Nano-Scale Science And

March 2004

Center For

Nano-scale Science And

Engineering

University of Kentucky

Safety Manual

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Table of Contents

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General Facility Use 1

Important Phone Numbers 2

CeNSE Wet Cleaning Bench Operating Procedure2

Furnace Use 2

Non-Standard Procedures 3

Cleanroom Garment Policy 4

Waste Disposal 4

Emergencies 5

Chemicals 6

Compressed Gasses 7

Fire Hazards 7

Electrical Safety8

Lab Etiquette 8

Agreement to Follow CeNSE Safety Procedures 9

Appendix A: Non-Standard Request Form 10

Appendix B: Sample MSDS 13

Appendix C: Cleanroom Attire 17

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Center for Nano-scale Science and Engineering Safety Rules

General Facility Use

Researchers must be trained on each instrument that is used. This training is done with Brian Wajdyk (, 257-6401).

Sign up is first come first serve. A calendar can be found at every instrument. Each user is required to sign his/her name, professor’s name and phone number. Instructors wishing to use the facility for course instruction must schedule at least a week in advance. The director, under special circumstances, may assign priority to special projects, weighing the needs of student progress.

The log must be filled out for every station (especially the chemical cleaning hood) to have a record of users and chemical systems.

Brian Wajdyk/Vijay Singh have the authority to immediately suspend privileges of any user who performs unsafe experiments and/or violates safety regulations. The door key code will be cancelled and unescorted entrance into facilities will be treated as trespassing and campus police will be notified. Access will be reinstated only after the majority of core professors vote to do so after agreeing on appropriate corrective actions such as a thorough safety report or ‘fabrication community’ service. This process will take several weeks and will interfere with student progress; thus following procedures is critical. Protest of suspension can be taken directly to Prof. Vijay Singh, who, as director, has final authority in all matters. Professor Singh has a strong commitment to safety and will not take this matter lightly.

Faculty member and others wishing to use the CeNSE facilities are responsible for providing the special accessories needed for their experiments. For example, the CeNSE will not provide process gases, deposition materials, substrates or non-standard cleaning chemicals.

The user must follow all University of Kentucky safety regulations and must provide MSDS paperwork for all chemicals and gases brought into the facility. Working alone with chemicals, furnaces and CVD equipment is forbidden. If a co-worker momentarily steps out of room then the door should remain open to allow prompt aid in event of mishap.

Users must use appropriate safety wear. If performing non-standard procedure you must provide your own safety wear. All gas cylinders must be securely fastened!! If researcher is bringing in a new cylinder, they must provide appropriate safety restraints and consult Mr. Spiggle.

The user is responsible for cleaning the equipment that he/she uses. If you are unsure of the operation of a piece of equipment, PLEASE ASK FOR HELP.

For further information or questions, please contact: Brian Wajdyk, , 257-6401. A schedule of lab hours for all personnel is posted.

Important Phone Numbers

Brian Wajdyk…………………………… 257-6401

University Police…………………………...257-1616

Electrical and Computer Engr. Office……...257-8042

ON THE UNIVERSITY OF KENTUCKY CAMPUS CALL 911 FOR POLICE, FIRE, OR MEDICAL EMERGENCIES.

CENSE Wet Cleaning Bench Operating Procedure

Failure to follow procedures can and will result in contamination that will ruin your experiment and ruin the experiments of everybody after you. Privileges to use the facility will be revoked if procedures are not followed precisely. Failure to follow correct safety procedures will result in loss of use privileges.

All equipment use, including the cleaning bench, must be logged.

The bench and glassware must be cleaned to original state after use.

No Glassware or chemicals shall be left on the bench after use, period.

Furnace Use

General: The furnace is one of the most important equipment in a fabrication facility as it is used to form gate oxides and dope materials to be chemically active. The furnace is very easily poisoned by impurities. Impurities dissolve into the glass and later release to ruin every sample after initial contamination (students thesis’ become ruined). Your peers and friends demand that all rules are followed. There are 3 critical rules:

1. Never put anything that has not been thoroughly cleaned into the furnace. The impurities will diffuse into the glass! The only way to know if a tube is ruined is for several students to fail at their experiment for months and deduce it was a contamination. People who don’t follow procedures will be rightfully scorned and facility privileges revoked.
2. Never exchange parts of one furnace (i.e. sample holder) to put in another. Impurities (i.e. dopants from one furnace can ruin the other. Keep all items in their labeled positions.
3. Never touch a furnace with your bare hands. The Na/Ca/etc. will diffuse in the quartz and ruin the tube.

There are 4 general types of furnaces:

1. Oxidation: This is the cleanest furnace and can only be used to oxidize Si.
2. Phosporus doping: This furnace can only be used to dope selected materials N-type conductors.
3. Boron doping: This furnace can only be used to dope selected materials P-type conductors.
4. General annealing: This furnace will be relatively dirty since a large variety of samples will go through it.

