Surfaces in Precision Engineering, Microengineering and Nanotechnology

1 2 3 4
L. De Chiffre (1), H. Kunzmann (1), G.N. Peggs (1), D. A. Lucca (1)
1 2
Technical University of Denmark, Denmark, Physikalisch-Technische Bundesanstalt, Germany,
3 4
National Physical Laboratory, United Kingdom, Oklahoma State University, USA

Abstract
This paper addresses the role of surfaces at the micrometric and nanometric length scales. Applications,
functional behaviour, and manufacturing issues are reviewed with respect to state-of-the-art and emerging
products fabricated using high precision technologies. Examples of surfaces obtained with precision
engineering, microengineering and nanotechnology are presented, encompassing surfaces in computers,
MEMS, biomedical systems, light and X-ray optics, as well as in chemical systems. Surface properties at
micro and nanoscale are considered, including geometry as well as physical and chemical properties.
Different manufacturing processes are reviewed with respect to surface fabrication, encompassing
conventional machining, microfabrication, and nanomanipulation. Surface metrology at micro and nanoscale
is briefly addressed, and its fundamental importance strongly emphasized.

Keywords: surface, precision engineering, microengineering, nanotechnology

The authors thank the following contributors: at micro and nanoscale are considered, including
(* indicates CIRP member) geometry as well as physical and chemical properties. The
paper contains a review of the different manufacturing
P. Bariani, Denmark processes, with respect to surface fabrication,
N.J. Bjerrum, Denmark encompassing conventional machining, microfabrication,
K.D. Bouzakis*, Greece and nanomanipulation. Surface metrology at micro and
E. Brinksmeier*, Germany nanoscale is briefly addressed.
F. Christensen, Denmark
J. Corbett*, UK Table 1 gives a schematic overview of applications,
H.N. Hansen*, Denmark functional behaviour, and manufacturing technologies that
N. Ikawa*, Japan are considered in this work with respect to surfaces.
T. Inamura*, Japan
M.J. Klopfstein, USA A number of keynote papers published by CIRP during the
L. Koenders, Germany last few years [1-5] provide the baseline for the paper.
R. Krger-Sehm, Germany Surface metrology has been the subject of the 2002
J.K. Nrskov, Denmark keynote paper [5] but is not extensively considered in this
M. Tricard, USA paper, though its fundamental importance is emphasized.
K.J. Weinmann*, USA

1. INTRODUCTION Examples of Fabrication

Functions
applications technologies
Surfaces act as interfaces governing the functional
behaviour of a product. Often, the behaviour controlling Computer Optical Machining
mechanisms involve surface details on a micrometre or chips Fluid dynamic Masking
nanometre scale. Many emerging products are based on Data storage Tribological Replication
achieving these small scales, as is the case in precision MEMS Biomedical Deposition
engineering, microengineering, and nanotechnology. Biomedical Mechanical Manipulation
systems Chemical Other
This paper considers the role of surfaces at the Micro-optical Aesthetic
micrometric and nanometric length scales. It contains a systems Other
review of important applications involving surfaces, X-ray optics
considering properties and functional behaviour, as well Fuel cells
as manufacturing issues, with respect to state-of-the-art Implants
and emerging products fabricated using high precision Other
technologies. A number of examples of surfaces obtained
with precision engineering, microengineering and
nanotechnology are presented, encompassing surfaces in Table 1: Examples of applications, functional behaviour,
computers, MEMS, biomedical systems, light and X-ray and high precision manufacturing technologies concerning
optics, as well as in chemical systems. Surface properties surfaces.
 2. SURFACES IN PRECISION ENGINEERING,
MICROENGINEERING AND
NANOTECHNOLOGY
2.1 Surfaces in computers and peripherals
The tremendous impact of computer technology has
become possible because of the progressive downscaling
of integrated circuits and storage devices. The smallest
features of the most modern integrated circuits are
already significantly smaller than 1 m, and the scale
reductions in storage media are equally impressive.
Commercial magnetic storage has now reached a density
of 400 million bits per square centimetre. This
corresponds to a square single-bit size of 500 nm side
length [6]. Considering that the critical dimension for
electronic devices needs to shrink down to 22 nm in the
year 2016, the fabrication of nanostructures has become
a technologically important research area [7].
The magnetic properties of a computer hard disk are
influenced by a surface region several nanometres thick.
In order to minimize head stiction to the disk surface,
surface polishing is followed by a texturing process
producing circumferential grooves or laser texturing, the
overall roughness of the structured surface being Rq = 3-
5 nm [5].
2.2 Surfaces in microelectromechanical systems
(MEMS)
In MEMS devices free-standing micrometre and sub-
micrometre sized structures are realized on the surface of
a polished silicon wafer by bulk or surface
micromachining. These structures are not just the
projection of a two dimensional feature into the depth, but
truly three dimensional [8]. Very often these structures
have to be movable like the cantilever used to support the
seismic mass of an accelerometer or microscale
mechanisms realized by IC compatible processes. MEMS
are characterized by small masses, tight functional
tolerances, smooth surfaces and light loads. Surface
mechanisms are then of tremendous importance in
determining their reliability. A major issue in MEMS is
stiction, as illustrated in Fig. 1. Removal of a silicon oxide
sacrificial layer is accomplished by wet HF etching. During
the subsequent drying operation some shrinking drops
may, due to their surface tension, bend the free standing
polysilicon structure down to the substrate. There, a
permanent adhesion occurs and the device functionality is
compromised, Fig. 1(a). Stiction may also occur at any
time during normal operation, as a result of an overdrive
or handling, Fig. 1 (b). Adhesion forces are indeed often
stronger than ones obtained by actuation. Single
mechanisms and their relative contribution in determining
the total stiction force have been discussed in [8].
Reduction of adhesion and friction forces at interfaces
may be achieved by modifying surface chemistry or
topography. Tribological coatings, well known in the area
of mechanical engineering have an interesting potential
as tribologically optimized surfaces for micro parts.
Important differences exist due to the small offset (0.1-
2m) and the low forces. Current research is focusing on
development of wear resistant surfaces which show
minimized friction and, above all, low stick-slip behaviour.
Nanocoatings of DLC (diamond like carbon), metal
doped-DLC and CNx were demonstrated also to have
excellent wear resistance against abrasive and adhesive
treatments [9]. Self assembled organic coatings have
been proved to eliminate release-related stiction and in-
use stiction, as well as reduce friction in microengines, but
some issues regarding their manufacturability and wear
resistance are not yet solved.
Fig.1: Typical stiction problems in MEMS. (a)
Micromachine stiction during release-etch process; (b)
stiction between overdriven suspended mass
accelerometer and limit stop [8].
Stiction in MEMS is the main problem from an industrial
point of view, while wear debris due to tight clearances and
contact fatigue can be of concern in dynamic devices such
as micromotors.
