Saliterman, Fundamentals of BioMEMS and Medical Microdevices, Ch.

2,3

Silicon & Soft

Microfabrication
Erik Johannessen, PhD
MN-BIO4600 Lecture 3
2015
SiliconMicrofabrication
Microfabrication vs. soft fabrication

Microfabrication is the process for the production of

devices in the submicron to millimeter range using
resist coated silicon or other ceramics (CMOS
processing).

Soft fabrication techniques include molding,

embossing, stamping, casting, thick-film application,
self-assembled monolayers (SAMs), and array
patterning using polymers and biological substances.
 Micromachining materials

MEMS devices are made from the same materials used

for microelectronics, including:
Single crystal silicon wafers.
Polycrystalline silicon (polysilicon) for resistive elements.
Gold, aluminum, copper and titanium for conductors.
Silicon oxide for insulation and as a sacrificial layer (to
allow release of moving parts).
Silicon nitride and titanium nitride for electrical insulation
and passivation.

The silicon materials have high strength at small scales

which allows higher strain levels and lower
susceptibility to damage and fracture.
 Soft Fabrication materials

BioMEMS devices employ an increasing factor of soft

fabrication materials, including:
Polymers
Surface modification for improved functionality.
Hydrogels
Environmentally induced changes in shape, size and
other attributes.
Electroactive Polymers
Electrically induced changes in shape, size and other
attributes.
Biological Materials
DNA fragments, biotin labeled albumin, and
streptavidin coated polystyrene beads for example.
Microelectronics Revolution

Fig 1: From radiotubes to integrated circuits.

Silicon

Fig 2: From molten silicon to IC chips.

 Single crystalline silicon growth
The Czochralski process used to obtain single
crystals of a material:
semiconductors (e.g. silicon, germanium and
gallium arsenide)
metals (e.g. palladium, platinum, silver, gold)
salts, and synthetic gemstones.

High-purity, semiconductor-grade silicon is

melted in a graphite crucible.
Dopant impurity atoms such as boron or
phosphorus can be added to the molten silicon
to changing it into n-type or p-type.

A precisely oriented rod-mounted seed crystal

is dipped into the molten silicon.
By precisely controlling the temperature
gradients, rate of pulling and speed of rotation,
it is possible to extract a large, single-crystal,
cylindrical ingot from the melt.
up to 2 metres in length, weighing several
hundred kilograms.

Silicon wafers are cut from the ingot and

polished
200, 300 and 450 mm diameter
Fig 3: The CZOCHRALSKI puller.
 Crystal orientation

Fig 4: Miller indices indicate crystal planes (orientation).

 Excercise

A) B) C)

A wafer is anisotropically wet etched along its <111> crystal

planes. Which one has the <100> wafer orientation?
Enter question text...

a) Ww
b) Ww
c) Ww
A) B) C)

A wafer is anisotropically
wet etched along its <111>
crystal planes.

- Which one has the <100>

wafer orientation?

30 0% 0% 0%
1 2 3 4 5 6 7 8 9 10 11a) 12 13 14 15
b)
16 17 18 c) 19 20
21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40
 Optical Resolution

3 z
R b min s
2 2
 Resist

Positive resist
Opaque regions of the mask protect the resist, and
hence the substrate below.
Radiation fragments polymer backbone.
Shipley S1805, 1818, UV-3.
Negative resists
The transparent regions of the mask protect the resist
(reverse image)
Radiation initiate polymerisation.
SU-8, polyimide, bis(aryl)azide rubber and Kodak KTFR.
E-beam resist (positive)
Poly(methyl methacrylate) - (PMMA)
Critical Dimension
this is the smallest feature to be resolved
Resolution
smallest line width to be consistently patterned.

3 z
R b min s
2 2

Fig 5: Spin coating of photoresist on a silicon wafer.

Schemes for Micro and Nanofabrication

Fig 6: Patterning with photolithography.

Schemes for Micro and Nanofabrication

1. Write Pattern 2. Develop pattern

3. Evaporate metal 4. Perform lift off

Fig 7: Patterning with electron beam lithography.