All proposed experiments outside of standard procedure must be approved before using in this tube. This is necessary to keep the tube functional. Researchers are welcome to provide their own quartz tubes to use in the furnace for specific needs. New tubes and fittings cost about $2,000. Room 369 has general use furnace recommended for ‘dirty’ process.

Safety: Dangerously hot quartz looks like cold quartz!! Never grab/touch quartz withoutknowing how long it has been out of the furnace or feeling radiant heat from a safe distance.Explosive gasses such as H2 must be safely diluted. H2and O2cannot share the same feed line.

Procedures:

Perform appropriate RCA/Piranha clean before placing samples in furnace!

Set furnace to operating temperature.

Set gas flows to desired conditions.

Slide sample in with quartz rod ensuring that rod only goes in storage tube or furnace.

Wear gloves!!

Don’t mix-up parts!!

After elapsed time, slide sample to edge of tube with quartz rod.

Let sample cool for 10 minutes with end cap in place.

When sample is cool remove plate/sample from furnace and replace end cap.

Turn off heater.

It is important that a small amount of gas flow while furnace is cooling, this is because as the furnace cools, air inside contracts drawing in air with dust. Over a short time this dust will contaminate the tube.

Never, never, never touch quartz tube with bare hands (no gloves). The Na from your hands will contaminate the tube.

Non-standard Procedures

To insure that the facility does not become contaminated, all non-standard procedures must be approved by Dr. Singh, Chen, Hinds or Mr. Spiggle.

Standard procedures that require no special approval (aside from required training) are:

RCA1, RCA2, Piranha cleans

Organic/resist strip with Acetone

HF etch

Oxidation, doping, diffusion, and H2/D2 passivation anneals

Photolithography

E-beam evaporation of Al, Au, SiO2, Al2O3

Sputtering with commercially purchased target

Thermal evaporation of Al, Au, Cu

Liftoff, metal etching

An experiment plan must be written for non-standard experiments. This plan must be approved. Verbal confirmation with an advisor is not acceptable, experiment plan must be written and on file with Mr. Spiggle. (This may seem like an inconvenience, but if you are at all a good scientist/engineer you would write this down anyways. 1 page + MSDS’s is sufficient in most cases). Performing non-standard procedures without approval will result in suspension of privileges. Items that must be included in discussion are:

Materials used

Materials Safety Data Sheets (MSDS can be conveniently found at

Safety hazards and precautions taken

Equipment to use

Contamination possibilities, minimization, and cleaning

Waste disposal

See appendix A for an example of a non-standard procedure request form.

Cleanroom Garment Policy

Cleanroom garments (suit, shoe covers, hairnet, and gloves) must be worn at all times while inside cleanroom area.

Suits will be available for shared use and disposed of by facility manager after useful lifetime. Please reuse shoe covers that are stored at the bottom of the cabinet. Do not turn ‘inside out’ after use.

Please reuse your personal hairnet. Please write your name on the hairnet and reuse. For visitors or 1-time users, dispose of hairnet after use.

Always wear disposable gloves in the cleanroom facility to minimize contamination.

See Appendix C, Cleanroom Attire.

Waste Disposal

Use waste containers for specified waste only.

If performing a non-standard procedure, you must provide your waste containers and label contents and owner (name, phone number).

When planning non-standard experiments, (i.e. buying new chemicals) at the same time plan for waste disposal and safety equipment. Also contact Brian Wajdyk anytime new chemicals are brought to facility.

MSDS are required. Fill out non-standard experiment request form.

Typically non-standard waste will be stored in sealed containers in former fume-hood outside of cleanroom area as cluttered chemicals/waste pose a serious hazard.

Emergencies

Emergencies, accidents and injuries can occur in any setting, at any time, without warning. It is every individual’s responsibility to be prepared physically and psychologically to handle an emergency. Preparation is the key to minimizing the effects of emergencies. Know the evacuation routes from any part of the laboratory. Familiarize yourself with the location and operation of all emergency equipment such as chemical shower, eyewash, etc. Any person receiving an injury or any nature shall report it without delay to the CeNSE staff.

The nature of the emergency will determine whether you will notify the CeNSE staff, the police or both.

Medical Emergencies

If you think a person requires immediate medical attention, always call the UK police at 257-1616.

Unconscious Victims: If rescuer is trained in CPR

1. Yell for help and have someone call 257-1616.
2. Establish Airway.
3. Check for Breathing.
4. Check for Circulation.
5. Start Ventilation or CPR if necessary.

Unconscious Victims: If rescuer is not trained in CPR

1. Yell for help and have someone call 257-1616.

Conscious Victims:

1.Yell for help and have someone call 257-1616.

2.Do not move patient or allow the patient to move around.

3.Try to control any heavy bleeding using direct pressure on the wound.

4.Try to keep the patient from going into shock by maintaining body temperature and elevating the lower extremities if possible.