2.3 Surfaces in biomedical systems
Miniaturization of medical diagnostic tools promise cost
reductions owing to the volume scaled reagents
consumption, time saving (diffusion time dependence),
improved reliability and ease of use. Concepts such as bio
compatibility in implanted chips, bio-recognition, cross
contamination and bio-fouling in analytical systems,
wetting properties and electrophoresis in micro-channels
often determine device success. Ultimately all these
factors depend on interactions at the surface. Recently
there has been a strong trend toward high aspect ratios
structures because they are capable of achieving a higher
active surface area per unit substrate surface area. This is
particularly important for chemical and biomedical
applications, which offer the possibility of higher packaging
densities of microstructural elements and higher
throughput in continuous flow systems. In biomedical
devices, where cells are present, interactions at the
surface involve biologic functional units ranging from water
molecules and small proteins at sub-nanometre size to
cells in the micrometre range. Protein adsorption
mechanisms on a synthetic surface play a fundamental
role in determining cell adhesion [10]. Many
microfabricated diagnostic tools are under development.
Several studies show the possibility of manufacturing
three-dimensional microstructures both in silicon and
polymeric materials to form microprobe arrays [11]. Aspect
ratios up to 100:1 are obtained using the SU-8 photoresist
[12]. In lab-on-chip applications, surface chemistry plays a
double role. In certain areas protein adsorption is highly
desirable, since it mediates cell adhesion and eventually
bio-recognition, on the other hand cell cultures have to be
restricted to some selected regions within the micro-array.
Indeed other pre-selected device zones are sensed to
provide a background signal, and therefore they have to
resist protein adsorption. In other words surface chemistry
is designed and realized to provide the tailored chemical
reactions only where desired. With respect to protein
resistance, a 20 nm thick plasma polymerized tetraglymer
coating layer has been shown to perform satisfactorily as a
control medium [13]. In biochip arrays for DNA analysis
several different single strand DNA segments are attached
to the surface in differentiated locations. Biochemical
response depends on matching the known DNA
fragments with the ones under test. Detector DNA
molecules immobilization must be accomplished in such a
way that surface binding is gentle enough to preserve
their bio-recognition function. Polarization forces at metal
surfaces as well as ionic or covalent interactions on many
metal oxides and semiconductor surfaces may determine
unacceptable loss of specificity. CMOS surfaces are
therefore modified by introduction of space layers and
linker molecules with the aim of preserving specificity and
localization in DNA biochip arrays [10]. At present there is
an increasing trend toward the adoption of polymeric films
and bulk materials in biomedical and chemical
microdevices. This is due to properties such as, for
example: transparency, corrosion resistance or
biocompatibility and the possibility of designing the
material itself as required by the specific application. The
role of the surface is of major importance also with
respect to signal detection in biosensors; reflectivity and
adsorption properties are relevant issues in thin-film
design of optical coatings. Electrophoretic separation of
chemical species is currently achieved in microfabricated
microfluidic devices. Polymer fabricated systems are
under development that are relatively cheap. In these
systems, the wetting properties are of major concern. A
different approach has been followed in programmable
biochips based on SAW actuation which have been
recently presented [14]. Here, instead of trapping the
liquid into microchannels, it is kept into micro-beakers and
transported across the surface of a chip. The surface is
chemically functionalized, see Figure 2, in such a way to
lay down fluidic tracks on the surface, very much like
printing circuits on electronic boards. In this way, specific
regions of the chip can be made hydrophobic or
hydrophilic. The tracks are shaped by lithography [14].
Fig. 2: Sketch of BioMEMS with selective texture for the
generation of droplets having a 20 pl volume. The
diameter of circles on the surface is approximately 30 m
[14].
Therapeutic tools such as implantable biocapsules and
drug delivery systems are the object of extensive
research. Microfabricated pumps for drug delivery
applications are based on actuated silicon membranes.
Fluid compression is achieved by overdriving a
reciprocating membrane. The return motion is due to the
membranes own elasticity. There, the squeeze effect is
limited by texturing one of the contacting surfaces. In
these devices, thermal mismatch due to the difference in
thermal expansion between silicon and silicon dioxide,
has been used to pretension the surface of valves
preventing leakage of strong drugs [15]. Retinal implants
based on CMOS technology have recently been reported
[16]. When adopting a subretinal principle, an electro-
active array of micro-photo diodes convert light into
analogue current which is transmitted to the tissue through
a passivation silicon dioxide layer and electrodes patterned
into a nanoporous TiN layer. This porous layer increases
the contact area by a factor of up to 100. Bioresistance is a
key for this kind of implant which is meant to have lifetime
duration. SEM of in vivo implants showed failure of the
passivation layer and pit corrosion of the silicon
underneath. Therefore the use of other protective layers is
under investigation. Micromachined nanoporous
membranes can be used to create immunoisolation
biocapsules to protect transplanted cells from
immunological attack. A fabrication protocol based on a
thin sacrificial oxide thermally grown and sandwiched
between two silicon structural layers gives membrane
structures with highly defined pore sizes, as small as 10
nm [17]. These were demonstrated to be suitable in
xenotransplantation: the typical dimensions of insulin,
glucose, oxygen and carbon dioxide molecules are below
3.5 nm, while the antibodies are demonstrated to be
retained by a membrane with a pore diameter of 30 nm.
The strict control of pore diameter is of great importance,
since even a small amount of pore diameters over the
nominal cutoff value would allow the passage of antibodies
in sufficient amounts to initiate immunorejection pathways.
An important area is that of implants for medical use,
where the current R&D on surface modifications pointing
toward complex and multifunctional surfaces identifies
three classes: one aiming at optimizing the topography
(pore distributions, roughness, etc.); the second one
focusing on the biochemical properties of surface coatings
and impregnations (ion release, multi-layer coatings,
coatings with biomolecules, controlled drug release, etc.);
and the third one dealing with the viscoelastic properties of
surface materials [18]. The surface is recognized by the
biological system through the combined chemical and
topographic pattern of the surface, and the viscoelastic
properties. In most cases, biorecognition is a central
component. Any attempt to make a sophisticated
functional surface for biointeractions must take into
account the highly developed ability of biological systems
to recognize specially designed features on the molecular
scale [10]. Famous examples are antibodyantigen,
enzyme substrate, and receptor transmitter recognition
(e.g., in cell membranes). The recognition is programmed
into the molecules through the combination of their 3D
topographic architecture, the superimposed chemical
architecture, and the dynamic properties. Consequently an
optimally designed surface for specific biological function
must take these aspects into account. Although the
fundamental interactions occur on the molecular scale
there is an interesting and unique synergistic connection
between the nanometre and the micrometre length scales
when cells are present, as e.g., in the cases of medical
implants, tissue engineering and cell-based bioelectronics.
Recent work in the area of surface modification by
texturing, implantation, and coatings can be found in
references [19-25].