 Substractive process
Dry etching (plasma)
Glow discharge methods (diode setups)
Plasma etching (PE)
Reactive ion etching (RIE)
Physical sputtering (PS)
Ion beam methods (triode setups)
Ion beam milling (IBM)
Reactive ion beam etching (RIBE)
Chemical assisted ion beam etching (CAIBE)
Deep Reactive Ion Etching (DRIE)
Wet etching (chemical liquids)
Potassium hydroxide (KOH)
Anisotropic etching of silicon
400x <100> plane versus <111> plane
Ethylene diamine and pyrocatechol (EDP)
17x <100> plane versus <111> plane, anisitropic
Does not etch SiO2
Carcinogenic
Tetramethylammonium hydroxide (TMAH)
39x <100> plane versus <111> plane, anisotropic
Does not etch SiO2
Buffered hydrofluoric acid (HF)
Isotropic etching of glass

Fig 8: Isotropic or anisotropic removal of material.

 Additive process
Physical vapor deposition
Thermal evaporation
Sputter coating
Molecular beam epitaxy (MBE)
Atomic monolayers in a single-crystal fashion

Chemical vapor deposition

Plasma enhanced CVD (PECVD)
RF plasma supply energy to the reactant gases
Permit deposition on substrate at low temperature
Atmospheric pressure CVD (APCVD)
Epitaxial films of Si and compound semiconductors
High growth temperature (>850C for Si)
Low pressure CVD (LPCVD)
Large diffusion coefficients at low pressures (< 10 Pa)
Advantage to coat large surface areas (wafer batch)
Atomic layer deposition (ALD)
Sequential dep. of two precursor chemicals
Perrmit film growth down to 1 atomic layer

Doping
Implantation & Diffusion
Oxidation
Growth by thermal oxidation (eg. SiO2)
Screen printing

Fig 9: Screen printing as example

of an additive process.
SOFT Microfabrication
 Soft fabrication methodologies

1. Soft lithography

2. Micromolding

3. 3-D Photopolymerization

4. Smart polymers and hydrogels

5. Nanomedicine techniques

6. Surface assembled monolayers

7. Thick-Film Technologies
Softlithography
 PDMS stamp

Fig 10: Mould of a PDMS stamp from a silicon master.

 Micro-contact printing

Fig 11: Micro-contact printing using a PDMS stamp.

PDMS exclusion moulding

Fig 12: Exclusion moulded structures of PDMS.

Fig 13: PDMS exclusion moulding of a microchannel device.
 PDMS casting

Fig 15: Moulds for PDMS casting.

 PDMS PDMS

PDMS PDMS

Master Master

Fig 3: PDMS casting.

 Microfluidic devices

Fig 14: Fluidic device for separation of ferromagnetic beads.

 UV-ozone surface treatment

Fig 16: Activation of PDMS & glass surface for bonding

to glass, (300 W, 30 Pa, 20 sec).
 Experimental observation

Fig 17: Use of the PDMS microfluidic device under a microscope.

 Mimicking nature

Temporaryadhesive:
Mimickingthefootof
geckos
Nanopillars inPMMAmaster
byebeamlithography
Period400nmx600nm
height
Closecontactwithsurface
(vander Waals interactions)

Permanentadhesive:
Musseladhesiveprotein
Sticktowetanddrysurfaces
Secretedasfluids,undergo
aninsitucrosslinking.
Containscatechols (key
componentofwetadhesive
proteins).

Fig 18: The use of PDMS casting to create

biomimicking structures.
Micromoulding
 Micromoulding

Injection Molding

Hot Embossing

Injection Compression Molding

Thermoforming

AMANDA
 Injection moulding

Fig 18: Injection mould of thermoplastics

 Injection moulding:
Variotherm Process
Means temperature control
Common form of injection molding
Mold evacuated and heated above glass
transition temperature.
Molten polymer injected under pressure
Mould cooled prior to demoulding
Also applicable for metals
Advantages
Complex 3-D architectures

Disadvantages:
Cost (low volume production)
Slow cycle production
Limited product size

Fig 19: Variotherm injection moulding

Hot embossing
Thermoplastic material
Heated to glass transition temperature
Preformed under pressure of 5-10 tons
Mould cooled prior to demoulding
Also applicable for metals

Advantages:
Low polymer flow
Continuous cycle production (low cost)
Definition of small structures
High MW polymers

Disadvantages:
Unsuitable for high aspect ratios
Limited to planar structures
Residual stress

Fig 20: Hot embossing.

