ORTIZ POLYMER MECHANICS LABORATORY MANUAL Room 12-065 (Chemistry Lab, Phone : (617) 258-6154) Room 13-5037 (Nanomechanics Lab, Phone : (617) 253-8779) Massachusetts Institute of Technology Department of Materials Science and Engineering 77 Massachusetts Avenue, Cambridge, MA 02139 USA Research Advisor : Christine Ortiz, Assisant Professor Office : Room 13-4022, Office Phone : (617) 452 3084 Fax : (617) 452 3085 Email : cortiz@mit.edu WWW : http://web.mit.
TABLE OF CONTENTS : PAGE 3 4 5-7 8-10 11-12 13-31 32 33-36 37 38-41 42-43 44 45-52 53 ITEM 1. Checklist for New Group Members and Collaborators 2. Ortiz Lab Phone and Office List 3. General Laboratory Policies 4. Collaborator User Agreement Policies 5. Laboratory Supplies Order Form 6. Laboratory Safety Procedures and Training 6.1 DMSE Safety Primer 7. Laboratory Notebook Guidelines 8. Description of Laboratory Equipment 9. Safety Precautions : Asylum Research, Inc. Molecular Force Probe 10.
1. CHECKLIST FOR NEW GROUP MEMBERS AND COLLABORATORS ITEM TO BE COMPLETED 1. Please read this entire laboratory manual. 2. Please obtain copies of the AFM and MFP instrumentation manuals. Please obtain, read, and go through the DI Scanning Probe Microscopy Training Notebook (all can be obtained from Tim Doyle in 12-009). 3. Finish all safety trainings as outlined in Section 6. of this laboratory manual. 4. Collaborators : please read, sign, and return User Collaboration Agreement Form to Prof. Ortiz. 5.
2. GENERAL LABORATORY POLICIES 1. Ortiz primary students and postdocs have priority on all laboratory equipment. 2. All new group members and collaborators should be initially trained by an Ortiz graduate student (MFP trainer : Monica Rixman (mrixman@mit.edu), AFM trainer : Laurel Ng (ljng@mit.edu)) The trainer should be provided with a one-page summary of their planned experiments in the near future before beginning training.
3. ORTIZ LAB PHONE LIST F01 CHEMISTRY LAB : 12-065 , PHONE : 258-6154 NANOMECHANICS LAB : 13-5037 , PHONE : 253-8779 GRAD STUDENT OFFICE : 12-022 , PHONE : 258-5934 PRIMARY GROUP MEMBERS : Name Email (@mit.
George Gluck (BIO-YR 4) ggluck RM 12-022 / 258-5934 Ryan Jones (GRAD-MECHEYR2) Jennifer McKeehan (DMSE-GRADYR1) Laurel Ng (GRADBEH YR1) jonesre 3-0229 ljng RM 38-377: 2536944 436-5692 Christine Ortiz (DMSEResearch Advisor) Monica Rixman (GRAD-DMSEPPST-YR2) Joonil Seog (GRADMECHE-PPST YR4) cortiz RM 13-4022 / 452-3084 Fax : 452-3085 RM 12-022 / 258-5934 557-9996 407-4741 (cell) 629-5944 (cell) 549 4512 577-5699 Kuangshin Tai (DMSE-GRADYR1) D.
COLLABORATORS : Name Email (@mit.edu) Office / Work Phone (area code : 617) Phone (Home) Reuben Dormike rdomike 617 253-0472 617-7944441 Xueping Jiang (GRAD-CHEME YR2) xpjiang RM 66-525 253-6450 577-5637 Ryan Jones (GRAD-MECHEYR2) Sang Park (DMD) jonesre 3-0229 sang_park@hsd m.harvard.edu 432-1472 Winnie Yong (GRAD-YR2NUCLEAR) Brice Smith (GRAD-YR2PHYSICS) 617-2908136 wyong elrond WY (2251163) BS(3544827) 7 BDAY Collaborating Group James Cooney (CHEME cconey@mit.
4.