2.4 Surfaces in light and X-ray optics
For general-purpose-research telescopes the description
of the optical quality of the surfaces is normally based on a
specified point spread function and a simple roughness
criterion. There are two types of mathematical
relationships relating surface roughness and other surface
figuring errors to scattering. However, the two basic
expressions are not normally used together. The root-
mean-square (rms) wavefront aberration in terms of
wavelengths is denoted by . For small aberrations, the
fractional loss L of intensity in the central peak of an
image that is close to the diffraction limit is simply related
to the Strehl ratio, that is a measure of image quality [26],
[16]:
2 2 2
L = 1 exp(-(2) ) 4 (1) reflected from the surface is elliptically polarized and, for
As pointed out by Born and Wolf [26], the formula is
derived for low-order (smooth) aberrations. In contrast,
the Total Integrated Scattering S, at normal incidence for
random roughness is given by:
2 2 2
S = 1 exp(-(4) ) 16 (2) were based on reflective optics [34-35] but in recent years
where is the rms surface roughness as deviation from a
mean plane [27]. Expression (1) applies to an optical
wavefront generating an image that is close to the
diffraction limit of resolution. Expression (2) in the form
shown applies to any beam of light in reflectance at
normal incidence. However, in case (2), rms wavefront
errors at normal incidence are equal to 2. We therefore
have = /2. The two expressions give similar results
despite having different origins. With the advent of
advanced design telescopes and recent developments in
polishing technologies, it may be possible to tailor the
characteristics of mirror surfaces to improve the optical
characteristics of an optical element. The major
advantage is that stray light could be managed in a much
more efficient way than currently possible [28] by
engineering the surface. It would be possible, for
example, to direct stray light away from key regions of the
field where maximum contrast is needed to meet the
science requirement.
Surface roughness plays a major role in reflective x-ray
optics. X-rays incident at very shallow angles can be
reflected with high efficiency off smooth metallic or metal-
coated surfaces, for example gold. Such mirrors, with
designs of varying degrees of complexity, are widely used
in x-ray telescopes and other x-ray imaging applications.
In typical applications, an x-ray telescope mirror is made
from glass ceramic material that is highly polished and
coated with metal, or it can be made from nickel
electrodeposited on a mandrel. In practice, such a
telescope receives x-rays from sources in space and they
first strike an annular parabolic surface and are then
reflected on to an annular hyperbolic surface (an optical
configuration developed by Wolter [29]). Frequently, such
surfaces are nested to improve the collecting efficiency of
the telescope. In telescopes with the best angular
resolution the geometry of the individual mirrors is as
close to perfection as possible but this implies a rigid
surface that has a thickness of some millimetres. For
applications where less angular resolution is needed foils
can be used. In both cases the surface texture of the
surface strongly affects the performance of the mirror
because it gives rise to x-ray scatter and therefore
minimizing the surface texture is a vital aspect of the
manufacture of such components. Fortunately, the
improvement between an optical component and an x-ray
component is not the ratio of the optical to x-ray
wavelengths because the x-ray optical component is
operating at grazing incident. It can be shown that a
surface texture improvement of about 25 is needed for the
x-ray case that has been demonstrated to be possible
[30]. A number of researchers have demonstrated
manufacturing and measuring substrates with surface
textures in the region of 0.4 nm Ra was possible in the
1980s [31] and figure accuracies of 0.2 nm are published
today. The very demanding metrology requirements
spawned a significant number of instruments designed to
measure exceptionally smooth surfaces and they were
both of the contacting [32] and the non-contacting [33]
types, such as ellipsometry, where a light beam of known
polarization is incident on the sample. In general the light
very thin coatings, the light will reach the lower interface
and the ellipsicity of the light will be thickness dependent.
The axial angular slope is another key parameter that must
be controlled during manufacture [30] and slopes in the
range of 2 to 5 microradians are required for optics with
good performance. Attempts at making x-ray microscopes
more success was achieved using zone plates, noteably
amplitude zone plates [36] but more recently by phase
zone plates [37-39]. There is much interest in x-ray
microscopes because their resolution is determined by the
width of the outer ring of the zone plate which can be of
the order of 35 nm which is therefore at least 10 times
better than an optical microscope. Moreover, the x-ray
microscope can be used to image intact cells to a depth of
a few micrometres [40-41].The normal type of x-ray
microscope takes an image of the whole specimen at once
but there are scanning variants where the object to be
measured is rastered whilst a picture is built up [42].
Multi-layer based x-ray optical systems represent an
important area. Multi-layer coatings are being used
successfully as beam-forming elements for soft x-ray
applications such as hard x-ray micro-probes [43]. Such
coatings that can be 100 layers thick are arranged in such
a way that reflections add in phase. However, the
thickness of such layers is of the order of 1 to 10 nm thick
and the surface texture must be carefully controlled to the
order of 0.1 nm Ra [44]. Windt et al. [45] point out that it is
very important to specify, and measure within, the surface
wavelength which influences the x-ray reflectivity, in this
-1
case from 1 to 100 m .
Examples of micro-optical systems are the OLED (organic
light emitting diodes), which are illumination sources based
on electrophosphorescent organic thin film layers (less
than 500 nm). Their light extraction efficiency is limited to
20% due to total internal reflection. This limitation is
partially removed when an ordered array of microlenses is
attached to the substrate surface opposite to that of the
OLEDs. Ten micrometre diameter PDMS microlense
arrays fabricated using transfer moulding were
demonstrated to improve external quantum efficiency of an
OLED by 50%. No alignment is required for these arrays
since the microlense diameter is about ten times smaller
than a display pixel [46].
2.5 Surfaces in chemical systems
The surface plays an important role in chemical systems
such as heterogeneous catalysis, fuel cells, etc., since
chemical reactions depend on the amount of active
surface, predominantly on the micrometre to nanometre
scale. Actually, catalysts are today the most important
group of commercial nanomaterials [47-48]. The majority
of industrial catalysts are high-surface-area solids onto
which an active component is dispersed in the form of very
small particles. These have dimensions of 1 to 20 nm and
are often referred to as nanoparticles. Catalysis will
continue to be an important area of nanotechnology since
solutions to many important resource, energy and
environmental problems require new catalysts with tailor-
made nanostructures.
An area involving catalysis which is receiving particular
attention is represented by fuel cells [49]. In a fuel cell,
basically consisting of two electrodes sandwiched around
an electrolyte, oxygen passes over one electrode and
hydrogen over the other, generating electricity, water and
heat. Several kinds of fuel cells have been developed, for
example [49]: Phosphoric Acid (PAFC), Proton Exchange
Membrane (PEM), Molten Carbonate (MCFC), Solid
Oxide (SOFC), Alkaline, Direct Methanol Fuel Cells
(DMFC), Regenerative Fuel Cells, Zinc-Air Fuel Cells
(ZAFC), Protonic Ceramic Fuel Cells (PCFC). As an
example, in PEM fuel cells, the proton exchange
membrane is a thin plastic sheet that allows hydrogen
ions to pass through it. The membrane is coated on both
sides with highly dispersed metal alloy particles (mostly
platinum) that are active catalysts. In PCFC cells,
gaseous molecules of the hydrocarbon fuel are absorbed
on the surface of the anode in the presence of water
vapor, and hydrogen atoms are efficiently stripped off to
be absorbed into the electrolyte, with carbon dioxide as
the primary reaction product. Figure 3 gives an
impression of the role played by the active surface area in
a MCFC cell cathode which is considerably expanded by
a high porosity.
Another important area is that of microchemical sensors,
which has been partially illustrated in connection with
micromedical applications in section 2.3.
Fig. 3: SEM micrograph of modified NiO cathode for
MCFC [50].