Hazardous Material Incidents

Material Safety Data Sheets (MSDS) are available for all chemicals found in the laboratory. A sample MSDS sheet is provided in Appendix B. Any precautions or special procedures to be followed in the event of an emergency should be followed and relayed to emergency personnel. Small volume spills should be handled using the appropriate containment material found in the lab following the MSDS procedures.

For large volume Hazardous Material Spills beyond the capability of available containment materials, the following procedures should be followed.

Spill or Release Inside the Lab:

1. Activate the Fire Alarm.
2. Evacuate the area.
3. Notify the UK Police (257-1616)
4. Time and safety permitting, shut down equipment, close doors, secure area and vital records.
5. Limit activity to protection of lives and evacuation of personnel.

Spill or Release Outside the Lab:

1. Notify the UK Police (257-1616).
2. Comply with directives from Emergency Personnel.
3. Evacuate the area.
4. Time and safety permitting, shut down equipment, close doors, secure area and vital records.

Evacuation

1.Proceed to your nearest exit or alternate exit if necessary. Do not stop to remove suit, however booties may be removed to improve movement. Shut all doors as you leave.

2.If you are unable to immediately evacuate the CeNSE, notify UK Police (257-1616) as to your location.

3.Communicate locations of all fire/medical/hazardous situations and of situations where laboratory staff or persons requiring special assistance remain on site to emergency personnel (257-1616).

4.Proceed quietly and orderly.

5.Do not use elevators.

6.Do not open door if hot or if smoke is present.

7.Once outside, assemble at a designated area and stay there. CeNSE staff or other university personnel will need to tally those present.

Chemicals

A wide variety of chemical information exists in the Center. Materials Safety Data Sheets (MSDS) supply all chemical specifications and some safety information. A sample MSDS sheet is provided in Appendix D. An MSDS binder can be found in the blue binder on the cleanroom’s outer room bookshelves, and a binder is on the bookshelf in room 369. If you have any questions concerning a given chemical, consult the MSDS binder and CeNSE staff before using it. You have the right to know all the hazards and risks of any operation you will perform in the laboratory. If your concerns cannot be satisfactorily addressed with the available information, you have the right to refuse to perform any part of an operation that you feel is unsafe.

Prior to working with any chemical, make sure you are properly protected. Rubber gloves and safety goggles must be worn for any work with acids and other corrosive chemicals. Always work with chemicals at the exhausted wet bench.

The cleanroom gloves you put on when you enter the lab are to prevent particulate contamination. They are not sufficient for protection against chemical burns. Use the chemical gloves provided over your cleanroom gloves to maximize protection.

If immersion or exposure of your gloved hands in caustic or corrosive material is required, you should leak-check the rubber gloves prior to use. To check for leaks, pressurize each glove with a nitrogen gun and immerse it in water. If bubbles are observed, notify the CeNSE staff and discard them. Gloves should be thoroughly rinsed and dried following use.

Chemical Storage

Do not store the NH4OH or Acetone within 3 feet of the HCl, H2O2, or H2SO4.

In general, acids (HCl, H2SO4) must be kept away from bases (NH4OH), and oxidizers (H2SO4, H2O2) should be kept away from flammables (acetone).

Contact Brian Wajdyk anytime new chemicals are brought to facility.

MSDS are required.

Chemicals must be labeled with contact information (name/phone).

Handling Chemicals

When measuring chemicals, any excess should be stored in a clean, labeled container for future use. It should never be poured back into its reagent bottle since this may contaminate the chemical and damage the next user’s devices.

Chemical Burns

Should you be exposed to chemicals, immediately remove the affected clothing and flush the area with large volumes of water for at least 15 minutes. The emergency shower and/or eye wash station should be used if necessary. Notify a staff member of the exposure as soon as possible.

HF burns are especially hazardous since there may not be any immediate discomfort. These burns are extremely serious and may result in massive tissue damage. Any burning sensation is an indication that damage has begun. If you are exposed to HF, flush the area well and be sure to scrub under and around your fingernails. HF Acid Aid is available at the sink outside the rear gowning station. Inhalation of HF has the potential for serious medical complications and medical assistance should be sought immediately.

First Aid

Minor injuries can be treated with the first aid supplies located in the blue first aid cabinet above the sink outside the rear gowning station.

Minor Chemical Spills

Absorbent materials, such as spill control pillows, are located in the tub next to the wet bench in the event of minor chemical spills. A CeNSE staff member should be contacted as soon as possible regarding the spill. The proper personal protective equipment and MSDS procedures should be observed at all times.

Mixing Chemicals

Never add water to acid. Add acid to water. Use containers appropriate for the material. For example, HF should never be in a glass container. Fuming containers should always be used at the wet bench for proper ventilation. Chemical processes should never be left unattended unless absolutely necessary, and then only if clearly labeled with name, date, time, expected return, and the chemicals involved in the process.

Chemical Disposal

Waste disposal containers are available for all chemicals in the lab. Chemicals should never be disposed of by washing down the drain. If you are unable to locate the proper container or it is full, contact the CeNSE staff immediately.