ORTIZ POLYMER MECHANICS LABORATORY COLLABORATOR USER AGREEMENT & POLICIES Supervisor: Christine Ortiz, Assistant Professor Department of Materials Science and Engineering (DMSE) Room 13-4022, 77 Massachusetts Avenue Cambridge, MA 02139 USA Phone : (617) 452 3084 Fax : (617) 452 3085 Email : cortiz@mit.edu WWW : http://web.mit.edu/cortiz/www/ Assistant : Tim Doyle Office : Room 12-006 Phone : (617) 253 6819 Fax: 617) 258 6936 Email : tbdoyle@mit.
ORTIZ POLYMER MECHANICS LABORATORY COLLABORATOR USER AGREEMENT FORM Collaborator Name: Campus Address: Campus Phone / Email: Home Address: Home Phone / Email: Advisor: Advisor Address: Advisor Phone / Email : Expected Dates of Experiments and Lab Usage: Date of AFM Training: AFM Trainer: Date of MFP Training: MFP Trainer: STUDENT SIGNATURE : ADVISOR SIGNATURE : ORTIZ SIGNATURE : Thank you for your cooperation with this policy.
5.
ORTIZ LABORATORY SUPPLIES ORDER FORM DATE VENDOR NAME VENDOR TELEPHONE OR URL ITEM NAME ITEM NUMBER PRICE (IF OVER $200 OBTAIN AUTHORIZATION FROM C. ORTIZ) QUANTITY UNIT (e.g. gallon, pack of 12, etc.) DATE NEEDED ACCOUNT NUMBER ADDITIONAL COMMENTS Please send to Tim Doyle (tbdoyle@mit.edu) or drop off to Room 12-099. Call if you have questions (3-6819).
6. LABORATORY SAFETY PROCEDURES AND TRAINING Manditory : I. Center for Materials Science and Engineering Requirements (CMSE) : I.A. Read the OSHA-mandated document, the Chemical Hygiene and Safety Manual. You can obtain a copy from the CMSE office, RM. 13-2090. I.B. Take the Center for Materials Science and Engineering (CMSE) Chemical Hygiene Hypercourse at : http://www.bostonconsortium.org/sub_gro_ehs_wbt.shtml II. Department of Materials Science and Engineering Requirements (DMSE) : II.A.
6.1 The DMSE Safety Primer Index • The DMSE Safety Program • Emergencies and First Aid • Basic Elements of Laboratory Safety • Chemical Hygiene • Radiation Safety Electrical safety • Cryogenic safety • Fire safety THE DMSE SAFETY PROGRAM Introduction Unfortunately, we tend to think of safety only after an accident. Laboratory safety, however, deserves and requires the same planning and attention that we give to research and teaching; it must not be an afterthought.
• • • • • Access to a laboratory will not be approved, and UROP proposals will not be signed, until the user has passed the examination and provided an acknowledgment of the safety briefing that has been signed by both the user and the Supervisor. Workers are to conduct themselves in a safe manner at all times, following the rules outlined in this Primer and other appropriate sources of information. The primary responsibility for safety resides with the individual worker.
• Mr. Joseph A. Adario Duties of the Safety Committee include: • The Committee assists the Departmental Safety Officer in formulating policies and procedures for laboratory safety, and also assists in formulating the examinations required under the Plan. • Each Departmental laboratory will be inspected twice yearly for compliance with safety procedures; these inspections are supervised by Mr. Kearney.
• After the emergency, promptly report the incident to the MIT Safety Office (phone 3-4736, room E19-207).
• • • • In case of a clothing fire, the victim should drop to the floor and roll, not run to a safety shower. A fire blanket, if nearby, should be used to smother the flames. After flames are extinguished, deluge the injured areas under a safety shower. Keep the water running on the injured areas for 15 minutes to remove heat and to wash off chemicals. Place clean, soaking wet, ice-packed cloths on burned areas, and wrap to avoid shock and exposure.
Conducting experiments • • • • • • • • • • • • • • • • • • • All injuries, accidents, and "near misses" must be reported to the Laboratory Supervisor. An Accident Report must be completed as soon as possible after the event by the Laboratory Supervisor. All chemical spills are to be reported to the Laboratory Supervisor, whose directions must be followed for containment and cleanup. Laboratory workers should follow the prescribed instructions for cleanup and decontamination of all spill areas.