3. SURFACE PROPERTIES AT MICRO AND
NANOSCALE
The issue of defining the surface itself has been reviewed
in the 2002 keynote paper [5] emphasizing the fact that a
surface also depends on the measurement technique
used to characterize it, and measurements at different
depths are needed for complete characterization. It is
moreover clear that interactions between geometrical,
physical, and chemical properties take place, and that the
influence from mesoscopic conditions, reaction velocities,
quantum effects, etc. becomes of paramount importance.
3.1 Geometry
A number of aspects among those listed below
differentiate the geometry of high precision surfaces from
the geometry of surfaces of conventional products:
Very fine topographical scales
High aspect ratios
Complex patterns
3D nature with re-entrances
Miniaturised components
Figures 4 and 5 show examples of surfaces on modern
products, where micrometre details govern the functional
behaviour of the surface through the so-called lotus effect
[51]. Figure 6 illustrates the typical dimensions of
structures obtained with different manufacturing
processes, which are, in general, interrelated. Going down
from millimetre to nanometre length scales is not only a
scaling of the size of the material, the nature of the
material itself changes. At distances of some nanometres it
is not only less material which is observed, the material
becomes atomic and discrete in character, i.e., the atoms
of the surface determine the physical and chemical
properties of the surface. On the other side we have to
take into account the atomic steps on surface crystals.
Steps at this scale depend on the treatment of the sample
and represent the surface heights becoming discrete.
Calculations of the roughness of such atomic surfaces
have been produced recently, [52-53].These calculations
take into account the available data of crystals and
knowledge acquired using the bulk values, although the
atoms on the surface show different structures, as
observed by Low Energy Electron Diffraction (LEED) and
Scanning Tunneling Microscopy (STM). The surface atoms
are arranged in such a way that the surface energy is
minimized. Accordingly, on a clean silicon surface of (111)
orientation we see a 7x7 unit cell, whereas on a (100)
surface a 2x1 structure is observed, Figs. 7 and 8. The
meaning of 7x7 is that the surface unit cell is 7 times larger
in the x direction than assumed from the bulk values, see
[54-56].
Fig. 4: A regular surface structure from which the Lotus
effect can be obtained (University of Bonn/Courtesy of the
PTB)
Fig. 5: Lotus effect of paint on glass (Courtesy of the PTB)
 physical state has been extensively treated in two recent
min. height of micro-structures in m keynote papers [5][57], and the critical importance of
hot molding surface and subsurface integrity of ultraprecision surfaces
3000 injection molding
has been documented [57]. As a result of the increasing
2000
need to characterize the mechanical response of surface
1000 regions in the nanometre range, significant efforts in the
min. lateral development of indentation instruments that measure load
dimensions in m
min. height of micro-structures in m versus depth have been made. Nanoindentation has been
3000 X-ray lithography shown to be able to successfully characterise the elastic
optical lithography modulus and hardness of the very near surface of solids
2000
and thin films, and nanoscratching has been employed to
1000 characterise thin film adhesion. The use of
min. lateral
dimensions in m
nanoindentation for the characterisation of the near
min. height of micro-structures in m surface residual stress state has also recently been
3000 discussed [5]. In addition to these measurements,
electrodeposition
micro laser beam nanoindentation has been used to study pop-in [58] - an
2000
cutting abrupt increase in penetration at a given load - which has
1000 been observed in a large variety of materials including
min. lateral
dimensions in m
metals [59] and semiconductors [60-61]. Pop-in is a near
5 50 100 150 200
surface behaviour which has been most commonly
associated with the sudden nucleation of dislocations and
the onset of plasticity [58], [62], although in some cases it
Fig. 6: Height versus lateral dimension of micro-structures has been attributed to oxide layer breakthrough [59].
produced using different fabrication processes (Courtesy Nanoindentation coupled with FEM modeling has been
of A. Weckenmann, University Erlangen-Nurenberg) used to determine the constitutive behaviour of the near
surface [63]. The fundamental nature of near surface
plasticity is also being investigated by nanoindentation and
relates to the fact that for many different crystalline
materials, hardness of the near surface is seen to
decrease with increasing depth. This indentation size
effect is thought to have a physical basis described by
strain gradient plasticity [64], [67] although rate effects are
also thought to play an important role [68].

Unique surface behaviour has also been investigated

Fig 7: STM image of a clean Si (111)- 7x7 surface.
Horizontal range: 20 nm; Vertical range: 15 nm; Z-range
(out of paper): 0.4 nm. The rhombus shows the 7x7
surface unit cell. (Courtesy of the PTB)
Fig. 8: STM image of a 20 nm x 20 nm large part of a
silicon (100) 2x1 surface with an atomic step. The step
height is 0.13 nm. (Courtesy of the PTB)
3.2 Physical properties
The mechanical properties of the surface and near
surface region can play an important role in the functional
behaviour of precision surfaces, e.g., frictional effects in
tribological systems. Characterisation of the near surface
using nanoindentation. For example, the near surface
photoplastic effect (PPE) in II-VI semiconductors [69 - 71],
has been reported. Whereas the PPE has been observed
in bulk single crystal II-VI semiconductors [72] for many
years, only recently has it been observed at the near
surface. Wolf et al. [69] examined the effect of white light
illumination on the hardness of (111)ZnSe.
Nanoindentation was performed using a Berkovich
indenter in darkness and under illumination by a tungsten
2
halogen lamp that produced 50 mW/cm on the surface.
Over the entire depth range (50 nm to 450 nm) an increase
in hardness of approximately 10% was observed. In further
studies by the same group, the spectral sensitivity of the
change in hardness was investigated, again on (111)ZnSe
[70]. The wavelength of the incident light was varied from
470 nm to 585 nm. The largest increase in hardness was
obtained with light of a wavelength of 510 nm, slightly
greater than that representing the band gap of the
material, 480 nm. Recently, Klopfstein et al. [71] studied
the effects of white light illumination on the
nanoindentation response of (0001) etched ZnO for a
depth from the surface of 25 nm to 275 nm. Illumination
resulted in a 40% increase of the load at which pop-in or
the onset of plasticity occurred. Figure 9 shows the
measured hardness as a function of contact depth with
sample illumination and in darkness. In both cases the
indentation size effect, an increase in hardness with
decreased indentation depth, was observed. To a depth of
100 nm the hardness of the illuminated sample was found
to be 7% to 20% greater than that measured in darkness.
Beyond this depth no observable difference in hardness
was found. The increase in near surface hardness with
illumination was attributed to the charging of dislocations
by surface states of the material. The lack of an observed
PPE for indentations with a contact depth greater than 100
nm was attributed to a reduced effect of the surface states
on dislocation charging in this region and insufficient bulk
charging resultant from short dislocation travel distances.
Figure 9: Hardness as a function of contact depth for
etched (0001)ZnO with sample illumination (circles) and in
darkness (squares). Error bars denote maximum and
minimum of the data [71].
In addition to the surfaces of bulk materials, the physical
behaviour of thin films is also of significant interest.
