throbber
Accessing
`Inaccessible
`Interfaces: In Situ
`Approaches to
`Materials Tribology
`
`W. Gregory Sawyer and Kathryn J. Wahl,
`Guest Editors
`
`Abstract
`The field of materials tribology has entered a phase of instrumentation and
`measurement that involves accessing and following the detailed chemical, structural,
`and physical interactions that govern friction and wear. Fundamental tribological
`research involves the development of new experimental methods capable of monitoring
`phenomena that occur within the life of a sliding contact. Measuring friction phenomena
`while the process is ongoing is a major improvement over earlier techniques that
`required the surfaces to be separated and analyzed, thereby interrupting the friction-
`causing event and modifying surface conditions. In the past, MRS Bulletinhas
`highlighted how insituapproaches can greatly enhance our understanding of materials
`structure, processing, and performance. This issue highlights insituapproaches as
`applied to materials tribology, namely, the study of contacting surfaces and interfaces in
`relative motion.
`
`Introduction
`Tribology is a field of study that is
`focused on the fundamental investigations
`of friction and wear. As recently summa-
`rized in a report on the “Frontiers of
`Fundamental Tribology,”1 new tools are
`needed to monitor tribological phenom-
`ena that are occurring within buried
` interfaces. These tools are essential for fun-
`damental studies of friction and wear
`because they are not intrinsic properties of
`a material; rather, they are functions of the
`tribological system (which includes the
`contacting surfaces that are in relative
`motion, the local environment, the back-
`ground temperature, the surface rough-
`ness and preparation, the sliding speeds
`and loads, and a host of other contribu-
`tors). Over the past half century, tribologi-
`cal systems have been discussed and
`described in terms of three basic groups of
`thematically linked elements:2 (1) the types
`
`of materials in contact and the contact
`geometry; (2) the operating conditions,
`including the gross motion, loads, stresses,
`and duration of operation; and (3) the
`environment and surface conditions,
`including the surface chemistry, surface
`topography, and ambient temperature.
`The incredibly large number of factors
`affecting tribological performance makes
`fundamental studies of materials tribology
`exceedingly difficult.
`Energy and material losses in moving
`mechanical devices as a result of friction
`and wear impose an enormous cost on the
`national economy. Engineering tribology
`involves the designs of bearings, bush-
`ings, and a wide variety of interfaces that
`support our everyday mobility and often
`aims to simultaneously reduce both fric-
`tion and wear. Practical solutions to miti-
`gate friction and wear have traditionally
`
`been through the use of fluid lubricants
`such as oils and greases. However, there
`are a number of applications where tradi-
`tional fluid lubrication strategies are either
`precluded or undesirable.3,4 Materials tri-
`bology, and in particular solid lubrication,
`is an area of research that aims to control
`friction and wear through both the appro-
`priate selection of known materials and
`the development of new materials and
`surface treatments.
`The contact between macroscopic sur-
`faces occurs on asperities, which are irreg-
`ularly shaped protuberances that exist on
`all engineering surfaces.5 Like fractals,
`these surface features occur across all
`length scales and define the distribution
`and shape of the real area of contact,
`which is orders of magnitude smaller than
`the apparent contact area.6–8 Thus, friction
`and wear arise from microscopic contacts
`that are under tremendous stresses and
`might have contact lifetimes of microsec-
`onds. In macroscopic systems, these con-
`tact locations are unknown and are buried
`in an apparent area of contact that is typi-
`cally inaccessible by most measurement
`techniques.
`Most materials tribology studies have
`focused on the friction coefficient and the
`wear rate. As shown in Figure 1, the fric-
`tion coefficient (µ) can be defined as the
`ratio of the friction force (Ff) to the normal
`force (Fn). The wear rate (K) is typically
`defined as the ratio of the volume of
` material removed (V) to the product of
`the applied normal load (Fn) and the dis-
`tance of sliding (d). Both the friction coef-
`ficient and the wear rate are sensitive to
`the starting conditions, load, speed, tem-
`perature, and environment. The initial
`transients during the approach to steady-
`state sliding are usually monitored but not
`modeled, and many of the reported and
`tabulated values for friction coefficients
`and wear rates are for steady-state
` conditions.
`To date, despite considerable efforts at
`understanding the origins of friction,
`there is no model capable of predicting
`friction coefficients from first principles.
`Similarly, there is no model for wear
`(which is often defined as the gradual
`removal of material from contacting sur-
`faces in relative motion) that is based on
`first-principles arguments. Thus, careful
`and proven experimental techniques rep-
`resent the most sophisticated and reliable
`approach for investigating, designing, and
`assessing the tribological worthiness of
`new materials. Fundamental studies of
`friction involve developing an under-
`standing of the real area of contact, surface
`chemistry, adhesion, and shear strength
`of the interface, as well as the nature of
`
`MRS BULLETIN (cid:127) VOLUME 33 (cid:127) DECEMBER 2008 (cid:127) www.mrs.org/bulletin
`
`1145
`
`Regeneron Exhibit 1166.001
`Regeneron v. Novartis
`IPR2021-00816
`
`