• • • Personal items brought into the laboratory should be limited as much as is practical to those things necessary for the experiment. Safety laboratory practices prohibit the presence of young children and babies in areas that have a potential for exposure to radioactive materials, toxic or hazardous chemicals, infectious agents, or where the children are exposed to possible injury from a laboratory or other type of accident.
• • many of these are also available from the Internet ( click here). The MSDS should be obtained from the supplier when new chemicals are purchased. Based on the information in the MSDS and the way in which the chemical is to be used, the research worker must be aware of the control methods that are required. These control methods encompass storage, use, and any disposal methods other than the normal pick up of waste chemicals by the MIT Safety Office.
Choice of chemicals: • • • • • The use of the following five chemicals is illegal in the City of Cambridge, MA, and must not be brought onto the MIT campus.
Waste Disposal: • • • A label indicating "Chemical Waste" with the chemical name and concentration should be placed on each container of chemical waste by the user. The MIT Safety Office should be called to collect such chemical wastes and for answers to chemical waste disposal questions.
• • name(s). In any event, at the end of each workday, the contents of all unlabeled containers should be labeled or are to be considered wastes and placed into a properly labeled waste container. If unlabeled containers of chemicals are discovered, properly label the container if the contents are known, or call the MIT Safety Office so that the material can be properly identified and disposed. All chemicals should be placed in their assigned storage areas at the end of each workday.
• • Always store flammable liquids away from oxidizers. Be aware that liquids with flash points at and above 100oF may also present a significant fire hazard in case of ignition. Procedures for Reactive Chemicals Reactive chemicals are substances which may enter into violent reactions with the spontaneous liberation of heat and/or gases too rapidly to be safely dissipated. This may result in the rupture of the container, an explosion, fire or the release of toxic gases/vapors.
• A chemical fume hood is a safety backup for condensers, traps, or other devices that collect vapors and fumes. It should not be used to "dispose" of chemicals by evaporation unless the vapors are trapped and recovered for proper waste disposal.
Vapor Detection Odor should not be relied upon as a means of determining that inhalation exposure limits are or are not being exceeded. Whenever there is reason to suspect that a toxic chemical inhalation limit might be exceeded, whether or not a suspicious odor is noticed, notify the supervisor and/or the Environmental Medical Service. As an interim measure, laboratory use of the chemical should be stopped, or the use of the chemical limited to a chemical hood.
whether flammable or nonflammable, miscible or non miscible with water. Organic solvents should be placed in suitable containers (1 gallon maximum) where there is no danger that vapors or the liquid will escape. Containers shall be capped tightly, labeled prominently, and picked up by the MIT Safety Office . • Mixtures of organic solvents that are compatible and combined in one container must be identified with an estimated proportion in fractions or percentages of each solvent in the mixture indicated.
Unknown Waste Chemicals Unknown waste chemicals cannot be accepted for disposal. Disposal contractors cannot accept or ship unknown waste. It is the responsibility of the Laboratory Supervisor involved to identify all chemicals; this may require polling laboratory personnel, students, and faculty members to ascertain the owner of such unknown waste and its identity. Ultimately, it may require the services of an analytical laboratory to analyze the waste.
Work on electrical devices should be done only after the power has been shut off in such a manner that it cannot be turned on accidentally. Internal current-carrying devices such as capacitors must be discharged. All "home-made" electrical apparatus should be inspected and approved by someone competent in electrical circuitry before being placed in service. Observe the following rules when working with electrical equipment: • Ungrounded wiring and two-wire extension cords are prohibited.
Oxygen is removed from the air by liquid nitrogen. Therefore, use liquid nitrogen only in a well-ventilated area so that the ambient oxygen concentration does not drop lower than 19.5% (same for liquid helium). The high pressure gas hazard is always present when cryogenic fluids are used, since these are usually stored at the boiling point. Never obstruct the vent valve on cryogenic containers. Wood or asphalt saturated with liquid oxygen has been known to explode when subjected to mechanical shock.