Although there are several techniques used to
characterize the mechanical properties of thin layers on
the order of 100 nm in thickness including for example,
ultra short surface waves [73], nanoindentation has been
successfully used to characterize the mechanical
properties (elastic modulus and hardness) of thin films as
a function of film thickness, growth condition, chemical
composition and residual stress state. For example, the
elastic modulus and constitutive behaviour of electron
beam PVD deposited zirconia have recently been
reported [74]. In another study, the mechanical properties
of sol-gel zirconia deposited on polished disks of 316
stainless steel were measured as a function of film
thickness from 0 nm (as polished) to 900 nm, for different
values of load [75]. Similar work has been done on sol-
gel-deposited titania (TiO2) on glass and copper with
thicknesses from 50 nm to over 200 nm [76], on aluminum
deposited on glass with thicknesses between 240-1700
nm [77], and on sol-gel-derived hard coatings on
polyester [78]. In this last study, the influence of UV
irradiation and low temperature heating on the thickness
and the hardness of the film was reported. The hardness
of the films was evaluated not only as a function of film
thickness but also as a function of the deposition
temperature of the film, since deposition temperature was
shown to be related to the thickness of the TiN and TiCN
coatings [79]. A correlation between the resulting
hardness of silicon oxinitride (SiOxNy) films and
processing temperature has also been reported [80]. The
effects on measured elastic modulus and hardness of the
substrate bias voltage and nitrogen partial pressure in the
deposition of titanium nitride (TiNx) thin films [81], and
vacuum annealing time in the deposition of Mo-Si-N/SiC
[82] have also been studied. The influence of the carbon-
to-nitrogen composition ratio, x, in TiCxN1-x thin films
deposited on cemented carbide substrates on the
mechanical properties including hardness and elastic
modulus has also been reported [83]. In this study,
TiCxN1-x thin films were grown with x=0 (TiN) to x=1 (TiC)
by varying the flow ratio between the reaction gases CH4
and N2. In another study by the same research group, the
mechanical properties of TiCxN1-x thin films deposited on
cemented carbide substrates were measured as a function
of the intrinsic stress on the film as measured by X-ray
diffraction [84]. Investigation into the effects of multilayer
structures of compositionally modulated Ti/TiN films on
their hardness where the modulation periods examined
were 10, 15, 20, and 40 nm has also been reported [85].
Fracture toughness of thin films has been calculated based
on the analysis of the energy release rate from the load-
displacement curve during nanoindentation. For
indentation techniques, radial cracks are produced during
the unloading cycle when brittle materials are indented by
a sharp indenter. The length of radial cracks is known to
correlate with the fracture toughness and is used to
calculate fracture toughness based on various equations
which have been reported [86], [87]. The fracture process
has been shown to progress in three stages [86]: (1) first
ring-like through-thickness cracks from around the indenter
result from high stresses in the contact area; (2)
delamination and buckling occur around the contact area
at the film/substrate interface by high lateral pressure; and
(3) second ring-like through-thickness cracks and spalling
are generated by high bending stresses at the edges of the
buckled film. The same model has been used to study the
fracture toughness of multilayer hard coatings deposited
on cemented carbide [88]. In this study, the changes in
slope of plots of load-penetration depth squared were
shown to reveal the changes of the coating/substrate
system. Two other methods based on correlating crack
lengths emanating from the corners of the indentation
when the indenter and load are removed, and correlating
fracture toughness have been reported [89]. A new
mechanical test, the cross-sectional nanoindentation test,
has recently been developed for measuring fracture
toughness [89]. In this test, indentations are made normal
to the wafer cross-section within the substrate and close to
the interface of interest. From the results of this test a
model based on elastic plate theory was developed to
numerically calculate the interfacial critical energy release
rate [90]. Inputs to the model are the thin film elastic
properties, thin film thickness, interfacial crack area and
maximum thin film deflection during the test. The
interfacial delamination area (crack area) was measured
by optical and scanning electron microscopy. The
maximum thin film deflection during the test can be
obtained from the load versus displacement curves and
the Berkovich diamond-tip geometry assuming that the
indenter shaft does not tilt during the test. The wear
resistance of brittle materials has been shown to be
principally determined by its fracture toughness as well as
elastic modulus and hardness [88].
3.3 Chemical properties
Heterogeneous catalysts are typically multiphase systems
and the structural and chemical states of the active
species depend intimately on process conditions. Particles
ranging in size from roughly 1 to 50 nm exhibit physical
and chemical properties that are intermediate between
those of the smallest element from which they can be
composed (such as a metal atom, the stoichiometric unit of
a metal oxide) and those of the bulk material [48]. Catalyst
performance can be sensitive to particle size because the
surface structure and electronic properties can change
greatly in this size range. Theoretical calculations have
been successfully attempted of adsorption properties,
reaction pathways, and activation energies for surface
chemical reactions [91]. The approach taken in surface
science has been to study elementary reactions on well
defined single crystal surfaces. Single crystal surfaces are
only crude models of the high surface area catalysts used
industrially. Catalysts need to have a high surface area,
and they often consist of a mixture of phases, some of
which have the catalytically active surface, while others
support the small particles of active phases or keep them
from sintering. Recently, it has become possible to
produce and study models of supported catalysts and to
study them under realistic high pressure and temperature
conditions. It was shown that catalysis is decisively
affected by atomic steps on the surface. Fig. 10 illustrates
the fact that chemical activity is tremendously reduced
when surface steps are covered with gold using PVD [92].
Ea = 36 5 kJ/mol
-10
log s0
-11
-12
-13
Ea = 126 21 kJ/mol
-14
0.0015 0.0020 0.0025 0.0030 0.0035
1/T (K-1)
Fig. 10: Dissociative N2 Adsorption on Ru(0001). The
energy Ea required for dissociation increases from 36
kJ/mol to 126 kJ/mol, if surface steps are covered with Au
atoms [92].
Fig. 11: STM image of a Ni(111) surface with 2% of a
monolayer of Au. The Au atoms appear black in the
images. The Ni atoms next to the Au atoms appear
brighter because of a change in geometry and electronic
structure, indicating that the chemical activity of the Ni
atoms may be modified by nearest-neighbor Au atoms
[96].
Through in situ studies, it is possible to obtain a detailed
atomic-scale description of the nanostructures and the
sites where the catalysis takes place, i.e., the active sites
under reaction conditions. In situ methods have been
successfully applied to elucidate the properties of a large
number of heterogeneous catalysts, recently with the
development of a novel high resolution Transmission
Electron Microscope (TEM) with in situ capabilities [92],
[95]. The electrons passing through the sample in the TEM
provide information not only about particle size and shape
but also about the lattice structure and the chemical
composition of individual particles. Also STM and AFM
have been used to examine the nanostructure of model
catalyst systems. Using STM, for example, it has been
possible to explain why the addition of small amounts of
Au to Ni catalysts used for the steam reforming of methane
reduces the tendency of such catalysts to deactivate
because of C deposition [96]. The STM image in Fig. 11
shows Au atoms located on a Ni surface. The presence of
the Au atoms near a Ni atom reduces the tendency of C to
bond to the Ni, and hence to initiate the formation of
carbonaceous deposits that deactivate the catalyst.
4. SURFACE FABRICATION IN PRECISION
ENGINEERING, MICROSYSTEMS AND
NANOTECHNOLOGY
In this section, different manufacturing processes are
reviewed with respect to surface fabrication. The
processes are grouped according to the following three
main areas:
Conventional machining (encompassing precision
engineering material removal operations as well as
EDM and laser machining)
Microfabrication (encompassing silicon micro-
machining as well as polymer replication processes)
Nanomanipulation (encompassing positioning and
manipulation as well as modification and patterning on
micrometre and nanometre scales using localized
tools).
