what comprises a toxic material and to what degree it is toxic based on lethal dosages for lab animals when administered orally or through inhalation. Materials with moderate to extreme toxicity are not allowed in the facility.

Common Toxics: hydrofluoric acid, tetramethylammonium hydroxide (TMAH), xylenes, and methyl isobutyl ketone (MIKB).

5.1.7 Non-toxic

A non-toxic material is one that is not likely to result in harmful effects with normal use.

Common Non-ToxicS:

Deionized Water Plumbed throughout the lab, 18 Megohm purity, filtered to 0.2 microns, sterilized by U.V. lamp.

Detergents - while they are skin and eye irritants, they are generally considered non-toxic.

5.2 Resists and Other Chemicals

Resists are typically polymer materials (with the exception of HSQ) that come dissolved in a solvent. Most of the danger associated with resist is due to the carrier solvent and its specific hazards. Once resists have been baked-out and the solvent desorbed they are generally considered safe, but one should always consult the SDS for each specific resist prior to use.

Resist Chemicals supplied by the Flexible Cleanroom

1. Shipley 1813 Positive Photoresist. 1813 is medium viscosity, spins out to 1.3 microns at 4,000 rpm.

2. Shipley 1805 Positive Photoresist. 1805 is very thin, spins out to 5000 Angstroms at 4,000 rpm.

3. Hexamethyldisilazane (HMDS) Shipley (common) Adhesion Promoter used with resists.

Resist Chemicals supplied by the Nano Patterning Cleanroom

1. PMMA (polymethyl methacrylate) is a popular e-beam resist. The PMMA polymer is dissolved the solvent Anisole. Exposure causes scission of the polymer chains acting as a positive tone resist.

2. CSAR 62 (replaces ZEP 520 A) are common positive tone e-beam resists with better durability than PMMA. They both come dissolved in Anisole at various concentrations and survive longer in SEM inspections and plasma etching conditions than the more common PMMA.

3. ma-N is a common negative tone resist dissolved in a combination of cyclopentanone and anisole.

4. HSQ (not supplied by the Nano Pattering Cleanroom) is an e-beam resist comprised of hydrogen silsesquioxane (HSQ) resin in a carrier solvent of methyl isobutyl ketone (MIBK). HSQ functions as a negative tone electron-beam resist. The HSQ monomer formula is H8Si8O12 and is cross-linked by exposure to e-beam radiation.

5.2.1 Other Chemicals in the Flexible Cleanroom

Consult the safety data sheets (SDS) or Safe Operating Procedures for more information about their hazard class and safe use.

1. Gold Etch Fast gold etch, made from Iodine, Potassium Iodide, and water. (also available in the Nano Patterning Cleanroom)

2. Chromium Etchant Type 1020 made by Transene.

3. Ceric Sulfate Used in mixing up chromium etchant.

4. Iodine Used to mix up gold etch.

5. Potassium Iodide Also used to mix up gold etch.

5.3 Miscellaneous Materials

Gallium Arsenide (GaAs) and its by-products are extremely toxic. Anyone working with GaAs must be constantly aware of how arsenic might be generated during processing. Physical contact with GaAs and anything that comes into direct contact with GaAs must be avoided. Scribing and cleaving GaAs samples must be done in an exhausted hood. All work surfaces must be wiped down afterwards to prevent the spreading of GaAs dust.

All GaAs waste, no matter how small, is considered hazardous. This includes GaAs-contaminated lab wipes. Place all of the GaAs waste in a sealed zip-lock plastic bag and place it in the Solid GaAs Waste can.

Compressed Gases: There are extreme hazards presented in working with pressurized gas cylinders. Only trained and qualified staff may install, disconnect, or change out gas cylinders.

Non-Toxic Gases: Non-toxic gases do not generally pose an immediate risk to health and safety. However, they can be asphyxiants and may pose health risks at high concentrations or with long-term exposure. House nitrogen (N2) is plumbed throughout the lab for the equipment and for general use. The nitrogen supply is at high pressure which can pose a hazard.

