3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE I LECTURE 4: FORCE-DISTANCE CURVES Outline : LAST TIME : ADDITIONAL NANOMECHANICS INSTRUMENTATION COMPONENTS ......................... 2 PIEZOS TUBES : X/Y SCANNING ............................................................................................................ 3 GENERAL COMPONENTS OF A NANOMECHANICAL DEVICE............................................................. 4 HIGH RESOLUTION FORCE SPECTROSCOPY (HRFS) ....................................................................5-9 Force-Distance Raw Data ....................................................................................................... 5 Force-Distance Data Conversion ............................................................................................ 6 Chemical Force Microscopy (CFM).......................................................................................... 7 Macromolecular Adhesion : Cartilage Aggrecan ...................................................................... 8 Lateral Force Microscopy (LFM) .............................................................................................. 9 Objectives: To understand high resolution force spectroscopy data; i.e. how it is converted from raw data, interpretation of different regions, and different types (i.e. normal, lateral, & chemically specific) Readings: Course Reader Document 10-11. Multimedia : Watch movie Introduction to AFM by Asylum Research, Inc., and the Force curve animation from NCState. 1 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE LAST TIME : ADDITIONAL NANOMECHANICS INSTRUMENTATION COMPONENTS High resolution displacement detection : Optical Lever (Beam) Deflection Technique Lateral Force V -V A+C B+D Microscopy (LFM) VA+ B-VC+D High resolution displacement control : "piezoelectric materials" : material which exhibits a change in dimensions in response to an applied voltage due to dipole alignment mirror A B C D Normal Force Microscopy 4-quadrant (NFM) position sensitive laser beam photodiode cantilever ε is linearly proportional to electric field strength : ε j = dij Εi sample probe tip ΔL = strain (m/m = unitless) Lo dij = strain coefficients or sensitivity (m/Volt) εj = D+ΔD Ei = electric field strength (Volt/m) d +Z D i = direction of applied field, j = direction of strain 1,2,3 = normal axes ; 4, 5, 6 = shear + Poisson's ratio ΔL = Lo d 31U 3 where d = wall thickness,U = operating voltage d ~ -Z electrodes Lo Lo+ΔL voltage applied -X +Y electrodes +X z (1) y (3) x (2) connecting wires 2 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE PIEZO TUBES X/Y SCANNING x/y (bottom) scanner (side view) : single axis positioner apply voltages to different sides of tube side view of monolithic tube z- piezo (top) left x-segment right x-segment U=0 z outer electrode - y inner electrode + ysegment front z - + + - + - -tube contracts radially (small amount) tube expands radially tube contracts radially -expands much more in z-direction due to lowers height height increases high aspect ratio tube tilts - reverse voltage- scan in opposite direction - same for y-axis positioning -Coupling - if you tell the piezo tube to move in x-direction, it will also move a bit in y and z, x is coupled to y and z Figure by MIT OCW. -Another approach : individual "piezo stacks" with flexures in a "nested design" (Introduction to AFM by Asylum Research, Inc. (Quicktime Movie)- Pset 2 3 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE GENERAL COMPONENTS OF A NANOMECHANICS DEVICE I. high-resolution force transducer III. displacement detection system δ sample II. high-resolution displacement control z 4 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE approaching A. tip and sample out of contact B. attractive interaction pulls tip down towards surface C. tip jumps to surface D. tip and sample / z-piezo move in unison (δ=cantilever deflection) δ1=0 δ2<0 δ3<0 δ4>0 G. tip and sample out of contact F. tip releases from surface E. attractive force keeps tip in contact with surface D. tip and sample / z-piezo move in unison Photodiode Sensor Output, s (V) HIGH RESOLUTION FORCE SPECTROSCOPY EXPERIMENT (HRFS): RAW DATA no interaction repulsive regime jump-to-contact 0 adhesion attractive regime 0 z-Piezo Deflection, z (nm) - Measure sensor output (Volts) vs. z-piezo displacement/deflection - See animation on the MIT Server (Force curve animation from NC State). retracting 5 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE HIGH RESOLUTION FORCE SPECTROSCOPY EXPERIMENT: CONVERTED F-D DATA repulsive regime Δδ Δz D kc attractive regime sample piezo Force, F (nN) x-axis conversion 0 D= Δz-Δδ Tip-Sample Separation Distance, D (nm) Contact vs. Noncontact region Zero x-axis position chosen (x=0) : by baseline far away from sample Zero y-axis position chosen (D=0) : as region of apparent infinite slope (artifact of soft spring, stiff sample) Jump to contact region : region of mechanical instability, cantilever moving too fast to collect data, lose all data in this region Adhesion force : maximum force needed to separate two bodies, determined by surfaces force/ intermolecular interactions; sources; hydration capillary forces in air, noncovalent interactions, polymer interactions, etc. 6 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE CHEMICAL FORCE MICROSCOPY (CFM) Vezenov DV, Noy A, Rosznyai LF, Lieber CM. 1997. J. Am. Chem. Soc. www.polymercentre.org.uk Image removed due to copyright restrictions. See Vezenov DV, Noy A, Rosznyai LF, Lieber CM. 1997. J. Am. Chem. Soc. Courtesy of The University of Sheffield Polymer Centre. Used with permission. 7 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE MEASURING MACROMOLECULAR ADHESION : CARTILAGE AGGRECAN Cartilage aggrecan is a very unique "bottle-brush" macromolecule that is largely responsible for the mechanical properties and health of cartilage tissue in our joints. (*podcasts later on in the semester on this topic, unpublished data by L. Han) Tip Motion H 9 Approach Retract 7 Force (nN) Image removed due to copyright restrictions. Diagram of cartilage aggrecan. 5 3 1 -1 -3 -5 0 200 400 600 Distance (nm) 800 1000 8 3.052 Nanomechanics of Materials and Biomaterials Thursday 02/15/07 Prof. C. Ortiz, MIT-DMSE LATERAL FORCE MICROSCOPY (LFM) shear of aggrecan “slip” HIGH NORMAL LOAD (F~20nN) “stick” “slip” “stick” “slip” Lateral Force (nN) “stick” 12 0.001M NaCl μΙ = 0.10±0.01 8 μII = 0.44±0.03 (II) (I) 4 0 10 20 Normal Force (nN) 30 -Measure shear / friction coefficient→nanotribology - study of friction and wear. -Linear dependence of lateral force on normal force between OH-SAM and aggrecan changed upon the point of full penetration of aggrecan layer by the nanosized probe tip. -At the same height, larger lateral forces were observed at lower IS, due to stronger shear resistance 9