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Introduction to Semiconductor

microfabrication technology
Felix Lu

Introduction to MEMS
ECE@ Duke University
Overview
I. Raw materials to wafers
I. Si refinement from sand
II. Si boule growth techniques
III. Wafer preparation

II. Doping
I. Diffusion
II. Oxidation
III. Ion implantation

III. Material growth and Deposition


I. Material deposition
II. Epitaxy
III. Wafer bonding

IV. Device processing


I. Etching
II. Contacts
III. Device fabrication overview

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Silicon refinement from sand
• Quartzite sand (silica) is reacted with carbon from coal
(coke) to make metallurgical grade silicon (MGS).
SiO2 + 2C ! Si + 2CO
MGS is ~98% pure trichlorosilane

MGS HCl (g) SiHCl3+ H2 (g)

Impurity Fractional
chlorides distillation
increases
purity.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Silicon refinement from MGS
Electronic grade Si (EGS) ~ 99.999999% pure

SiHCl3+ H2 (g) 2Si + 3HCl

Very pure Polycrystalline Si

Re-melt and recrystallize


into single crystal.

Czochralski
2 examples:
Float Zone

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Single crystal pulling
Czochralski (CZ) technique

Single
crystal Si
boule Seed
crystal
http://en.wikipedia.org/wiki/Czochralski_process

http://lachlan.bluehaze.com.au/usa2003/octob
er2003/16oct2003a/

Molten Si

http://www.isomet.com/FinalWebSite/FOHomePage/FOXtalGrowth.htm

Interaction with the crucible introduces up to ~1018 cm-3 oxygen!


Fall 2005 Microfabrication Technology Introduction to MEMS
ECE@ Duke University
Single crystal pulling
Horizontal Bridgeman
window
Low Temperature furnace (~630 °C) High temperature furnace (~1200 °C)

Stationary tube

GaAs seed
Excess arsenic GaAs melt
Quartz ampule

After T.R. AuCoin and R.O. Savage, in Gallium Arsenide Technology, D.K. Ferry, ed., Sams (1985)

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Single crystal pulling
http://www.tf.uni-kiel.de/matwis/amat/elmat_en/kap_6/advanced/t6_1_3.html

Float Zone
Very pure Si crystals

Melting and purification done at the


same time.

Impurities prefer to stay in the liquid so


solid is very pure, also making hard to
dope uniformly along the length!

T.F. Ciszek, M.R. Page, T.H. Wang, and J.A. Casey; Float-
Zone and Czochralski Crystal Growth and Diagnostic
Solar Cell Evaluation of a New Solar-Grade Feedstock
Source, 29th IEEE PV Specialists Conference New Orleans,
Louisiana May 20-24, 2002

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Si wafer process

http://smtbook.com/instructor_guide.pdf

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Wafer Orientation
for 6” wafers or smaller*
(111) p-type (111) n-type See also, SEMI M1-0302,
http://wps2a.semi.org/wps/portal/_pagr/116/_pa.116/121?docName=P0
01204
(111A) (111B)

45°
_ _ 90° 90°
(01 1) (01 1)
Si GaAs
(100) p-type (100) n-type
Sometimes flat is here

90° 135°

_ _ 1230

(01 1) (01 1) From www.usna.edu/EE/ee452/LectureNotes/05-Processing_Technology/18_Silicon.ppt

After W.R. Runyan and T.J. Shaffner, Semiconductor Measurements & Instrumentation, 2nd Ed., McGraw Hill, 1998.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Single crystal properties of Si

Kurt Petersen, Silicon as a mechanical material, Proc. of the IEEE,


1982, vol. 70, no. 5, pp. 420.
Fall 2005 Microfabrication Technology Introduction to MEMS
ECE@ Duke University
Wafer surface characterization
Dektak

http://www.veeco.com/appnotes/AN526-StylusCap_04065.rf.pdf

Nomarski differential interference contrast


Optical
zygo® profilometer

http://www.zygo.com/?/products/nv6000/

http://www.microscopyu.com/articles/dic/reflecteddic.html

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Temperature and Pressure
measurement
Fabrication involves processes which have to take place in a narrow range of
temperatures and pressures.
Temperature measurement: Peltier/Seebeck junction thermocouple
http://www.electronics-cooling.com/Resources/EC_Articles/JAN97/jan97_01.htm
http://www.picotech.com/applications/thermocouple.html
http://www.omega.com/temperature/Z/pdf/z021-032.pdf