`

`Accessing Inaccessible Interfaces: In SituApproaches to Materials Tribology
`
`Macroscopic Tribology
`Testing
`
`Fn
`
`Ff
`
`pin-on-disk
`configuration
`
`friction coefficient
`(ratio of friction force to normal force)
`µ = Ff/Fn
`
`wear rate
`(volume lost per unit normal load per distance of sliding)
`
`K =
`
`V
`Fn d
`
`(
`
`mm3
`N m
`
`)
`
`Fn
`
`real area of
`contact
`
`Ff
`
`flat-on-flat configuration
`
`locally high pressures
`within the real area of contact
`
`plowing and plastic
`deformation
`
`debris
`generation
`
`fn
`
`ff
`
`hard asperity or probe tip
`
`counterface material
`
`Wear and Friction at the Nanoscale
`
`Figure 1. Tribology measurements for friction coefficient (µ) are traditionally made dynamically through force transducers that record both
`the lateral, or friction force (Ff) and the normal force (Fn). Whether a spherically tipped pin or a flat countersurface, the real area of contact
`(shown in blue) is a very small component of the apparent or projected contact area. The wear rate (K), defined as a ratio of the volume of
`material removed (V) to the product of the normal load (Fn) and the sliding distance (d), is rarely measured under dynamic conditions.
`As shown in the inset (lower right), the contact pressures at the asperity level (ƒf and ƒn, where Ff = ∑ƒf and Fn = ∑ƒn) are typically large
`and approach the flow stress of the softer material. Single-asperity tribology measurements of friction can be accessed using atomic force
`microscope probes, and the deformation and structural transformation at this scale can be studied using tools such as insitutransmission
`electron microscopy.
`
`deformation and energy dissipation
`occurring at the asperity junctions.
`
`State of the Art
`There are no standard reference samples
`(such as the standard kilogram prototype
`maintained by the International Bureau of
`Weights and Measures) in materials tribol-
`ogy because the specimens are consumed
`during testing. Thus, friction and the pro-
`gression of wear must be monitored by
`sensitive force and displacement measure-
`ments and with periodic interruptions to
`examine the contacting surfaces. As illus-
`trated in Figure 2, two common in situ
`approaches are used to follow and link
`chemical, structural, and physical interac-
`tions with friction and wear processes.
`
`The most common in situ tribology
`approach has been to perform detailed
`measurements on the surface of the sam-
`ple within the environment but outside
`the contact. The tribofilms and surface
`topography that develop during testing
`can be carefully studied between contacts;
`postprocessing of the data enables cycle-
`by-cycle analysis that can be used to link
`data from the current cycle with the fric-
`tion and wear measurements of the previ-
`ous cycle. The advantage here is that the
`testing of the samples can take place
`under the appropriate tribological system
`conditions in an environment that is not
`varying during observation and experi-
`mentation. Full-scale engineering compo-
`nents down to devices on the scale of
`
`microelectromechanical systems can be
`analyzed in this way. A serious limitation
`is that the analytical measurements are
`not carried out within the contact, so infer-
`ences need to be drawn between the
`observations outside the contact and
`the probable dynamics (chemical and
`mechanical) that exist within the contact.
`In situ approaches that enable meas -
`urements within a contact are ideal.
`However, such approaches frequently
`require compromises of sample composi-
`tion, geometry, and testing environment
`to be made. For example, transparent
`materials enable observations of the inti-
`mate contact areas but are often not the
`traditional counterface material for the
`application. Additionally, spherical or pla-
`
`1146
`
`MRS BULLETIN (cid:127) VOLUME 33 (cid:127) DECEMBER 2008 (cid:127) www.mrs.org/bulletin
`
`Regeneron Exhibit 1166.002
`Regeneron v. Novartis
`IPR2021-00816
`
`

