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A SEMINAR REPORT
Submitted by
Of
Dr. M. F. Wani
List of Symbols
2
Symbol Definition Units
r Radius of a meniscus m
R Radius of a ball m
Ftotal Total normal force N
Fapplied External applied normal force N
Fadhesion Adhesion force N
Fa Pull-off force N
t Thickness of beam m
h Initial separation between substrate and cantilever m
s Deflection length of cantilever m
Ff Friction force N
γ Work of adhesion J/m2
µ Coefficient of friction
Γ Surface-interaction energy J/m2
List of Figures
3
Figure No. Sources
1 B. Bhushan, Springer Handbook of Nanotechnology, Springer, 2nd ed.
(2007)
2 www.mems.sandia.gov
3 www.mems.sandia.gov
4 B. Bhushan, Introduction to Nanotribology, Wiley, 2002
5 www.nlbb.com
6 www.nlbb.com
7 www.mems.sandia.gov
8 B. Bhushan, Introduction to Nanotribology, Wiley, 2002
9 www.nlbb.com
10 H. Liu and B. Bhoshan, J. Vac. Sci. Technol. A22, 1388 (2004)
11 www.mems.sandia.gov
12 H. Liu and B. Bhoshan, J. Vac. Sci. Technol. A22, 1388 (2004)
13 H. Liu and B. Bhoshan, J. Vac. Sci. Technol. A22, 1388 (2004)
ABSTRACT
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MEMS devices are made of single-crystal silicon, LPCVD polysilicon films and other
ceramic films. Very little is understood about tribology and mechanical characterization of
these materials on micro- to nano scales. Atomic force microscopy/friction force microscopy
(AFM/FFM) techniques are increasingly used for tribological studies of engineering surfaces
at scales, ranging from atomic and molecular to micro scales. These techniques have been
used to study surface roughness, adhesion, friction, scratching/wear, indentation, and
boundary lubrication of bulk and treated silicon. Commonly measured roughness parameters
are found to be scale dependent, requiring the need of scale-independent fractal parameters
to characterize surface roughness. Measurements of micro-scale friction and macro scale
friction show that friction values both on micro- and macro scales of all samples are about
the same. The micro scale values are lower than the macro values as there is less ploughing
contribution in micro scale measurements. Local variation in micro scale friction is found to
correspond to the local slope. Directionality in the friction is observed on micro scale which
results from the surface preparation and anisotropy in surface roughness.
Microscratching/microwear and nano indentation studies indicate that coated/treated silicon
is superior to bare silicon. Chemically bonded lubricants appear to be suitable for MEMS
devices. Finally, ultra smooth surfaces under extremely lightly loaded conditions are
required for ultralow friction and near zero wear.
[1] INTRODUCTION
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The moving contact of two solid surfaces results in friction and wear. Annually, friction and
wear are estimated to cost the United States 6% of the gross national product, [1] or over half
a billion dollars per year. Friction is a familiar concept that many people assume is well un-
derstood. Students often learn in high school or introductory college physics that friction can
be described by a simple expression _Ff= mFN, where Ff is the magnitude of frictional force,
m is the (constant) coefficient of friction, and FN is the magnitude of the normal force bet-
ween two surfaces—and that there is a different coefficient of friction for initial motion (i.e.,
beginning at rest) and for two surfaces already moving (sliding friction), with tabulations of
the coefficients of friction available for various pairs of surfaces. However, these relatively
simple concepts—which often fail in practice, because the phenomenological co- efficient of
friction turns out to be a function of the details of the preparation of the two surfaces in con-
tact, the operating conditions, the sliding velocity, and so on—hide the fact that friction is a
very complicated phenomenon, little understood fundamentally, and dependent on processes
taking place at the nano scale.
Experimentally, the development of versions of the surface force apparatus that permitted the
controlled oscillatory sliding motion of two surfaces (typically mica) at measurable gaps of
the order of nanometres opened up the possibility of studying friction and lubrication at the
nano scale [2]. Similarly, around the same time, the ever increasing availability of computing
power made it possible to perform molecular-level simulations of the tribology of nano-
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confined systems [1]. For more details, several recent reviews of various aspects are availa-
ble. [2] In this article, we will focus on a relatively small set of nanotribological experiments
and related theoretical calculations. However, before doing so, we briefly comment on some
applications of nanotribology to provide some perspective on the range of situations encoun-
tered.
Size (nm)
Figure -1: The above figure shows the characteristic dimension of different
MEMS/NEMS system.
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biological sciences due to their existence in many forms [3]. Example of MEMS/NEMS is
given in figure-2.