Thermoforming
Thermoplastic material
Polymer film placed in mould
Evacuation & clamping of film
Heating above the glass transition temperature
Applied pressure (gas) presses the film against
the mould insert.
Cooling and demoulded
Advantages:
Mass production from film roll (disp. wrapping)
Large product size
Rapid prototyping from a variety of moulds

Disadvantages:
Unsuitable high aspect ratios, sharp corners
Limited to planar structures

Fig 21: Thermoforming.

 AMANDA

Surface micromachining, micro-moulding

and diaphragm transfer
Polymer film deposited and
patterned on silicon wafer
Separate moulded housing structure
Polymer film removed from wafer and
transferred to housing structure
Dicing into individual chips

Advantages:
Low-cost batch fabrication
Integrate pumps, valves and
transducers on chip

Fig 22: Integrated polymer membrane pump manufactured by AMANDA.

3DPhotopolymerisation
 3-D Photopolymerisation

Three-dimensional photopolymerization is based on

layer-by-layer assembly, and is used for rapid
production of devices for modeling and prototyping:

Stereolithography (SL)

Microstereolithography (MSL)

Dynamic Projection MSL

UV curing occurs between 225 and 550 nm.

Free radical or cationic curing mechanisms

 3-D Photopolymerisation
Free radical
Initiation: a photoinitiator (exposed to UV light) breaks down creating
components with an unpaired electron - free radical.
Propagation: the free radical attacks a monomer, takes an electron from
the - bond to form a more stable -bond with the carbon atom. The
remaining electron return to the second carbon atom, turning this into a
free radical and the cycle continues.
Termination: occurs when the growing chain stops by the action of a
contaminant (e.g. O2) producing a radical that is much less active.
Acrylates polymerized by free radicals.

Ionic polymerisation
Initiation: Creation of an active site with a positive/negative charge that
attacks the - bond to form a more stable -bond with the carbon atom.
Propagation: addition of monomers moves the charge down the chain
until termination occurs.
Termination: occurs with an anion-cation recombination or when
monomers exhausted (living polymer).
Epoxies polymerized by cationic curing.
 Stereolithography
Computer driven laser scans a
photocurable resin
Photopolymerisation layer by layer
3-D Structure built from 2-D planes
Parts are fabricated a it moves
through the z-axis focal plane.
After polymerisation the part is
lowered permitting access to fresh
resin.
Materials
Polymers
HDDA - 1,6-hexanediol
diacrylate.
Ceramics
Require a polymeric binding
agent
High temperature sintering
Metals
Direct laser sintering

Spot size/layer thickness

Fig 24: Illustration of a sterielithographic process. 100s micrometer
 Micro-stereolithography
Sub-micron resolution of the
xyz-stages and fine focus UV-
laser spot
Polymerized layers 1-10 m
thickness

Projection MSL
Builds an entire layer at a time
Focused image from a mask

Dynamic mask projection

LCD mask
Rapid layer by layer
polymerisation

Fig 25: Projection MSL (top) and dynamic mask projection (bottom).
MSL Fabricated parts

Fig 26: MSL fabricated parts.

 MSL Fabricated parts

Turbine

Fig 27: MSL fabricated parts.

Smart polymers
 Smart Polymeric Materials

exhibit significant changes in their characteristics with small changes

(external stimuli) in their environment.
 Described in detail by the FLORY-REHNER theory [33,34] and the
FLORY-HUGGINS theory [35,36]:
Reversible soluble-insoluble (SIS) polymers in aqueous media
The swollen phase - dominated by polymer-solvent interactions - best mixing of
the polymer chains and the aqueous solution max value of hydrophilicity
The shrunken phase - determined by polymer-polymer-interactions, which
remove solution out of the gel max value of hydrophobicity
SIS polymers comprise weak acidic and weak basic (ionisable) groups
The phase transition occurs close to the acid dissociation constant which is
mostly identical with the pKa of the ionisable group.