4.1 Machining
A number of processes are particularly relevant for the
manufacture of ultra-precise microstructures: diamond
turning, diamond milling, contour boring (Figure 12), micro
grinding and ultrasonic assisted processes such as
diamond cutting as well as ultrasonic lapping. For the
ultraprecision manufacturing of complex surfaces and
microstructures diamond turning and fly-cutting are
commonly employed. However, for certain tasks these
processes have geometric and kinematic limitations.
Diamond contour boring and ball-end milling extend the
types of surfaces which can be generated to almost
arbitrarily shaped mirror arrays and profiles with high
aspect ratio, being suitable machining methods for the
fabricating of microstructures [57], [97-102].
Fig. 12: Contour boring with half-arc monocrystalline
diamond tool. Left: Details of machining a mould for
lenses; Right: tool details [102].
A number of ultra-precision machine tools has been
developed over the last twenty years in order to meet the
ever growing demand for reduced dimensional tolerances,
together with high surface and subsurface integrity Error!
Reference source not found.. For many industries the
above requirements, coupled with the advent of new
advanced materials, including glasses and ceramics, is
leading to the capabilities of conventional machining
methods and machine tools being eclipsed by new
processes and machine systems currently at the research
stage. The design of these machines is fundamental in
improving machining performance by, for example,
designing for high loop stiffness, the minimalisation of
thermal effects [103] and friction, and the incorporation of
advanced measurement and control systems. In addition,
for highest accuracy, automatic control and software
compensation methods are becoming increasingly
important. Past examples of ultra precision machine tools
include the Large Optics Diamond Turning Machine,
developed at Lawrence Livermore National Laboratory in
the USA [105], and the Cranfield Nanocentre diamond
turning and grinding machine [106] developed in the UK.
More recently, an ultra precision double disk grinding
machine aimed at 'ductile' grinding of 400 mm diameter
silicon wafers, within a flatness of 100 nm has been
developed in Japan [107]. The machine has achieved
extremely high quality ductile mode grinding of the silicon
wafers with very low (sub micron) dislocation damage. A
further recent development has been the realisation, in
the UK, of another ultra precision grinding machine tool
Tetraform 'C'. Tetraform includes a combination of novel
concepts for the design of machine tool structures, which
have been developed to provide a very high dynamic
stiffness, which is required to machine, directly, brittle
materials with extremely low levels of subsurface
damage. The machine utilises a passively damped space
frame, with all loads being carried in closed loops. The
resulting structural design, coupled with the use of
hydrostatic leadscrews and guideways for each axis,
provides very high static and dynamic stiffnesses [108].
Fig.13: Optical quality machining of M50 bearing steel
There is a growing interest in the production of optical
quality surfaces on metallic components, particularly to
control tribological properties. The ability to machine
metallic surfaces to optical quality (< 10 nm Ra) has a
significant impact on both the time and economics of
manufacture, particularly when slow polishing and lapping
processes can be eliminated. However, to achieve
realistic material removal rates the machine tool must
have a high dynamic stiffness. As an example, Tetraform
C has been used to grind M50 bearing steel. Figure 13
illustrates a stepped workpiece where the upper surface
was ground using a 200 m wheel depth of cut and the
lower region a 500 m wheel depth of cut. A 76 m CBN
cup wheel was used in association with electrolytic in-
process dressing (ELID). Wyko plots for both surfaces
demonstrate a measured Ra value of 2.3 nm and 5.4 nm
for each surface [109].
Important research work has been carried out by CIRP
members concerning computer simulation of the
mechanisms involved in chip formation and surface
generation in single crystal nanoscale cutting [110-119].
Manufacturing of lenses by an alternative precision
polishing method called magnetorheological finishing
(MRF) has demonstrated ability to produce optical
surfaces with an accuracy better than 30 nm peak to valley
and surface roughness less than 1 nm on optical glasses,
single crystals (calcium fluoride, silicon), and glass
ceramics [120]. In MRF, see Figure 14, material removal is
accomplished through hydrodynamical forces resulting
from the flow of magnetorheological fluid. In contrast to
conventional polishing, a quasi-solid boundary in the
magnetorheological fluid produces a high shear stress, but
no normal load, resulting in material removal with a
minimum of material damage.
Fig. 14: Polishing mechanism in MRF [120].
Another example of precision finishing, Zeeko's
Precessions polishing process uses a spinning, inflated
membrane tool, which is pushed against the part to create
a variable-sized polishing spot [121-124]. The tool rotation-
axis is precessed to create a near-Gaussian removal-
profile, and the spot traverses the part under control of a 7-
axis CNC machine-tool. A numerical optimiser interprets
measured metrology data and computes the optimum
spot-sizes and dwell-times across the part to minimise
form-errors. Nanometric surface textures are possible
using such a technique with good control of waviness.
Laser micromachining has established itself as a means
for manufacturing of microsystems for various applications
during the past years. These new applications demand for
the quality of micromachined devices combined with more
functionality. The short pulse duration, high pulse energy
and extremely small penetration depth of excimer laser
radiation into irradiated surfaces facilitate the machining of
brittle-rigid materials as ceramics and glass. Another
special characteristic is the large beam profile of this kind
of laser. Thus, it is possible to modify large surface areas
at one time or, by the use of a mask, it is possible to create
many differently shaped structures [116], [125-127].
4.2 Microfabrication
Microfabrication encompasses operations such as
lithography, oxidation, etching, wafer bonding,
electroplating, deposition of silicon wafers, etc. involved in
the micromachining of silicon as well as polymer
replication processing by hot embossing or imprinting,
injection molding, laser ablation, soft lithography, x-ray
photolithography, etc.
Much importance is currently given to solving the stiction
problem during micromachining of silicon for the fabrication
of microsystems. Release related stiction in MEMS can be
minimized by several engineering approaches:
sublimation-drying and supercritical CO2 drying and vapor
HF etching preventing meniscus formation were
successfully applied. Another approach is to perform a
partial undercutting of the surface microstructure and fill
the voids with a polymer layer. Physical surface
modification: the surfaces are roughened to reduce the
effective contact areas, selective etching is typically
employed to change the surface topography [128], [129].
Chemical surface modification methods have been
attempted, including low surface energy plasma
polymerized fluorocarbon film deposited in the field-free
zone of plasma reactors. A more effective chemical
surface modification involves the formation of a self-
assembled monolayer (SAM). Several classes of organic
films have been explored, including alkyl- and
perfluoroalkyl-trichlorosylane SAMs, dichlorosilane- and
alkene-based molecular films. Among these classes of
films, the most widely used is the octadecyltrichlorosilane-
based SAM. Despite the progress made so far, some
crucial issues concerning their manufacturability have not
been addressed yet such as: reproducibility, scale up
from single dies to whole wafers and eventually multi-
wafer cassettes are currently engineering challenges.