Recent examples of NEMS devices are sensitive sensors, high frequency resonators and
ultrasensitive low power switches. Molecular gears, motors and nano bearings and engines
are future devices that will be used in medical treatments inside the human body.
MEMS/NEMS devices can be broadly classified into 4 types depending upon factors like
design and contact mode, as shown in table-1. Based on this classification, material failure
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mechanisms can be fracture, creep, tribological issues like stiction, friction, and wear,
delaminating, and other factors like corrosion, pitting and contamination [4].
Table -1. Types of MEMS devices and their description and operating conditions.
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Figure-3: Showing a micro gear unit rotate a very high speed up to 250,000 rpm, thus
resulting damage due to friction and wear.
Electrostatic motors suffer from variety of tribological problems. The intermittent contact at
the rotor/stator interface and physical contact at the hub/flange interface result in friction and
wear. In a micro motor, the rotor is driven electro statically in the stator. Adhesive wear and
abrasive wear often occurs between the rotor and ground plane. Stiction is problem often
occurring between the rotor and stator, rotor and the substrate.
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techniques is to simulate friction and wear in traditional engineering applications with respect
to both size and time scales.
Fcap=4 rπγ
Where r is radius of meniscus, γ is surface tension of water and “R” is radius of ball. This
process occurred in general. The adhesion contributes to friction between surfaces when
operated under low normal forces as in many MEMS. This can mathematically expressed as
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Fa=1.5 πRγ....................................................................................................... (1)
Here γ is the work of adhesion expressed in J/m2 and R is radius of AFM tip.
Mastrangelo and Hsu [10] developed the cantilever beam array (CBA) technique to measure
adhesion taking into account surface roughness. The setup consists of a 20-µm wide array of
cantilever beams that extend from 150-1700 µm in length, and are 2-µm above the surface.
The beam lengths are incremented by 50-µm. These beams are brought into contact with the
underlying surface by electrostatic actuation or by pushing it down with a probe needle. The
surface energy of the S-shaped beam is calculated as:
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At most interfaces of technological relevance, contact occurs at numerous point. It is
impartant to investigate single asperity contact in the fundamental tribological studies as
shown in figure-5.
In the AFM (figure-6), a cantilever tip (radius of about 30 nm, corresponding to a contact area
of _10_15 m2) is passed over the surface of interest; by measuring the deflection of the tip in
both the horizontal and vertical directions, the surface morphology and the friction can be
simultaneously measured. Much of what we know about the rheology of nano confined
liquids comes from the laboratories of Granick and Klein, and we briefly describe them here.
In Granick etal.’s SFA experiments, the lubricant of interest is confined between atomically
smooth, step free single crystals of muscovite mica. Changes in the surface separation are
measured by optical interferometry. Surface forces are applied and the resulting motion
detected using piezoelectric bimorphs. The contact region results from two crossed curved
surfaces; hence, the contact region is circular with a diameter on the order of 100 mm
(corresponding to a contact area of _10_8 m2). The diameter is measured by viewing
flattened interference fringes through an optical microscope. In Klein and Kumacheva’s SFB,
[7] the contact region is also formed by crossed mica cylinders with a contact area
of_10_10m2. The normal and lateral (or shear) forces between the two curved mica sheets are
measured by monitoring the bending of two orthogonal sets of leaf springs. Different types of
AFM tips which is used are given in figure-7.