Basic group (e.g. NH2 NH3+)

Protonates in acidic media (NH2 NH3+), basic group acquire postive charge
repulsion between chains, hydrophilic towards solution (counterions) - swelling
Deprotonates in basic media (NH3+ NH2), basic group acquire neutral charge
no repulsion reduced/no interactions with counter ions - shrinking.
Acidic group (e.g. COOH COO-)
Protonates in acidic media (COO- COOH) - neutral charge no repulsion
reduced/no interactions with counter ions - shrinking
Deprotonates in basic media (COOH COO-), negative charge & repulsion
between chains, hydrophilic towards solution swelling
Osmotic pressure
Retention of counterions inside gel matrix increased pressure
Source: Andreas Richter et al., Review on Hydrogel-based pH
Sensors and Microsensors. Sensors 2008, 8, 561-581
 The swelling and shrinking of hydrogels requires a transport of
matter, which is time-consuming
The initiating stimulus has to be transferred into the hydrogel (eg H+) by
continuous mass diffusion
Polymer ionisation
The hydrogel swells or shrinks absorbing or releasing swelling agent.
The polymer chains of the network have to be moved to obtain their new
positions.
Comprising both the solvent diffusion and the net chain motion
cooperative diffusion coefficient Dcoop

Dcoop = cooperative diffusion

DT = stimulus diffusion
DS = mass transfer diffusion
= time constant, swelling process
r = final radius of characteristic
dimension

is increasing with an increasing counter pressure

when employed as sensor/actuator
r kept as small as possible
 The radius of the hydrogel during the swelling process is
expressed as

whereas the shrinking process follows

In this case the characteristic time constant describing a buffer-

mediated diffusion reaction is given by:
= gel thickness,
DHB = diffusivity of the buffer
molecule into the gel
H0 = hydration
gel = buffer capacity of the hydrogel
HB = buffer capacity of the buffer
solution
Source: Andreas Richter et al., Review on Hydrogel-based pH
Sensors and Microsensors. Sensors 2008, 8, 561-581
 Smart polymer applications

Controlled drug delivery

Thermo-responsive microfluidic actuator

Sensors (displacement based pressure/cantilever)

Optical control by fiberoptics at a distance

Tissue scaffolding devices with selective diffusion

Biocompatible coating of implants

Nanomedicine
BioMEMS may be the platform for nanomedicine
technology. Features below 100 nm:

Nanoimprint lithography (NIL),

Laser assisted direct imprint (LADI),

Nanotransfer printing (nTP),

Molecular transfer lithography (MxL),

Atomic force microscopy (AFM) material placement,

Self (surface)assembled
monolayers
 Self-assembled monolayers
(SAMs).
Formed by exothermic interaction of
a surface group with the substrate.
Lateral reordering of side chains/tail
group
Angular tilt maximise van der Waals
interactions

Langmuir-Blodgett
Material monolayer (e.g. lipids) are
floated on an aqueous surface
By dipping the substrate into the
aqueous solution a monolayer of
the floating film is deposited on to
the substrate
Repeating the dipping process adds
layers

Fig 34: SAM assembly and the Langmuir-Blodgett process.

ThickFilm Technologies
 Screenprinting

Incorporation of paste and

colloidal compounds that may be
applied as inks:
Achieving layer thicknesses from
10 to 50 m
Commonly used to fabricate
sensors.

Sol-gel techniques:
Sol: suspended colloidal
solution,
Gel: Transition to a gelatinous
phase
Applied by screen printing in the
gel phase
Sintered into a film coating

Fig 35: Sol-gel technology.

 Summary

Biomedical Micro Electro-Mechanical Systems

Topics of study (curriculum):
Introduction to BioMEMS
Principles of Biochemistry
Silicon and Soft Fabrication Techniques
Polymer Materials
Microfluidic Principles
Sensor Principles and Microsensors
Microactuators and Drug Delivery
Clinical Laboratory Medicine
Micro-Total-Analysis Systems
Detection and Measurement Methods
Genomics and DNA Microarrays
Proteomics and Protein Microarrays
Emerging BioMEMS technologies
Packaging, Power, Data, and RF Safety
Biocompatibility, FDA and ISO 10993
 Thank you

Erik Johannessen, tel: 31009385, eaj@hbv.no