Durability of monolayer coatings is still a concern. Non
organic coatings as DLC and Me-DLC films were
fabricated via PECDV methods. The deposition
temperature below 200C has allowed the use of
polymers (SU-8 for instance) as substrate. Adhesion to
the substrate was also proved to be acceptable.
Extensive research work is going on to develop polymer
microdevices, particularly for microfluidic and biomedical
applications.
Process conditions using replica techniques such as hot
embossing, microinjection moulding and soft lithography
of elastomeric polymers should be chosen to take account
of the design of the microstructures to be manufactured.
The critical dimensions that can be replicated by injection
moulding with an acceptable quality are mainly
determined by the aspect ratio of the microstructures
[130]. For aspect ratios lower than unity, these minimal
dimensions reach values in the submicrometre scale, for
example in the manufacturing of CDs. In the case of
higher aspect ratios, the conventional injection moulding
process no longer achieves a sufficient replication quality
mainly because the resin hardens before complete filling
of the mould. By using special microinjection moulding
techniques, polymeric microstructures with minimum wall
thicknesses of 10 m, structural details in the range of
0.2 m and surface roughness of about Rz<50 nm can be
manufactured. The greatest advantage of this approach
consists in the aspect ratios that can reach values up to
20. Hot embossing [131] of high aspect ratio
microstructures requires control over properties such as
sidewall roughness of the embossing master and the
chemical interface between the tool and the polymer. With
respect to friction minimization during the de-embossing
phase, 80 nm rms is an empirical limit for the fabrication
of structures with an aspect ratio larger than 0.5. The
LIGA process and ASE silicon etching allow sidewall rms
values in the order of 10 and 8 nm respectively.
Therefore, they are perfectly suited to high aspect ratio
replication. Addition of release agents to the polymer
allows replication of aspect ratios up to 50. Replica
techniques allow fabrication of polymer independent
components such as fluidic conduits. These elements are
then aligned and assembled with CMOS electronics into
sensors and actuators. Approaches based on parallel
fabrication of aligned electronics and polymer
microstructures have been attempted as well. Lithographic
patterning of polymides and SU-8 are employed to
produce polymer microstructures on a wafer substrate,
using x-ray lithography aspect ratios of 100:1 can be
obtained [12]. Other approaches reported in the literature
are liquid crystal polymers [132], and etching techniques.
Fluoropolymers are inert to most solvents and chemicals,
hence micromachining of these polymers offer great
potential for use in microdevices containing corrosive fluids
or gases. The low surface energy makes the fabrication of
microstructures from these substrates most difficult when
using conventional micromachining techniques. Low
energy ion beam treatments on fluoropolymer surfaces
have been demonstrated to enhance the wetting
characteristics of photoresists with a minimal surface
modification (Rsq 40 nm) [11]. An alternative method using
direct plasma etching has recently been proposed. This
approach is known as deep reactive ion silicon etching
(DRIE). It allows the fabrication of high aspect ratio
structures with a smaller minimum feature size than replica
techniques and the ability to integrate devices with
associated CMOS electronics [133]. MEMS membranes
patterned with polymer lines have been fabricated, with
potential application in microfluidics. Localized stiffening is
achieved due to the polymer lines, making possible the
selective actuation of separate regions of the membrane.
Unfortunately, roughness and footing in the bottom edge of
the polymer microstructure were evident. Thin parylene
films are suitable for manufacturing elastic membranes
owing to its low Youngs modulus and can be used for the
fabrication of check valves in microfluidics. In this
application, gas phase BrF3 is used to roughen the valve
seat surface. This process reduces stiction and surface
tension in the valve by minimizing contact area between
the mating surfaces. The roughened valve seat surface
also leads to enhancement of the adhesion of the parylene
anchors. Surface modification techniques to improve
wetting properties in microchannels are currently being
addressed. As an example sulfunation of PCA micro-
channel surfaces was demonstrated to influence the
electro-osmotic flow as well as surface topography, the
effects of sulfunation lead to a smoother PCA surface and
a significantly higher electro-osmotic flow for pH values
below 8 [134]. Replication has been used for the mass
production of CDs, optical components, as well as
roughness calibration standards [135], to mention some
examples.
As the semiconductor industry progresses towards
extreme ultraviolet (EUV) lithography there is an increased
demand for ultraprecision surfaces with surface roughness
values less than 1 nm. Mirrors for x-ray optics and
synchrotron radiation sources also require nanometre level
peak-to-valley roughness. In addition to surface
roughness, the crystallinity of the near surface may also be
important, e.g., Bragg diffraction optics. A few examples of
the many different physical and chemical processes used
to generate ultraprecision surfaces are discussed below. In
a series of papers Mori et al. [136-138] demonstrated the
use of plasma chemical vaporization machining (CVM) to
achieve nanometre level surface roughness. In plasma
CVM, a plasma is generated between an electrode and the
sample in the presence of a gas, typically helium with SF6,
or CF4 at nearly atmospheric pressure. The shape of
electrodes which have been used include a hollow cylinder
[139], a rotating disk [138], a rotating cylinder [137] and an
inner-diameter saw [136]. Mori et al. [137] claimed that the
removal of material is by the chemical interaction of the
plasma and the sample resulting in no mechanical damage
to the sample. Plasma CVM using a rotating cylinder for
the electrode reduced the surface roughness of a Si wafer
from 2.2 nm P-V to 1.4 nm P-V over a length of 250 m
[137]. The technique has also been used with fused
silica, polycrystalline molybdenum, polycrystalline
tungsten and polycrystalline silicon carbide. Okamoto et
al. [140] demostrated the use of plasma CVM in the
production of amorphous silicon solar cells. They used a
multi-wire electrode to create a series of grooves in the
solar cells which were approximately 30 cm x 40 cm in
size. Solar cells produced with plasma CVM had similar
performance as ones produced by laser patterning.
Elastic emission machining (EEM) is another technique in
which the material is thought to be removed by a chemical
mechanism [141], [142]. The technique has been revised
since first introduced [143]. The elastic sphere previously
used has been replaced by a nozzle that directs ultrapure
water mixed with powder onto the surface. The powder,
SiO2, Al2O3, or ZrO2, reacts with the sample and then is
washed away by the fluid. The technique is very sensitive
to organic impurities and dissolved oxygen in the
ultrapure water which can oxidize the surface of the
sample. EEM was used to reduce the roughness of a
silicon workpiece from 3.2 nm P-V value to 0.98 nm P-V
value for a 21 mm x 25 mm measurement area [142].
The technique has also been used on germanium [141]
and quartz [142].
In contrast to the chemical action of plasma CVM and
EEM, ion beam machining and figuring use the kinetic
energy of ions to remove material. The technique has
been used for the planarization of samples [144] as well
as for the production of an off-axis ellipsoidal mirror [145].
Fechner et al. [144] optimized an ion planarization
technique introduced by Johnson and Ingersoll [146] for
many different materials. In this planarization technique
photoresist was spun onto the workpiece surface with a
spin coater. The photoresist coated workpiece was then
ion milled with the angle of the ion source at the
planarization angle, the angle at which the material
removal rate for the photoresist and the workpiece was
the same. This technique was used to reduce the
roughness of OFHC copper from 24.7 nm rms to 2.95 nm
rms for a 40 m x 40 m measurement area [144]. The
technique was also used to planarize fused silica, CaF2,
silicon, garnet, and electroless nickel. In addition, the
technique was applied to smooth the surface of a 103 mm
diameter CaF2 convex lens with a 248.4 mm curvature.