Toxic Gases: The Spilker Building is not rated for toxic gases, so no toxic gases are stored in either facility.

Nano Structured Materials: Being a part of the Stanford Nano Shared Facilities is reasonable to assume a fair number of Nano Structured Materials will make their home in the cleanrooms. Exposure to nanomaterials may occur through inhalation, dermal contact, or ingestion depending on how personnel use and handle them. The full health effects of exposures to nanomaterials are not fully understood at this time. For example, a peer-reviewed toxicity study on carbon nanotubes (CNTs) indicated that the toxicity of nanoparticles depends on specific physiochemical and environmental factors and thus the toxic potential of each nanoparticle needs to be evaluated separately. Results of existing studies in animals or humans provide some basis for preliminary estimates of areas of concern.

Required Personal Protective Equipment for working with Nano Structured Materials:

For non-destructive handling of solid nanoparticle composites or nanoparticles permanently bonded to a substrate.

Disposable nitrile or PVC gloves. Do not reuse gloves.

Wet cleaning procedures and/or HEPA vacuum for surfaces/equipment.

For nanomaterials in liquid media, nanostructured powders, or cleaving or breaking substrates with nanoparticle fixed to the surface

Conduct task within a fume hood

Add a second layer of disposable nitrile or PVC gloves. Do not reuse gloves.

Use a face shield if splash potential exists from liquid

6. Chemical Storage

6.1 Background

To prevent accidental mixing of incompatible materials, every chemical in the lab must be stored in the designated area appropriate for its hazard class. Each storage area is designed for safe storage of chemicals of a particular set of hazard classes (i.e., they are appropriately ventilated, chemically resistant, and built against the main physical hazards presented by the chemicals to be stored there.) Thus, it is a safety imperative that all chemicals in the lab be stored appropriately in one of these designated storage areas. No chemicals may be kept in personal storage areas.

By law, we are required to maintain an up-to-date list and amounts of all hazardous chemicals and materials in the entire facility. Violations and inaccurate chemical inventory control can result in the closure of the facility.

6.1.1 Flammables

Flammable chemicals, mostly solvents, are to be stored in flammable liquids cabinets or under the stainless steel wet benches. Exceptions are the small solvent squeeze bottles, which are located in secondary containment troughs in the solvent and spinner benches. Acetic acid is stored in a flammable liquids cabinet because it is considered a flammable liquid. Nonflammable solvents and organics may be stored in the secondary containment drawers under the solvent and spinner benches.

6.1.2 Corrosives

The acids and bases are stored in secondary containment drawers underneath the white corrosion resistant plastic acid and base wet benches. Keep acids under the acid bench and bases under the base bench. Make sure chemicals sharing a compartment are compatible with each other. See the lab supervisor if you have questions or if you arent completely sure about where to properly store something.

6.1.3 Oxidizers

In the Nano Patterning Cleanroom oxidizers are stored under the left side of the acid wet bench and in the Oxidizer cabinet under the fumehood in 005 Spilker.

Additional information on chemical storage can be found here:

http://www.stanford.edu/dept/EHS/prod/researchlab/lab/storage_group.html

MSDS (material safety data sheet) information can be found here:

http://www.stanford.edu/dept/EHS/prod/MSDS/index.html

The designated chemical storage areas in the Nano Patterning Cleanroom are:

Location

General Hazard Class

Chemical Type

Processing Use

Solvent Bench

Flammable, toxic

Solvents

Cleaning, developer, resist removers

Spinner Bench

Flammable

Solvents

e-beam resists

Acid Bench right side

Corrosive

Acids

Cleaning, etching

Acid Bench left side

Oxidizer

Oxidizers

Cleaning, etching

Refrigerator

Flammable

Solvents

e-beam resists

Base Bench

Corrosive

Base

Resist developers

6.2 General Use Chemicals

We supply a number of chemicals that are commonly used in semiconductor processing (the Flexible Cleanroom) and e-beam writing processes (the Nano Patterning Cleanroom). Containers that are already opened should be used first. Notify staff when chemicals are running low. For the Nano Patterning Cleanroom a full list of these chemicals, required PPE, disposal, engineering controls, and appropriate Safe Operating Procedures is listed in Appendix B.