`

`Accessing Inaccessible Interfaces: In SituApproaches to Materials Tribology
`
`in situ approaches
`within the contact
`
`Fn
`
`Ff
`
`pin/counterbody
`
`real area of
`contact
`
`in situ approaches
`within the environment
`
`specified
`environment
`
`tribofilm
`
`wear track
`and debris
`
`solid lubricant
`coatings or bulk
`materials
`
`Figure 2. Various insituapproaches have been employed in tribological studies.
`Fundamental measurements of the real area of contact, the interfacial film or tribofilm
`chemistry, and the wear track morphology and wear rates are common goals. Here,
`microscope objectives illustrate pathways for insitustudies. The most common approach is
`to examine the surfaces emerging from a contact within the specified environment. A more
`complex scenario is to perform the measurements within the contact, as illustrated by the
`objectives looking through a transparent counterbody from above, below, or the side. Some
`compromise of the sliding contact (for example, materials, geometry, or scale) is typically
`required to achieve an insitumeasurement of this type.
`
`nar geometries are frequently selected for
`their suitability to the measurement rather
`than to the application. A number of ana-
`lytical techniques have been employed for
`in situ tribology studies. Many of these
`techniques are listed in Table 1, with
`examples of the measurement application,
`resolution, and limitations.
`The miniaturization of force and dis-
`placement measurement technologies
`have enabled a new suite of tribological
`test equipment that can be relatively easily
`integrated within a variety of existing
` surface analytical instruments. In other
`cases, advances in surface-science instru-
`mentation have enabled these tools to
`be integrated with existing tribological
`equipment. Together, the merging of
` surface analytical instrumentation and
`careful tribological instrumentation is pro-
`viding new and exciting opportunities to
`study the fundamentals of friction and
`wear.
`
`In This Issue
`In this issue of MRS Bulletin, we high-
`light the possibilities of applying in situ
`methods to the study of buried sliding
`interfaces found in tribological contacts.
`We have selected topics describing the
`state of the art in five areas ranging from
`the propagation of interfacial slip along
`crack fronts that simulate geological inter-
`faces relevant to earthquakes to nanoscale
`single-asperity contacts probing how
`small collections of atoms accommodate,
`and are transformed by, sliding. Whereas
`previous MRS Bulletin issues tackling
`materials tribology9–11 have highlighted a
`combination of parallel experimental and
`computational methods, the focus of this
`issue is on the development of experimen-
`tal approaches allowing direct probing of
`materials mechanics and chemistry active
`in sliding contacts. Two of the articles
`address fundamental studies of liquid and
`solid lubrication using a range of in situ
`
`microscopy and spectroscopy approaches.
`The article by Cann reviews the applica-
`tion of infrared and Raman microscopy to
` liquid-lubricated contacts, showing how
`the relationship between molecular con-
`formation, pressure, additives, and lubri-
`cant degradation can be correlated to
`friction performance. The article by Wahl
`and Sawyer reviews in situ approaches
`to understanding
`solid
`lubrication
` phenomena. Examples are provided to
`illustrate how optical and interference
`microscopy, Raman microscopy, and elec-
`tron microscopy are applied to link real-
`time changes in interfacial film chemistry,
`morphology, and rheology to friction and
`wear events.
`The remaining three articles address the
`state of the art in examining tribological
`contacts controlled by asperity-scale inter-
`actions. Marks et al. describe advances in
`in situ transmission electron microscopy to
`understand asperity–asperity interactions.
`The tools for controlling indentation
`and sliding of nanoscale contacts within
`the field of view of an electron microprobe
`provide unprecedented opportunities to
`observe atomic-scale tribological deforma-
`tion processes in real time. The article by
`Bennewitz and Dickinson reviews another
`aspect of the state of the art in in situ
`atomic-scale measurements of wear. In this
`case, carefully prepared surfaces and
` controlled chemical environments allow
`examination of the role of defects and
`chemistry in the initiation of wear and its
`relation to atomic-scale friction. The last
`article, by Rubenstein et al., describes
`in situ optical measurements of the onset of
`sliding that show that the crack front
`motion comprises velocities from sluggish
`(tens of meters per second) to beyond the
`shear wave speed (>1,000 m/s). These
`direct observations indicate how the onset
`of sliding is influenced and controlled by
`these unusual crack propagation modes.
`These articles illustrate a subset of the
`wide range of possibilities for applying
`in situ experimental methods to the chal-
`lenge of understanding the materials and
`interface science of buried sliding inter-
`faces. The in situ approaches could confirm
`or refute commonly accepted lubrication
`models and will allow closer comparison
`with molecular simulations of friction
`processes. Progress in materials tribology
`will depend on developing a detailed
`understanding of what is happening in
`buried sliding interfaces.
`
`Acknowledgments
`W.G.S. and K.J.W. gratefully acknowl-
`edge the support of the Office of Naval
`Research and the Air Force Office of
`Scientific Research.
`
`MRS BULLETIN (cid:127) VOLUME 33 (cid:127) DECEMBER 2008 (cid:127) www.mrs.org/bulletin
`
`1147
`
`Regeneron Exhibit 1166.003
`Regeneron v. Novartis
`IPR2021-00816
`
`