7. LABORATORY NOTEBOOK GUIDELINES • Each section has a clear, descriptive heading of the experiments which were performed and detailed writing of the experimental observations, thoughts, and results. • Each entry is dated. • Each entry is legible. • Each entry is in English. • Each entry is written immediately after the work was performed. • Multiple lab notebooks should be labeled numerically in the order of which they were written. • Experimental data, originals or copies (e.g.
8. DESCRIPTION OF LABORATORY EQUIPMENT Molecular Force Probe (MFP) Asylum Research, Inc. : • Brief description of MFP and MFP specifications from Asylum Research, Inc. • MFP Saftety Precautions • Power Spectral Density of Deflection Thermal Noise of 0.01 N/m Cantilever taken with MFP in Air and Water • Thermomicroscopes Microlever Specifications and Corresponding Force Noise Levels with MFP (*courtesy of J. Cleveland, Asylum Research, Inc.
PureLab Plus UV/UF Laboratory Water Purification System (US Filter) AT200 Analytical Balance (MettlerToledo) PerpHecT pH Meter (ThermoOrion) 34
Nanomechanics Software : •IC Adams Nanomechanics Software Optical Microscopes : • Axioskop 20, Zeiss, Inc. with transmitted and reflected light, differential interference contrast, cross-polarizers, incident light flourescence. • Axioplan Zeiss, Inc.
Micro- and Macro- Mechanical Testing Equipment : • Rheometric Scientific (Polymer Labs) Minimat 2000 Miniature Materials Tester with Environmental Chamber • DMS 110 SEIKO and DMS 200 Dynamic Mechanical Rheology Station available through the MIT CMSE shared facilities 36
9. MFP SAFETY PRECAUTIONS Ortiz Nanomechanics Lab : 13-5037 1. PHOTODIODE AND LASER KNOBS : Please be sure not to push them beyond their range of motion. They are quite sticky at the ends and may get stuck or the belt may come off. 2. FLUIDS. Although there is minimal danger if fluids leak down into the base, please be careful when inverting the head and keeping the tip wet.
10. MULTIMODE AFM SAFETY PRECAUTIONS Ortiz Nanomechanics Lab : 13-5037 I. TIPHOLDERS : • Only use the AFM tipholders provided with the Multimode, do not use any early-model AFM tipholders from older AFM's, they may short out the power supply. II. LASER : • During and prior to laser alignment, avoid looking directly at the laser beam, the laser spot, or reflected laser light-especially with highly reflective samples. Staring at the laser beam can cause eye damage.
boxes, or other components containing electronic parts. Avoid spilling all corrosive fluids on exposed surfaces; otherwise damage will result (e.g. shorting out of piezo tube scanners). In case of a spill, immediately clean and dry all affected surfaces thoroughly. • Do not overfill the fluid cell. • Do not allow solvents to splash on the scanner tube or wiring at the center of the scanner body: certain components (e.g. wiring insulation) may be dissolved, causing scanner failure. IV.
Withdraw and then re-engage again. Thermal drift or other reasons may cause the z-center to change gradually with time. It change suddenly when if tip leaves the surface resulting in a fully retracted piezo (-220V). • Avoid using maximum scan sizes for long periods of time. Some crystals have sensitivities which will allow them to scan much larger than their nominal size specification.
computer, outputs to the piezo might be at random values (up to +/- 220V). • Do not unplug cables to / from energized hardware. Turn OFF first. • Do not insert a conducting object into the phase extender box while it is energized (e.g. screwdriver). • When closing the System.par file after viewing, if you are asked to SAVE CHANGES, be sure to say NO. VII. ENGAGEMENT / IMAGING • Never attempt to manually engage using the course adjustment screws.