In the Nano Patterning Cleanroom: Our facility, including our safety equipment, personal protective equipment (PPE), and even staff expertise is focused on chemicals that support the Nano Patterning Process. For chemicals that substantially deviate from this mission, we may refer users to other labs that are better equipped to handle their chemicals safely.

Prior to using a chemical in the Nano Patterning Cleanroom you must first:

1. Review and understand the Safe Operating Procedures (SOPs) for that chemical or class of chemicals either on-line or in the binder in 006 H

2. Sign off (either in the binder or on-line) that you have read and understood the SOPs for that chemical.

6.3 Introducing New Chemicals

New chemicals are not to be stored or used in the facility without prior approval of the facility staff.

1. In the Flexible Cleanroom, contact Tom Carver to receive approval before using/storing any new chemicals. An SDS (Safety Data Sheet) must be provided prior to approval. If approved, a plan will be developed for using and storing chemicals safely. It is advised that you do not purchase any chemicals before receiving approval. There are, in rare cases, chemicals that are deemed too hazardous to be used in this facility, so alternatives may need to be discussed.

2. In the Nano Patterning Cleanroom email the staff (nano-snpcleanroom-staff@lists.stanford.edu) the following information and wait until approval has been granted before bringing the chemical into the lab:

a. A Safety Data Sheet (SDS)

b. Prepare a Safe Operating Procedure (SOP) document for your desired process. Carefully detail:

i. The hazard(s)

ii. Required Personal Protective Equipment

iii. Special Handling Procedures for working with the chemical(s)

iv. Safe Disposal Methods.

WARNING: UNAPPROVED CHEMICALS FOUND IN THE LAB ARE SUBJECT TO DISPOSAL WITHOUT NOTICE.

6.4 Personal Chemical Storage

Chemical storage space is limited in the labs. Large personal or group use bottles of chemicals already provided by the facility are not allowed. In the Nano Patterning Cleanroom an exception is made for small bottles of resist and the like which do not take up as much storage space. Storage of personal containers of chemicals or materials already approved by facility staff must comply with the following restrictions:

1. The container must either have a Manufacturers Label or a Secondary Use Label containing all the information listed in section 4.2.

2. The container must be stored in the appropriate hazard class storage area (wet bench or chemical cabinet)

3. In the Nano Patterning Cleanroom: Personal containers, even if they have the original manufacturers label, must have a yellow NPC label completed.

4. From time to time we review the chemical inventory and may purge old chemicals.

7. Chemical Handling

7.1 Personal Protective Equipment

Protective gear is required whenever handling or transporting chemicals within the facility. The degree of protective gear depends on the usage of the chemical. The table below is a guideline as to the level of personal protective equipment required for various chemical types. A more complete list is found in Appendix B.

Chemical Type

Recommended personal protective equipment

Corrosives or oxidizers

face shield, apron, chemically-resistant gloves

Solvents

face shield, chemically-resistant gloves

Photoresist

vinyl gloves over nitrile or latex gloves

7.2 Safe Operating Procedures

You must abide by the following safety procedures when using chemicals in the labs:

1. Follow Safe Operating Procedures (SOP) for the process/chemicals you are using.

2. In the Nano Patterning Cleanroom:

1. SOPs for common lab supplied chemicals are found in a binder in the wet bench room

2. Leave a Chemical-In-Use tag before stepping away from your work.

3. Use the required PPE for the chemicals you are using.

4. Keep the chemicals contained within the appropriate lab bench (engineering controls)

5. The work surface must be clean and dry when you have completed your work.

6. When you return chemicals, the bottles must be clean and dry.

7.3. Chemical Exposure

In case of a localized external exposure:

1. Promptly flush the affected area with water, for at least 15 minutes.

2. For larger area external exposure, use a safety shower.

3. Remove your clothing while under the shower and flush for at least 15 minutes.

Exposure of corrosives to the eyes is extremely serious;

1. Flush immediately, either with the water spray gun at the wet bench or preferably the eyewash station.

2. Eyes should be rolled up and down, and side to side, continuously, to allow clean water to flush behind the eyeball.

For any exposure to corrosives, you should be taken to the emergency center for evaluation and treatment.