`

`Accessing Inaccessible Interfaces: In SituApproaches to Materials Tribology
`
`Table I: In situapproaches used for tribological interface studies
`
`Technique
`
`Measurement
`
`Optical microscopy
`
`Tribofilm formation and motion, contact size
`
`Interferometry (contact)
`
`Contact separation
`
`Interferometry (wear track) Wear
`
`Raman microscopy
`
`Composition/chemistry, film thickness
`
`ATR-FTIR spectroscopy
`
`Chemical bonding
`
`TEM + EELS + AFM/
`nanoindentation
`
`Microstructural transformation, interfacial film
`formation composition, chemistry
`
`SEM/EDX
`
`Surface morphology, composition
`
`Cross section of sliding surfaces w/o separation
`
`Structure
`
`Spatial
`Resolution
`~ 1 µm
`~ 1 µm
`~ 1 µm
`
`Limitations
`
`One counterface must be optically transparent.
`
`One counterface must be optically transparent.
`
`Index of refraction or reflectivity changes can
`distort results.
`
`One counterface must be optically transparent.
`
`~ 1 µm
`mm to cm One counterface must be IR-transparent.
`(width of
`crystal)
`
`0.1 nm
`
`10 nm
`
`0.1 nm
`µm’s
`
`Interface region must be electron-transparent;
`vacuum environment
`
`Contact charging, contamination in low
`vacuum environments
`
`Potential beam damage from FIB sectioning
`
`Requires synchrotron access
`
`SEM + FIB
`SFA + x-ray diffraction
`or neutron relativity
`
`AFM
`
`AES
`
`XPS
`
`Friction, surface topography, contact stiffness, wear
`
`~ 1 nm
`
`Difficult to ascertain contact size, chemistry
`
`Composition
`
`Composition, chemical state
`
`10 nm
`10s of µm
`
`Cannot probe inside contact zone
`
`Cannot probe inside contact zone
`
`Contact resistance
`
`Coating thickness, damage, interfacial film formation
`
`Note:ATR-FTIR, attenuated total reflection Fourier transform infrared spectroscopy; TEM, transmission electron microscopy; AFM, atomic force microscopy; EELS,
`electron energy loss spectroscopy; SEM, scanning electron microscopy; EDX, energy dispersive x-ray spectroscopy; FIB, focused ion beam; SFA, surface force
`apparatus; AES, Auger electron spectroscopy; XPS, x-ray photoelectron spectroscopy.
`
`References
`1. S.S. Perry, W.T. Tysoe, Tribol. Lett. 19 (3), 151
`(2005).
`2. F.P. Bowden, D. Tabor, Br. J. Appl. Phys. 17
`(12), 1521 (1966).
`3. P.J. Heaney, A.V. Sumant, C.D. Torres, R.W.
`Carpick, F.E. Pfefferkorn, Diamond Relat. Mater.
`17 (3), 223 (2008).
`
`4. M.R. Hilton, P.D. Fleischauer, Surf. Coat.
`Technol. 55 (1–3), 435 (1992).
`5. J.A. Greenwood, J.B. P. Williams, Proc. R. Soc.
`London A 295 (1442), 300 (1966).
`6. B.N.J. Persson, Phys. Rev. Lett. 8711 (11),
`116101 (2001).
`7. B.Q. Luan, M.O. Robbins, Nature 435 (7044),
`929 (2005).
`
`8. C. Campana, M.H. Muser, M.O. Robbins,
`J. Phys.: Condens. Matter 20 (35) (2008).
`9. “Materials Tribology,” MRS Bull. 16 (10),
`(1991).
`10. “Nanotribology,” MRS Bull. 18 (5), (1993).
`11. “Fundamentals of Friction,” MRS Bull. 23
`■■
`(6), (1998).
`
`Mechanical and
`Aerospace Engineering,
`Gainesville, FL 32611,
`USA; and e-mail
`wgsawyer@ufl.edu.
`Sawyer is the N.C.
`Ebaugh Professor of
`Mechanical and
`Aerospace Engineering
`at the University of
`Florida. He received his
`PhD degree from
`Rensselaer Polytechnic
`Institute in 1999.
`Sawyer’s research
` interest is in the area of
`materials tribology. Over
`the past decade, the
`
`Tribology Laboratory at
`the University of Florida
`has developed numerous
`experimental appara-
`tuses for interrogating
`materials under extreme
`environments, including
`vacuum, cryogenic, and
`high temperature. The
`laboratory also designed
`and built an array of tri-
`bometers that are cur-
`rently scheduled to be
`operated in space as
`part of a 2009
`NASA–Materials
`International Space
`Station Experiment.
`
`Sawyer also has been
`active in developing
`polymeric nanocompos-
`ites for solid lubrication
`(recently demonstrating
`ultra-low wear with
`polytetrafluoroethylene
`nanocomposites) and
`probing the molecular
`origins of friction and
`wear (using a coupled
`computational simula-
`tion and experimental
`tribology program at the
`University of Florida).
`Additionally, Sawyer
`was chair of the 2008
`International Joint
`
`W. Gregory Sawyer
`
`Kathryn J. Wahl
`
`W. Gregory Sawyer,
`Guest Editor for this
`issue of MRS Bulletin,
`
`can be reached at the
`University of Florida,
`Department of
`
`1148
`
`MRS BULLETIN (cid:127) VOLUME 33 (cid:127) DECEMBER 2008 (cid:127) www.mrs.org/bulletin
`
`Regeneron Exhibit 1166.004
`Regeneron v. Novartis
`IPR2021-00816
`
`