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Square pyramidal silicon nitride tip square pyramidal single crystal silicon tip
We now briefly review the findings from Granick’s and Klein’s experimental studies. For
nonpolar fluids, such as short alkanes and octamethylcyclotetrasiloxane (OMCTS, which is
approximately spherical with diameter _9 A° ), the low-shear-rate (i.e., Newtonian) viscosity
is many orders of magnitude greater than that of the same fluid in the bulk. Moreover, the
fluid makes the transition to non-Newtonian shear thinning behaviour at strain rates that are
orders of magnitude lower than those of the corresponding bulk fluid. A case in point is
dodecane. The experimental results are from Granick’s group[1] and correspond to six layers
of dodecane confined between mica sheets. Note that the Newtonian viscosity is 6 orders of
magnitude greater than bulk dodecane at the same temperature and pressure, and that
transition to non-Newtonian shear thinning is observed for a strain rates of _103 sec_1,
compared with _1010 sec_1 for bulk dodecane (derived from simulations) at the same
temperature and at a pressure equal to the normal pressure in the confined experiment. As the
transition to non-Newtonian behaviour takes place at strain rates approximately equal to
the inverse of the slowest relaxation time in the system, these results suggest that under nano-
confinement, relaxation times are increasing by many orders of magnitude, perhaps indicating
the onset of an ordered or glassy state. A stronger conclusion is made by Klein, who, for
nano-confined OMCTS, finds a transition from fluid like behaviour (when the distance
between the confining surfaces accommodates seven layers or more of OMCTS) to solid-like
behaviour for six layers or less. ‘‘Solid-like’’ behaviour, in this context, means the existence
of a measurable yield stress, the stress below which no sliding motion takes place. A liquid
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has zero yield stress, as the application of any amount of stress causes flow. The measured
yield stress is Klein’s experiment is less than that of a typical bulk solid, suggesting the
formation of a ‘‘soft’’ solid (or certainly one with a different structure than a bulk). However,
for nano-confined water, strikingly different results are found.[25] Klein’s experiments show
no dramatic increase in viscosity under nano confinement— the increase in viscosity is not
directly measurable, but can be shown to increase by less than a factor of 3. Even at extreme
nano confinement (three water layers), water does not exhibit many orders of magnitude
increase in viscosity nor does it exhibit properties associated with an ordered solid-like phase
(such as sustaining a yield stress). As we shall see below, computer simulations of
nanotribological behaviour exhibit many of the features of the above experiments, and there
has been general structure evolves from a disordered structure over a period of nanoseconds,
and exhibits a nonzero yield stress.
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of magnitude range. Given that the rapid-quench Pt-nano particle- free experiments confirm
his earlier results, Granick concludes that the Pt nano particles do not play a dominant role in
determining the rheology of the nano confined system. Granick also reasserts the absence of
an order–disorder transition in the nano confined fluid, similar to his previous findings. As of
the writing of this article, Klein has not responded in print to the issues raised by Christensen
et al. However, from discussions with Klein and members of his group, it appears that, long
before any questions were raised about Pt nano particle contamination, the Klein group
adopted experimental protocols to minimize the presence of Pt nano particles on their mica
surfaces.
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nanoscale processes involved in lubrication in biological systems (e.g., the lubricants in joints
are predominantly water), as well as utilize the principles of biological lubrication to
engineer biomimetic lubricants.
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[8] Quantification of Friction at Micro-/ Nanoscales
Friction is hard to characterise due to its dependence on chemical, mechanical, environmental
and physical aspects of a material couple. High coefficient of friction must be minimized to
increase the reliability. In nano scopic contacts under low normal forces, adhesion dominates
the friction force. A nonzero friction force was noticed even in the absence of any external
applied normal force. This nonzero frictional force in the contact arises from adhesion .These
observations are in contradiction to empirical Amontons’ law that predicts an infinite
coefficient of friction. The friction force between Pt-coated AFM tip and a mica surface in
ultrahigh vacuum (UHV) varies with load in proportion to the contact area, as predicted by
the JKR theory. The above observation revealed that the adhesion force in contact act as a
additional normal force. The JKR theory was found to fit with the measured friction versus
normal force curve at nano scales. According to JKR theory, the total friction force, Ff, in the
contact and modified Hertzian contact radius, a, are:
Ff =µ ¿
a 3=R/ K ¿
With μ coefficient of friction, L applied normal force, R the radius of contracting body, K the
effective elastic modulus of the material couple,γ the adhesion energy per unit area. The
coefficient of friction increased with decreasing normal force but, when the same friction
force is divided by applied normal force plus the adhesion force, a constant coefficient of
friction was obtained. Therefore, at low normal forces, the coefficient of friction can be
apparent (normal force) and real (adhesion +applied normal force). Adhesion is significant
factor that must be controlled to reduce both stiction and friction force in micro component.
The friction force is increases with increase in true contact area. As true contact area
decreases, the interaction zone between two surfaces becomes small and adhesion reduces. At
low contact pressure in micro component, the roughness greatly affects adhesion and hence
friction.
The measurement of friction with an AFM is known as lateral/ frictional force microscopy
(LFM/FFM).The force sensor in FFM is a micro fabricated cantilever ending with a sharp tip.
The tip is brought into repulsive contact with counterpart. The load is derived from normal
deflection of the cantilever. On sliding, the lateral force acting on the tip is derived from the
twist of the cantilever. Bending and twisting is measured by sensing with laser beam reflected
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on back side of cantilever. Apart from AFM, a surface force apparatus (SFA) is used for
characterising surface interaction at atomic scale. A quartz crystal microbalance (QCM) is
another technique used to measure frictional forces between surfaces and thin absorbed layers
[4]. SFA and QCM are suitable for investigation of tribological phenomenon. Sunderanjan
and Bhushan [1] successfully determined by, AFM, the static friction force encountered in a
surface micro machined micro motor. The AFM tip was pushed against a rotor arm of
micrometer so as to generate lateral deflection. This deflection measured static friction of
micro-meter.