All chemical exposures must be reported to the staff. For any significant exposure, the lab member should be taken to the emergency center for evaluation and treatment. See section 10 for medical treatment.

7.4 Transporting Chemicals to/in the Lab

When transporting chemicals to/in the lab use the following PPE:

1. Chemical resistant gloves

2. Safety Glasses

3. A chemical transport bucket/container to provide secondary containment

7.5 Chemical/Hazardous Waste Collection and Disposal

Disposing of chemical waste in a safe manner is every lab users responsibility. Improper disposal of waste could result in explosion and injury. Violations of proper waste disposal laws may even result in shutdown of the facility. Any chemical waste generated by the lab must be labeled properly. The label on a container of hazardous waste must say:

1. "HAZARDOUS WASTE"

2. The name of the chemical(s) along with approximate percentages. The name must not be abbreviated (For example: Hydrochloric Acid 10 %, Water 90 % rather than 10% HCl in H2O)

3. The name of the person that generated the waste. One person, not a group's name.

4. List the hazards of the chemical (flammable, toxic, corrosive)

5. The date that the waste STARTED accumulating.

6. The physical state of the chemical (liquid, solid, sludge etc.) even if it's obvious!

Hazardous chemical waste must not be allowed to accumulate for periods longer than 9 months to do so is punishable by instant fines assessed by the county inspector.

No chemicals can be disposed of down the sinks. The lab sinks drain to a sewage treatment plant not a chemical neutralization tank.

The labs provides convenient forms which when filled out completely, meet the legal labeling requirements for hazardous waste. The forms MUST BE FILLED OUT COMPLETELY.

The University provides a pickup service for Hazardous Waste that has been properly labeled. There are specific areas for the accumulation of hazardous waste while it waits to be picked up by Health & Safety. See the lab supervisor if you don't know where to store hazardous waste. Improperly labeled waste will not be picked up. Hazardous waste must be placed in secondary containment trays and be separated from incompatible chemicals.

See the lab supervisor before generating any hazardous waste. Certain chemicals require specialized containers for safe storage and handling. Some containers may need to be vented to prevent accumulation of pressure or explosive gases.

For your convenience, the lab provides an acid waste cupsink, a waste cupsink for mixtures containing hydrofluoric acid, a base waste cupsink, a solvent cupsink, and a special bottle for the collection of waste sulfuric acid and peroxide mixtures (Piranha).

The acid cup-sinks are only for disposing of small quantities of the acids which the lab supplies.

The base cup-sink is only for bases.

The solvent cupsinks are only for the disposal of small quantities of labsupplied solvents. Do not add anything other than labsupplied solvents to the solvent cupsinks!

There is a bottle with a vented cap in the acid sinks for disposal of sulfuric acid and peroxide wastes (Piranha).

It is the responsibility of the users to dispose of other chemicals and large quantities of chemicals themselves. See the lab supervisor for help with disposing of chemicals.

In the Flexible Cleanroom:

Empty bottles of acids or bases are to be rinsed thoroughly and disposed of in the trash. Bottles should be emptied "to the last drop".

Empty bottles of solvent are to be drained completely (to the last drop) and then disposed of in the trash or saved to use as hazardous waste containers. Leave the lids loose so any remaining solvent can evaporate.

Solventsoaked wipers, if still wet when through using, should also be bagged in ziplock baggies and placed in the yellow bin. However, if the wipers are completely dry when through (no perceptible odor), then they can be disposed of in the wastebasket as ordinary trash.