`

`Accessing Inaccessible Interfaces: In SituApproaches to Materials Tribology
`
`Roland Bennewitz
`
`Gil Cohen
`
`J. Thomas Dickinson
`
`Jay Fineberg
`
`Laurence D. Marks
`
`Tribology Conference
`and serves on the edito-
`rial boards of the jour-
`nals Wear and Tribology
`Letters.
`
`Kathryn J. Wahl, Guest
`Editor for this issue of
`MRS Bulletin, can be
`reached at U.S. Naval
`Research Laboratory,
`Code 6176, Washington
`DC 20375, USA; tel.
`1-202-767-5419; and
`e-mail kathryn.wahl@nrl.
`navy.mil.
`Wahl heads the
`Molecular Interfaces and
`Tribology Section at the
`Naval Research
`Laboratory (NRL). She
`joined the NRL in 1992 as
`a National Research
`Council Postdoctoral fel-
`low and became a staff
`scientist in 1995. She
`received a B.A. in
`Physics and Mathematics
`from St. Olaf College in
`1987, and a Ph.D. in
`Materials Science and
`Engineering from
`Northwestern University
`in 1992. Her research has
`focused on fundamental
`physics and chemistry of
`sliding and adhesive
`interfaces, both at macro-
`scopic and nanometer
`scales. Currently, her
`research efforts include
`the development of
`in situ chemical and
`mechanical methods to
`probe bioadhesive con-
`tacts created by marine
`biofoulants, such as bar-
`nacles. Wahl chaired the
`2008 Tribology Gordon
`
`Research Conference,
`serves on the editorial
`boards of Tribology Letters
`and Wear, and is a fellow
`of the American Vacuum
`Society.
`
`Roland Bennewitz can
`be reached at INM—
`Leibniz Institute for New
`Materials, Campus D2 2,
`66123 Saarbrücken,
`Germany; and e-mail
`roland.bennewitz@inm-
`gmbh.de.
`Bennewitz is head of
`the Nanotribology Group
`at the INM—Leibniz
`Institute for New
`Materials in Saarbrücken,
`Germany. He received
`his Habilitation degree
`from the University of
`Basel, Switzerland, in
`2002. Bennewitz was an
`assistant professor at
`McGill University in
`Montreal, Canada, from
`2004 until 2008, where he
`also held the Canada
`Research Chair in
`Experimental
`Nanomechanics. His
`main research focuses are
`the microscopic mecha-
`nisms of friction and
`wear and the mechanical
`properties of materials
`with a nanometer-scale
`structure.
`
`Philippa M. Cann can be
`reached by e-mail at
`p.cann@imperial.ac.uk.
`Cann is a principal
`research fellow in the
`Tribology Group at
`Imperial College
`London. Throughout the
`
`last 20 years, her research
`has focused on experi-
`mental studies of lubrica-
`tion and lubricants,
`particularly grease lubri-
`cation of rolling element
`bearings. More recently,
`Cann has been develop-
`ing experimental meth-
`ods in biotribology and,
`in particular, synovial
`joint lubrication research.
`Her research has been
`recognized by a number
`of awards: the IMecE
`Thomas Stephen Prize
`(1996), the STLE Walter
`D. Hodson Award (1998),
`the STLE Wilbur Deutsch
`Award (2001), the NLGI
`Authors Award (2000),
`and the Royal Swedish
`Academy of Engineering
`Sciences, Jacob