Bhushan [1] successfully characterised the stiction and friction with a digital micro mirror
device (DMD) used in lightweight projection displays.
Figure-8
Figure-8 shows friction profile as a function of normal load for Si (100), where the abrupt
increase in coefficient of friction causes damage of structure.
The quantitative data obtained from FFM measurements do not represent data during real
applications .The contact pressure in FFM are high, namely in the range of GPa, whereas
MEMS have maximum operating pressure of 400MPa. Single asperity contact in FFM
eliminates the effect of roughness and oversimplifies the real contact situations in MEMS.
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LFM/FFM measurement are very sensitive, menticulous calibration of cantilever stiffness
force conversion factor is essential. Same material tested with different lateral force
calibration techniques give rise to different results.
Moreover, nanotribology techniques like AFM, QCM, SFA operate at sliding speeds that are
too slow compared to the typical operating speeds. Large contact size and non isothermal heat
generation, limit the usage of conventional equipment. Coming to analytical models and
atomistic simulation, there is no mean to extrapolate AFM data and to simulate tribological
events at the dimensions and operating conditions of real devices[1].On the other hand,
atomistic simulations are normally performed at sliding speeds above the operating speeds of
MEMS device sin the range of thousands of mm/s[5].
Now new tribological tool developed using micro fabricated devices with a bulk
microstructure, surface topography, and surface chemistry that closely represent real contact
situations in MEMS. Limet al developed a planer surface friction apparatus for measuring
friction at micro scales. This device uses an electrostatic comb drive to move a shuttle
laterally.
This obtained a very high coefficient of friction of 5.9 to 3.9 between polysilicon surfaces,
and 3.5 to 1.5 between polysilicon and silicon nitride tested in ambient air. A continuous
sidewall tribometer was also developed by Senft and Dugger[6], which allow in situ
measurement of kinetic friction between MEMS sidewall contact while operating at realistic
speeds for millions of sliding cycles. The latest addition to characterize friction between
micro machined surfaces is an inchworm tribo meter [1]. The device consists of planer poly
silicon rails that make contact with planner track. This instrument can operate under loads in
the range of µN.
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In wear test performed with AFM, the diamond tip of the AFM cantilever is brought into
contact with counter material at a high normal force and the surface is scratched for a given
period of time. Afterwards, the profile of the scratch mark is scanned with the same tip but
at a light load. There are two scratching methods: line scratching and scanning scratching
[2]. Wear resistance of DLC films is directly proportional to their thickness. AFM is now used
to characterize the wear resistance of SAM monolayer for MEMS/NEMS applications. There
is an example of virgin and treated Si, in which consideration of scratch and wear is given in
figure-9.
Figure-9: this represents the micro scratch tests using a diamond tip in AFM
Machcha proposed another method for measuring the wear at nano scale. This method
relies on 20-30mm deep, micrometer sized indentations made on sliding surface that act as
reference point. This method was used to quantify wear on a contact recording head con-
sisting of diamond like carbon pads used in magnetic hard disk.
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Figure-10: Generating points of friction and wear in bio molecular layer.
The wear resistance of coatings can be measured in terms of coating lifetime by observing
the evolution of friction force with time. To demonstrate the concept of wear and friction,
figure-10 has been given which shows generating points of friction and wear due to
interaction of bio molecular layer on a synthetic micro device with tissues. Let consider an
example of nanotracter, which is friction based MEMS device made of polysilicon material.
For this device, effect of no. of cycle on friction and wear is given on the basis of test.
TEST PROCEDURE
The device can be traversed back and forth (defined as one cycle) by prescribing the number
of steps. To accelerate the wear between the contact surfaces, the device is operated with an
additional normal load of around 100 μN on the leading clamp during its motion. At selected
intervals of wear cycling, static coefficient of friction was measured by conducting a friction
test, where the device is walked to its farthest position against the load spring and held in
place with a large normal force on the leading clamp. The normal force is gradually decreased
until the device starts to slide back towards its zero position due to the tangential force (which
is related to the distance) exerted by load spring. Based on the normal force at which the
device starts to move and the tangential force, friction coefficient can be determined.
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TEST RESULTS
A typical test result showing the travel distance as a function of number of wear cycles is
presented inFig.12. The travel distance decreases gradually until device failure (unable to
move any longer). The coefficient of friction measured during this test is shown in Fig. 13.