Photoresistsoaked wipers and foil are considered hazardous waste, and should be accumulated and disposed of as hazardous waste by bagging in ziplock baggies, and be accumulated and disposed of as hazardous waste by bagging in ziplock baggies, and placing in the yellow bin in the lab. Please squeeze all of the air out of the baggies and make sure the baggie is sealed airtight.

Broken glass should be carefully picked up and put into the green Sharps container, which is located on the bench just outside of the yellow room.

In the Nano Patterning Cleanroom:

Bottles should be emptied "to the last drop" and placed in the fumehood in 005 Spilker. Put a plastic bag around empty containers of strong acids or based

Wipers or Qtips, which may have small dribbles of acid or base, are to be rinsed thoroughly with water and placed in a zip-lock bag, sealed, labeled and left in the back of their respective hood.

Photoresist contaminated wipers and foil are considered hazardous waste, and should be accumulated and disposed of as hazardous waste by bagging in ziplock baggies, and placing in the yellow can in the lab. Please squeeze all of the air out of the baggies and make sure the baggie is sealed airtight.

Solvent contaminated wipers and Q-tips should also be bagged in ziplock baggies and placed in the yellow can.

Broken glass should be carefully picked up and put into the red Sharps container, which is located on the bench outside the Nova SEM room (Note: there is a separate container for GaAs waste)

Hazardous waste tags are available in room 005 Spilker or on top of the yellow flammables cabinet in the wet bench room.

How to Change Local Waste Containers

Please follow the following steps when changing a waste container

1. Obtain an empty waste container.

2. Fill out and adhere the Hazardous Waste Tag to the container

3. Cap the old, filled container, making sure that the outside of the container is clean and dry and make sure the hazardous waste label is legible and securely attached.

4. In the Nano Patterning Cleanroom: transport the old, filled waste container to the fume hood in 005 Spilker or the appropriate chemical cabinet in 005 Spilker.

Do not Attempt to change on of the 5 gallon carboys. Notify lab staff for them to change.

7.6 Solid Hazardous Waste Disposal

Solvent/resist contaminated objects are considered solid hazardous waste. These include gloves, lab wipes, swabs, plastic syringes, and syringe filters. Hazardous waste items must be placed in the hazardous waste cans and not in the standard garbage cans. At times these items can give off gas vapors. If any items are emitting an odor, they must be placed in a fully sealed zip-lock bag before being placed in the yellow hazardous waste can.

Sharps: Objects which can cut or puncture the skin are also considered hazardous. These sharps include items such as broken wafers, razor blades, broken glass, razor blades/exacto knives/scalpels, or hypodermic needles.

In the Nano Patterning Cleanroom:

Pipets or anything that is hard and can puncture a plastic bag and is contaminated with resist or solvent residue must be places in the red sharps container located in the spinner bench.

Other sharp objects should be placed in the red sharps container outside the SEM room.

Gallium Arsenide pieces can be disposed of in a red sharps container immediately outside the Nova SEM room.

WARNING: Any lab member failing to strictly adhering to the waste disposal rules, either intentionally or unintentionally will be subject to administrative action and this may result in a loss of lab privileges.

7.7 Chemical Spills

In the event of a minor spill or release that can be cleaned up by local personnel using readily available equipment (absorbent, available from EH&S in Small Spill Kit):

Notify personnel in the area and restrict access. Eliminate all sources of ignition.

Review the SDS (located near the lab entrance) for the spilled material, or use your knowledge of the hazards of the material to determine the appropriate level of protection.

Wear gloves and protective eyewear. Clean up using absorbent. Put the contaminated absorbent in a labeled hazardous waste container.

If greater than 30 ml, or if it will take longer than 15 minutes for you to clean-up, immediately call EH&S at 725-9999 to report the spill, and then notify lab staff.

In the Nano Patterning Cleanroom: Place the waste container in the fumehood in 005 Spilker

Submit on-linewaste pickup requestto EH&S or notify lab staff.