`Wallenberg Foundation
`Grant (2004). In 2004,
`Cann was awarded the
`Institution of Mechanical
`Engineers, Tribology
`Silver Medal from the
`Tribology Trust.
`
`Gil Cohen can be
`reached at the Racah
`Institute of Physics,
`Hebrew University of
`Jerusalem, Givat Ram,
`Jerusalem 91904, Israel;
`tel. 972-2-6585720; fax
`972-2-6584437; and
`e-mail gilc@vms.huji.ac.il.
`Cohen has been a labo-
`ratory researcher at the
`Hebrew University of
`Jerusalem since 2003. He
`received his PhD degree
`from the Hebrew
`University of Jerusalem
`in 2000. His research
`
`interests include friction,
`fracture, nonlinear phe-
`nomena, and biophysics.
`
`J. Thomas Dickinson
`can be reached at
`Washington State
`University, Pullman, WA
`99164-2814, USA; tel.
`509-335-4914; and
`e-mail jtd@wsu.edu.
`Dickinson is the Paul
`A. Anderson Professor
`of Physics and Regents
`Professor at Washington
`State University (WSU).
`He also leads the Surface
`Dynamics Group at
`WSU. Dickinson
`received his bachelor’s
`degree from Western
`Michigan University
`and his PhD degree in
`physics at the University
`of Michigan. He joined
`the faculty at WSU in
`1968. Dickinson’s work
`has focused on the
`interaction and conse-
`quences of mechanical,
`chemical, and radiative
`stimuli on primarily
`nonmetallic materials.
`His current research
`interests include
`nanometer scale
`tribochemistry and
`VUV/femtosecond laser-
`surface interactions. He
`is the author/co-author
`of more than 320 refereed
`publications and is a
`fellow of MRS, APS, AVS,
`and AAAS.
`
`Jay Fineberg can be
`reached at the Racah
`Institute of Physics,
`Hebrew University of
`
`Jerusalem, Givat Ram,
`Jerusalem 91904, Israel;
`tel. 972-2-6585207; fax
`972-2-6584437; and
`e-mail jay@vms.huji.ac.il.
`Fineberg has been a
`faculty member at the
`Hebrew University of
`Jerusalem since 1992 and
`holds the Max Born
`Chair in Natural
`Philosophy. He received
`his PhD degree from the
`Weizmann Institute of
`Science in 1988. His inter-
`ests include fracture, the
`dynamics of friction,
`nonlinear wave interac-
`tions, and nonlinear phe-
`nomena. The recipient of
`a number of prestigious
`awards, Fineberg also
`has authored numerous
`scientific papers.
`
`Laurence D. Marks can
`be reached at the
`Department of Materials
`Science and Engineering,
`Northwestern University,
`Evanston, IL 60208, USA;
`tel. 847-491-3996; and
`e-mail L-marks@
`northwestern.edu.
`Marks is a professor of
`materials science and
`engineering at
`Northwestern University.
`After receiving his BA
`degree in chemistry at
`the University of
`Cambridge, UK, and his
`PhD degree in physics at
`the Cavendish
`Laboratory, Cambridge,
`UK, Marks was a post-
`doctoral researcher at
`Cambridge and at
`Arizona State University.
`
`MRS BULLETIN (cid:127) VOLUME 33 (cid:127) DECEMBER 2008 (cid:127) www.mrs.org/bulletin
`
`1149
`
`Regeneron Exhibit 1166.005
`Regeneron v. Novartis
`IPR2021-00816
`
`