Pressure measurement:
thermocouple Ionization gauge

http://www.lesker.com/newweb/Pressure_Measurement/Thermocouple
http://www.duniway.com/images/pdf/pg/hot-filament-ion-gauge-tube.pdf

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
A sampling of cleaning methods
• Chemical
– Wet
• Pirahna : H2SO4:H2O2 (4:1) [90 °C for 15 minutes]
• RCA (or SC)
– RCA1 (SC1) removes organics and particulates
» NH4OH:H2O2:H2O (1:1:5) 70 °C for 10
– RCA2 (SC2) removes metallic contaminants minutes
» HCl:H2O2:H2O (1:1:5)
– Dry
• oxygen plasma: reactive oxygen ions convert hydrocarbons to CO2 and H2O.
• UV/Ozone: reactive O3 oxidize hydrocarbons.
• Mechanical
– Ultrasonic Small scale mechanical agitation…
http://www.techsonic.fr/megatheory.htm
– megasonic

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Doping of Semiconductors
Metals : ~10-7 to ~10-8 Ohm·m
Resistivity of Semiconductors : ~10-6 to ~107 Ohm·m (including semi-insulating III-V’s)
Insulators : ~1010 to ~1015 Ohm·m
http://www.geokem.com/images/pix/periodic.gif

http://www.astro.virginia.edu/class/oconnell/astr511/lec11-f03.html

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Doping considerations
Doping vs. alloying

~ 1ppm or less ~.1 – 99%


“Si:P” “SixGe1-x”

Selective etching of layers and dopant selective etching


Mostly for III-V’s
Intrisic Si from n+ Si: KOH(40%) at 60 °C and ethylenediamine-pyrocatechol
(EDP)(After G.E. Rittenhouse et al., J. Vac. Sci. Tech., B 10(6), 2860-3 (1992))

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
http://www.occdsb.on.ca/~pop/Music.htm

Why “Si is king”


• SiO2: acts as etching mask, passivation for surface
states, high quality gate insulator.

• III-V oxides : typically unstable.

• GeO : soluble in water!


•Masato Aizawa, Anne M. Cooper, Marek Malac, and Jillian M.
Buriak, Silver Nano-Inukshuks on Germanium, Nano Letters,
VOLUME 5, NUMBER 5, MAY 2005, American Chemical Society

Pictures from http://sinclair.ece.uci.edu

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Thermal oxidation of Si
H2O
O2 H2O
O2
amorphous Diffusion through amorphous
SiO2 oxide SiO2 Diffusion through
oxide
Reaction with Si
Reaction with Si

Si Si

Wet oxidation : faster but dirtier, both from extra oxygen in water.
Dry oxidation: slower but cleaner.
SiO2 is less dense (and amorphous) than Si and so a film of SiO2 of
thickness x0 consumes about 0.45 x0 of Si. [after Mayer and Lau, 1990]

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Wafer bowing
e.g.
oxide

Top layer is under substrate


compressive stress from the
substrate.

Top layer is under tensile


stress from the substrate. substrate

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
The oxide surface
H H H
HF dipped Si surfaces tend to
be hydrophobic : Si Si Si
H termination minimizes water
interaction with Si. Drop of water
on Si surface.
Freshly oxidized Si surfaces
tend to be hydrophilic :
Silanol groups (Si-OH) stick to water.
Joanne Deval, et al., Reconfigurable
hydrophobic/hydrophilic surfaces in
microelectromechanical systems (MEMS), J.
Micromech. Microeng. 14 (2004) 91–95

After Tong and Gösele,


Semiconductor Wafer Bonding,
John-Wiley & Sons, 1999

“mature” oxides can also be hydrophobic


depending on surface chemistry of oxide.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
example
Forming S and D for p-MOSFET.
Predeposition (“predep”)
Anneal BN wafer (which has B2O5) with Si wafer in N2.

oxide mask
Si wafer with
BN
wafer B2O5 http://www.bn.saint-gobain.com

Drive-in
Anneal doped Si wafer with steam and oxygen.