11. FORCE CURVE DATA CONVERSION (M. Rixman) For data from the DI Multimode AFM 1. Export the raw data as an ASCII file Do this in the Offline/Utility menu. Header information is known to cause problems in some third party software applications and should therefore not be included in the ASCII file. Be sure to save the raw data file. The header information will be required for the data processing, and can be accessed from the raw data file. 2.
a determined distance from the previous z-position has been traveled. The Z distance between data points may be calculated as follows: Z dis tan ce between data po int s = Z scan size (nm) Samps / line The raw ASCII data has now been converted and is ready for further analysis. 4. Convert the deflection vs z-piezo position data into force vs separation Begin by plotting the raw data; there is some key information to be gotten from the plot. First locate the jump-to-contact point of the extension curve.
12. INSTRUCTION FOR CONDUCTING STATISTICAL ANALYSIS ON HIGH-RESOLUTION FORCE SPECTROSCOPY ADHESION DATA 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. Open the raw experiment *.PXP datafile of interest in Igor Pro. On the first drop down menu, go to File/Open File/Procedure and then open the procedure file RecordCursor.ipf (the source code will open).
13. PROCEDURES FOR IMAGING OF STANDARDS AT ATOMIC-SCALE RESOLUTION USING THE DIGITAL INSTRUMENTS MULTIMODE AFM Ortiz Nanomechanics Laboratory@MIT F01 I. Sample Producers and Preparation • Muscovite Mica is a yellowish, light-colored, transparent to translucent silicate (subclass : phyllosilicates) mineral with the following chemistry : K2Al4Si6Al2O20(OH,F)4, Potassium aluminum silicate hydroxide fluoride.
• use oxide-sharpened Si3N4 probe tips, e.g. Model NPS which has the following specifications (http://www.di).com/products2/NewProbeGuide/ContactModeProbes.html : PARAMETER spring constant nominal tip radius of curvature cantilever leg length cantilever configuration reflective coating shape of tip tip half angle VALUE 0.
sample is rotated until the atoms are oriented vertically or when the fast scan axis is parallel to the a or b crystallographic axis. The Proportional Gain should stay at zero except for large scan sizes (~70% of the scanner range). The system determines the minimum value of the Integral Gain. If you start with a value less than the system's minimum, you wont get an image. •Filters, you should be able to obtain an image with the filters off.
Figure 1. AFM High-Resolution Contact Mode Image of Mica from A.Belyayev, State Research Institute of Physical Problems & NT-MDT, Moscow, Russia. (unpublished) (*downloaded from : http://www.ntmdt.ru/scangallery/index.php?action=fullview&id=34) Figure 2. AFM High-Resolution Contact Mode Image of HOPG (*downloaded from : http://stm2.nrl.navy.mil/how-afm/how-afm.
Figure 3. AFM High-Resolution Contact Mode Image of HOPG (*downloaded from : http://www.physics.sfasu.edu/afm/afm.
(http://www.energosystems.ru/fgallery.htm) Figure 4.
IV. Off-line Image Analysis. • Go to Off-line / View / Top View option and measure the spacings between atoms. The spacings should be as follows (as shown in Figure 5) : MICA : A=0.519 nm, B=0.900 nm, C=1.37 nm HOPG : A=0.255 nm, B=0.433 nm, C=0.666 nm hexagonal atomic lattice A C B Figure 5. Hexagonal Atomic Lattice Record the spacings for ~ 10 atoms observed in a captured image and average them.
VI. References 1. Binnig, et al., Europhys. Lett. 3, 1281 (1987) [graphite] 2. Albrecht, et al., J. Vac. Sci. Tech. A 6 271 (1988) [molybdenum sulfide boron nitride] 3. (a) Manne, et al., Appl. Phys. Lett. 56 1758 (1990), (b) Meyer, et al., Appl. Phys. Lett. 56 2100 (1990), (c) Meyer, et al., Z. Phys.B. 79 3 (1990) [sodium chloride (001), lithium flouride] 4. Ohnesorge, et al., Science 260 1451 (1993)[(1014) cleavage plane of a calcite (CaCO3) crystal] 5.
14. TRAVEL AND REIMBURSMENT POLICIES Research grants will cover the following for approved business travel : 1. direct transportation (e.g. flights, taxis, car rental) 2. housing (e.g. hotel) 3. conference fees and registration All arrangements should be made in advance by the group member and also paid for by the group member.