`

`Accessing Inaccessible Interfaces: In SituApproaches to Materials Tribology
`
`Arno Merkle
`
`Andrew Minor
`
`Shmuel M. Rubinstein
`
`Oden L. Warren
`
`He joined the faculty of
`Northwestern University
`in 1985. Marks’ current
`research interests include
`nanotribology,
`dry-cutting, transmission
`electron microscopy,
`oxide surface science and
`catalysis, nanoparticles,
`solid-oxide fuel cells,
`nanoplasmonics, and
`density- functional theory.
`In addition, he is the
`author or co-author of
`more than 250 refereed
`articles.
`
`Arno Merkle can be
`reached at Carl Zeiss
`SMT Inc., One
`Corporation Way,
`Peabody, MA 01960,
`USA; tel. 617-515-5031;
`and e-mail
`a.merkle@smt.zeiss.com.
`Merkle is a transmis-
`sion electron microscopy
`(TEM) specialist at Carl
`Zeiss SMT Inc. for their
`operations in North
`America. In 2001, he
`received a BA degree in
`physics at Gustavus
`
`Adolphus College in St.
`Peter, MN. Merkle
`earned his PhD degree in
`2007 from the Materials
`Science and Engineering
`Department at
`Northwestern University.
`His research experience
`and collaborations
`extend to a number of
`institutions worldwide,
`including Argonne
`National Laboratory
`(USA), the Max Planck
`Institute for Metals
`Research in Stuttgart,
`Germany, and the
`Fraunhofer Institute for
`the Mechanics of
`Materials in Freiburg,
`Germany. Merkle’s
`research interests com-
`bine both theoretical
`(physical model genera-
`tion) and experimental
`(in situ TEM) approaches
`to understanding funda-
`mental nanoscale mecha-
`nisms at tribological
`interfaces. He is the
`recipient of a DAAD
`research grant and was
`named teaching
`
`assistant of the year
`while at Northwestern
`University.
`
`Andrew Minor can be
`reached at 1 Cyclotron
`Road, MS 72, Berkeley,
`CA 94720, USA; tel. 510-
`495-2749; fax 510-486-
`5888; and e-mail
`aminor@berkeley.edu.
`Minor is an assistant
`professor of materials
`science and engineering
`at the University of
`California, Berkeley
`(UCB), and also a
`faculty scientist at the
`National Center for
`Electron Microscopy
`at the Lawrence
`Berkeley National
`Laboratory. He
`received his bachelor’s
`degree in economics
`and mechanical engi-
`neering from Yale
`University and
`his MS and PhD degrees
`in materials science
`and engineering from
`UCB. Minor’s research
`group focuses on
`
`nanomechanical
`size effects, characteriza-
`tion of soft materials,
`and novel in situ TEM
`methods for materials
`science research.
`
`Shmuel M. Rubinstein
`can be reached at the
`Racah Institute of
`Physics, Hebrew
`University of Jerusalem,
`Givat Ram, Jerusalem
`91904, Israel; tel. 972-2-
`6584330; fax 972-2-
`6584437; and e-mail
`rshmuel@vms.huji.ac.il.
`Rubinstein is nearing
`completion of his PhD
`degree studies at the
`Racah Institute of
`Physics of the Hebrew
`University of Jerusalem.
`He received his BS
`and MS degrees from
`the Hebrew University
`of Jerusalem. The
` recipient of the Charles
`Clore fellowship in
`2007, Rubinstein’s
`interests include the
`dynamics of friction,
`fracture, and nonequilib-
`
`rium electro-osmotic
`instabilities.
`
`Oden L. Warren can be
`reached by e-mail at
`owarren@hysitron.com.
`Warren is the chief
`technology officer of
`Hysitron, Inc. He received
`his PhD degree in physi-
`cal chemistry from Iowa
`State University, where he
`performed ultrahigh-
`vacuum surface science
`research on ultrathin-
`film systems. Thereafter,
`Warren advanced the
`interfacial force micro-
`scope as a postdoctoral
`fellow at Sandia National
`Laboratories, New
`Mexico, and the
`University of Western
`Ontario, Canada. He
`joined Hysitron in 1998,
`where he has led a
`number of major instru-
`mentation development
`projects related to
`nanomechanical
`testing—including
`serving as the principal
`investigator of several
`U.S. Department of
`Energy Small Business
`Innovation Research
`grants. Warren has
`co-authored more than
`50 papers in surface
`science, nanomechanics,
`and nanotribology
`fields and has received
`an R&D 100 Award
`for the development
`of a quantitative
`nanoindenter for the
`transmission electron
`microscope.
`
`■■
`
`1150
`
`MRS BULLETIN (cid:127) VOLUME 33 (cid:127) DECEMBER 2008 (cid:127) www.mrs.org/bulletin
`
`Regeneron Exhibit 1166.006
`Regeneron v. Novartis
`IPR2021-00816
`
`