The roughness at the center of the lens was reduced from
3.38 nm rms to 0.5 nm rms for a 1 mm measurement
length [144]. Because of the curvature of the lens, the
centre was smoother than the outer portions of the lens.
Schindler et al. [147] used ion beam milling without a
planarization film to reduce the roughness of a 200 mm
diameter SiC mirror from 208 nm P-V to 41 nm P-V
measured over the entire mirror surface. The technique
can also be used to machine a specific shape into the
workpiece. Often this is accomplished by inserting a
mask in the path of the ion beam which is then raster
scanned across the part. Mercier et al. [145] used this
technique with a specially designed mask to create an off-
axis ellipsoidal shape from a cube of silica. Further
examples of recent developments in the science and
technology used for the creation of perfect surfaces can
be found in the proceedings of a recent international
conference on production engineering [148].
4.3 Nanomanipulation
Since the invention of scanning tunneling microscopy
(STM) and atomic force microscopy (AFM) nearly two
decades ago, these instruments have been used to
fabricate surface structures ranging from ~100 nm down to
atomic dimensions. Examples of atomic and molecular
manipulation include the positioning of individual atoms on
a surface using low temperature STM, as well as the
removal/deposition of atoms at room temperature due to
electric field or mechanical processes. Experiments that
use such processes to carry out larger-scale material
transfer and/or surface modification include field-
evaporation of hundreds of atoms from Au tips, electron-
stimulated processes in STM chemical vapor deposition,
and miscellaneous mechanical and thermal processes. An
extensive review with more than 200 references on this
area can be found in [151]. STM/AFM nanolithography
ranges from manipulation of single atoms using low
temperature STM (Figure 15) to memory storage using
AFM thermoindentation. The forces between an STM tip
and an adsorbed atom can be used to move the atom to a
new location on the surface. Usually, metal surfaces are
used as substrates because the surface corrugations are
small and, therefore, smaller forces are necessary to move
adsorbed atoms. Unfortunately, the atoms can also more
easily diffuse on such metal surfaces, so STM
manipulation of such atoms is usually done at low
temperatures where thermal diffusion is minimized. STM
can then be used to either laterally move an atom on the
surface, or vertically relocate it by transferring the atom to
the tip and then redepositing it in another location. Another
system where low temperatures are not required for STM
manipulation is the restructuring of atoms on a
semiconductor surface. These experiments are typically
carried out at room temperature and under ultra-high
vacuum conditions to maintain surface cleanliness.
Individual surface atoms can be removed and/or deposited
by direct tip-sample contact, high tunneling currents, or
voltage pulses. Field evaporation occurs when surface
atoms are ionized and extracted by a high electric field.
Fig. 15:Sequence of low-temperature STM images (49 nm
49 nm) showing the construction of a triangular corral
composed of Ag atoms on a Ag(111) substrate [152].
Historically, this process was initially performed using the new fields of observation but also offered hitherto unknown
single-electrode tip geometry of a field ion microscope possibilities to locally influence and transform matter at the
(FIM). More recently, however, evaporation has been level of large atoms, single molecules, and atomic clusters
observed at lower field values using the double-electrode [6].
tip/sample geometry of STM. Because evaporation
usually occurs from the tip (vs. the sample) due to the
higher field there, the choice of tip material is important.
The fabrication of nanoscale structures using STM and
AFM has been a field of relatively active research since
the inception of these techniques. A unique advantage of
these scanning probe techniques is the ability to
manipulate matter down to the atomic level and to form
structures not possible by other means. More recently,
attempts have been made to develop more
technologically interesting structures for use in device
production. Unfortunately, the serial nature of the writing
process makes it time consuming and not economical for
commercial applications. One solution to this problem has
been the introduction of multiple tip arrays. Techniques
such as dip-pen lithography or thermomechanical
indentation are adaptable to such an array geometry and
may eventually yield viable device applications. For
example, in current magnetic data storage the
superparamagnetic effect will ultimately limit room
2
temperature magnetic data density near 100 Gb/in [149]. Wavelength
Thermomechanical data storage using AFM tip arrays has
already demonstrated data densities higher than this limit Fig. 16: Diagram of wavelength vs. amplitude for different
[150]. At present, however, it is still an open question as surface roughness instruments (courtesy of the PTB).
to whether these specialized lithography techniques will
eventually mature into technologies of widespread
application.

5. SURFACE METROLOGY AT MICRO AND

NANOSCALE
Surface metrology has been the object of the 2002
keynote paper [5] and is not specifically considered in this
paper, but its fundamental importance is emphasized.
Metrology is a prerequisite for the success of any modern
production technology, including precision engineering,
micro engineering and nanotechnology.

The present situation concerning surface metrology can

be illustrated with respect to the traceability of surface
topography measurements: Fig. 16 shows the range of
different measuring instruments while Fig. 17 a similar
diagram regarding calibration standards. Comparing the
present possibilities with requirements from production
mentioned in other sections of this paper, the need for
developments in the nanometre range appears clear.
Another clear challenge is the true 3-dimensional
characterization of surface details involving re-entrances,
as discussed in [4] and [5]. In general, the need for
measurement and testing in nanotechnology has been
considered by a position paper compiled by the High
Level Expert Group on Measurement and Testing under
the European Framework Programme for Research and
Development [153]. The report addresses nanometrology
from the following perspectives:
Written standards
Scientific instrumentation
Validated measurement procedures
Measurement standards
Chemical analysis
Biology
In this context, it is also worth remembering that it was
actually the invention of the scanning probing
microscopes during the 1980s, which not only opened up
Wavelength
Fig. 17: Diagram of wavelength vs. amplitude for different
surface roughness calibration standards (courtesy of the
PTB).
6. CONCLUSIONS
Surfaces act as interfaces governing the functional
behaviour of a product, the controlling mechanisms often
involving surface details on a micrometre or nanometre
scale. Many emerging products are based on achieving
these small scales, as is the case in precision engineering,
microengineering, and nanotechnology. This paper,
providing a schematic overview of applications, functional
behaviour, and manufacturing technologies, clearly shows
that the surface properties are of decisive importance for
an increasing number of modern products. Advances have
been made in tailoring surfaces for different high-end
applications. Advances have been made towards better
characterization of surfaces at sub-micrometre levels and
understanding of the mechanisms that involve surface
geometry, together with physical and chemical material
properties. As the scale is reduced, the role of different
mechanisms is affected, and several mechanisms of
different nature may strongly influence each other. Finally,
the fundamental importance of metrology in connection
with surfaces at micrometre and nanometre scales is
strongly emphasized.
7. REFERENCES
[1] Evans, C.J., Bryan, J.B., 1999, Structured,
textured or engineered surfaces, Annals of the
CIRP, 48/2:541-556.
[2] Corbett J., McKeown, P.A., Peggs, G.N.,
Whatmore, R., 2000, Nanotechnology: International
developments and emerging products, Annals of the
CIRP, 49/2:523-546.
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