The friction values increase gradually from 0.2 to 3 and then decrease back to a steady value
of around 0.45. Careful observation of the features (noise like) in Fig.12 reveals periodic
drops in the travel distance. These intervals correspond to the cycles immediately after the
friction tests. Thus the friction test also appears to strongly influence the evolving surface
conditions. Thus by minimizing the number of friction tests the device life has been extended
to almost 700,000 cycles.
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Figure-13: Evolution of friction coefficient as a function of wear cycle
Surface roughness is not complete solution for addressing adhesion issues because most of
the chemically roughened surfaces react with water vapour and become smooth over the long
term [9]. Apart from this, rough surface gives rise to high local contact pressure thereby lead
to wear in the contact area during operation.
Another way to reduce the problems due to adhesion, friction, and wear is by surface
modification of materials using special coatings or solid lubricants with low surface energy,
low friction, good wear resistance. The coatings applied are typically a few molecular layers
thick and specialy selected such that they do not modify stress state of the poly silicon
substrate .
Diamond has recently emerged as a promising coating thanks to its highest hardness
~100GPa and high elastic modulus ~ 1100GPa. DLC coated surfaces sliding against each
other have very low coefficient of friction between 0.02 and 0.1 compared to silicon surfaces
with coefficient of friction of 0.45-0.6.
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Material Adhesion Micro scale Macro scale Hardness
(nN) coefficient of coefficient of (GPa)
friction using friction using
AFM/FFM pin on disk
fretting
equipment
Silicon Si(001) 50-80 0.004-0.07 0.45-0.6 12
Silicon oxide 35 0.087 0.65-1
Silicon nitride 50 0.06 0.66-0.45 30-50
Titanium 0.16 35
carbide
Diamond like 0.02,0.01 0.08-0.1 90
carbon
Diamond 15 0.01 0.02, 0.05, 0.20 100
0.11
Amorphous 33 0.02 0.11 0.05 0.20 90
carbon
DLC coatings have the disadvantage that their tribological properties are highly depended on
thickness. Thus, DLC coatings can be applied only on components where large component
thickness. The disadvantage of CVD poly-crystalline diamond coating is its high surface
roughness [8]. Most of the ceramic based coatings are deposited using PVD techniques.
Intricate parts of a device remain inaccessible for line-of-sight deposition techniques [8] .
Some typical results of ceramic coatings are listed in table 1.2.
To overcome the problems encountered with hard coatings, research was diverted towards
superhydrophobic organic coatings. These are very thin organic monolayer coatings, either
physisorbed or covalently bound to the surface with water contact angle greater than 90°.
These films are self limiting in thikness and can penetrate through the liquid or vapour phase
to deeply hidden interfaces. There are two types of organic molecules commonly applied on
solid substrates, namely Langmuir-Blodgett (LB) films and self assembled monolayers.
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CONCLUSION
Nanotribology and nan oscale lubrication are fields that are still at an early stage, with ongo-
ing experimental and theoretical controversies. The importance of nanoscale lubrication
fields as diverse as automobiles, hard disk drives, and biology, as well as the difficulty of
simulating and performing experiments on these systems, will ensure that it will continue to
be a very active area of research. Tribological problems are still hindering the future deve-
lopment of contact MEMS/NEMS. A good understanding of surface roughness and true
contact area plays a major role in affecting the friction and wear. Most of the theoretical
models on adhesion and friction are based on the assumptions that surface remains flat.
Analytical solutions and atomistic simulations in tribology are far from real engineering
contact situations. Further development in this area is necessary.
An improvement in laboratory testing tools is also needed. Tools that can operate at contact
pressures, thermal conditions, and sliding speeds corresponding to real application condition-
ns. Limitations from a material point of view must be bypassed.
A major challenge that still has to be tackled is the in depth understanding of the evolution of
material surface properties when two surfaces interact and rub against each other.
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REFERENCES
[1]. B. Bhushan, CRC Handbook of Micro/nanotribology, 2nd edn, 1999, page no. 1-9.
[3]. B. Stark, MEMS Reliability assurance guidelines for space applications, Jet Propulsion
Laboratory, NASA, JPL Publication, 1999, page no. 56-75.
[4]. J. A. Walraven. Failure mechanisms in MEMS/NEMS , ITC Intern. Test Conf. 33.1,
2003, page no. 98-108.
[8]. R. Huber, N. Singer, Out with the old and in with the new, Materials today Jul/Aug
2002, page no. 2-9.
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