This document is available on Docket Alarm but you must sign up to view it.


Or .

Accessing this document will incur an additional charge of $.

After purchase, you can access this document again without charge.

Accept $ Charge
throbber

Still Working On It

This document is taking longer than usual to download. This can happen if we need to contact the court directly to obtain the document and their servers are running slowly.

Give it another minute or two to complete, and then try the refresh button.

throbber

A few More Minutes ... Still Working

It can take up to 5 minutes for us to download a document if the court servers are running slowly.

Thank you for your continued patience.

This document could not be displayed.

We could not find this document within its docket. Please go back to the docket page and check the link. If that does not work, go back to the docket and refresh it to pull the newest information.

Your account does not support viewing this document.

You need a Paid Account to view this document. Click here to change your account type.

Your account does not support viewing this document.

Set your membership status to view this document.

With a Docket Alarm membership, you'll get a whole lot more, including:

  • Up-to-date information for this case.
  • Email alerts whenever there is an update.
  • Full text search for other cases.
  • Get email alerts whenever a new case matches your search.

Become a Member

One Moment Please

The filing “” is large (MB) and is being downloaded.

Please refresh this page in a few minutes to see if the filing has been downloaded. The filing will also be emailed to you when the download completes.

Your document is on its way!

If you do not receive the document in five minutes, contact support at support@docketalarm.com.

Sealed Document

We are unable to display this document, it may be under a court ordered seal.

If you have proper credentials to access the file, you may proceed directly to the court's system using your government issued username and password.


Access Government Site

We are redirecting you
to a mobile optimized page.





Document Unreadable or Corrupt

Refresh this Document
Go to the Docket

We are unable to display this document.

Refresh this Document
Go to the Docket