Chemical spills that occur outside the ventilated area of a chemical wet bench can pose inhalation and contact hazards. Unless you are trained and specifically instructed by a staff member who has evaluated the situation, DO NOT attempts to clean up the spill yourself.

In the event of a spill or release, which may or has impacted the environment (storm drain, soil, air outside the building), or spill or release that cannot be cleaned up by local personnel:

1. Notify Stanford Responders: Call 725-9999

2. Notify Lab Staff

8. Emergency Information

8.1 Emergency Equipment

In the Flexible Cleanroom

The location of the safety equipment in the lab will be shown to all new lab users.

1. There are fire extinguishers located in room 131 (the gowning room), on the back wall near 131G, and in 128A (lab supervisors workroom)

2. There are safety showers and eye wash fountains in room 131C (the yellow room) and in 131B and 131D (the two service chases on both sides of 131C). The area in front of the safety showers should never be blocked for any reason.

3. Above the acid bench there is a bottle of pH neutral eye wash and a tube of HF burn cream (calcium gluconate).

4. Above the acid and base cabinets are spill kits, although all large spills should be handled by EH&S, or the fire department.

5. There are phones located in rooms 131A, 131C, and 131G (see appendix C).

6. There are First Aid kits located in the gowning room (131), as well as in room 128A.

In the Nano Patterning Cleanroom

The location of the safety equipment in the lab will be shown to all new lab users during the lab safety tour.

1. There are fire extinguishers located in room 006 (the gowning room), and in 005 Spilker (the room on the side of the main cleanroom).

2. There are safety showers and eye wash fountains in room 005. The area in front of the safety showers should never be blocked for any reason.

3. Above the base and solvent bench there are bottles of pH neutral eye wash.

4. Above the acid bench is at least one tube of HF burn cream (calcium gluconate).

5. There are spill kits on the wire shelving rack in 006H (the wet bench room), although all large spills should be handled by EH&S, or the fire department.

6. There are red emergency phones connecting to Stanford Emergency Operation located in 006E and 005 Spilker

7. There are regular lab phones located in rooms 006E (at the JEOL computer station), 006A (at the CAD station), and 006G next to the Nova SEM (see Appendix D).

8.2 Emergency Exit Information

In the Flexible Cleanroom

There are many emergency exits throughout the lab. Besides exiting through the gowning room, you can exit through any of the pushtoopen double glass doors, or through service chases. In a real emergency such as a large chemical spill, fire, or after an earthquake, dont worry about cleanroom protocol, just GET OUT through the nearest exit. The Emergency Assembly Point is located in the front courtyard of the Nano Building (106, SEQ). As soon as practical after an accident, please notify Tom Carver (carver@stanford.edu) so that the required documentation can be provided to EH&S regarding the accident. Notify Tom Carver if any emergency supplies are used up so that they can be replaced.

In the Nano Patterning Cleanroom

There are several emergency exits from the lab, but your first choice should be the double doors that open from 006A into the hallway (these are to the left as one enters from the gowning room). In a real emergency such as a large chemical spill, fire, or earthquake, dont worry about cleanroom protocol, just GET OUT through the nearest

exit. The Emergency Assembly Point is located in the front courtyard of the Nano Building (106, SEQ). As soon as practical after an accident, please notify lab staff at (nano-snpcleanroom-staff@lists.stanford.edu) so that the required documentation can be provided to EH&S regarding the accident. Notify Cliff Knollenberg at (cknollen@stanford.edu) if any emergency supplies are used up so that they can be replaced.

8.3 General Emergency Response

In the event of an imminent or actual health-threatening emergency (threatening local or public health, safety, or welfare; or the environment outside the immediate area):

1. CALL 9-911 for the Fire Department or In the Nano Patterning Cleanroom pick up a red emergency phone to speak directly with Stanford Emergency Operations.

2. Alert people in the vicinity, activate local alarm systems.

In the Nano Patterning Cleanroom the fire alarm pull station is too the left of the Emergency Exit

3. REMAIN NEARBY TO ADVISE EMERGENCY RESPONDERS.

4. Once personal safety