The oxidation over the S


and D, minimize out
diffusion of B.
http://plasticdog.cheme.columbia.edu/undergraduate_research/projects/patricia_wang_project.htm

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Ion implantation

http://bmrc.berkeley.edu/courseware/ICMfg92/images/gif/doping.gif

Implantation of H ions of 50 kV into Si

After
http://humanresources.web.cern.ch/Humanresources/exter
nal/training/tech/special/ELEC2002/ELEC-
2002_11Apr02_3_PDF.pdf

After F. Lu, Ph.D. thesis, (2004)

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Material deposition and growth
“deposition” – amorphous or polycrystalline layer
– Contact metal
– Insulating layer

“growth” - single crystal layer


- epitaxy : MBE, CVD

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Evaporation
Pump down to get a good vacuum.

A good vacuum increases the mean free


path of the evaporant.

Maximize distance between source and target


for more uniform coverage.

Thermal evaporation: materials which have a very high


melting point (comparable to the boat) or materials
http://www.haanappel.net/ryan/resume/experience-
which form a eutectic with the boat cannot be thermally
dielectric.php evaporated.

Adhesion layers for Au to Si:


Electron beam evaporation Ti, Cr

http://www.mpi-halle.mpg.de/~mbe/si.html

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Sputtering
What is sputtering? (a.k.a. physical vapor
deposition)

Why sputtering? What’s wrong with


evaporation?
- some materials are difficult to evaporate.
http://www.ece.utep.edu/research/webedl/cdte/Fabrication/pictures/sputter.htm - low melting point substrates.
- evaporating thick layers quickly may burn photoresist or
heat up target.
- Adhesion of sputtered films is often better.
- Deposition is different from evaporation- which is from a
point source.
Layer stoichiometry = target stoichiometry
(source) - changes in composition easy to do.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Electroplating
Typically to make thick layers of metal
(>~1µm) on top of evaporated and
patterned metals.

http://www.ganoksin.com/borisat/nenam/electroplating-and-electropolishing.htm

V
Unplating biases remove asperities unplating

time

plating

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Chemical Vapor Deposition
a.k.a. CVD, VPE,
and for III-V’s : MOCVD, OMCVD,
MOVPE, OMVPE

http://www.esi-group.com/SimulationSoftware/CFD_ACE/MOVPE.html

http://python.rice.edu/~arb/Courses/Images/360_02_handout9.jpg

PECVD – able to deposit films at much lower temperatures by using a plasma


to “crack” the gas into its components.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
From two Greek words: “epi” = “on” and “taxis” = “arranged”, after John
Orton, “The Story of Semiconductors”, Oxford University Press 2004, p. 6

Molecular Beam Epitaxy


Highly abrupt
interfaces

Effusion cells
http://www.veeco.com/images/mbe_structure.jpg

RHEED
www.sandia.gov/media/NewsRel/NR2000/laser.htm

cryopanels

Appropriate other meanings of MBE:


Mostly Broken Equipment
Massive Beer Expenditures
Maniac Bloodsucking Engineers
Mega-Buck Evaporator
Many Boring Evenings (how do you think this list came about?)
Minimal Babe Encounters (see previous item)
Mainly B.S. and Exaggeration
Flourescent screen Medieval Brain Extractor
http://www.ece.utexas.edu/projects/ece/mrc/groups/street_mbe/mbechapter.html http://www.ece.utexas.edu/projects/ece/mrc/groups/street_mbe/mbeacronym.html

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Lattice mismatched epitaxy
a1

a2
Misfit dislocation
a2

Separate layers thickness of epilayer thickness of epilayer


< critical thickness > critical thickness

• J.W. Matthews, A.E. Blakeslee, “Defects in epitaxial multilayers,” Journal of Crystal Growth, 27, 118 (1974).
• R. People, J.C. Bean, “Calculation of critical layer thickness versus lattice mismatch for GexSi1-x/Si strained-layer
heterostructures,” Applied Physics Lett., 47, 322 (1985).

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Heterogeneous integration
Deposition techniques:
Allow amorphous or polycrystalline material layers on single
crystal substrates.

Crystal growth techniques (MBE, CVD)


Mix and match epilayers of different materials

Thermal expansion coefficient


If not matched well enough:
Lattice mismatch high dislocation density at the interface

Single crystal layer


…but what if you want layers that do not match well with each other for a particular
device?
…or, if you want a single crystal layer on top of an amorphous layer?
Si on Insulator (SOI)
Fall 2005 Microfabrication Technology Introduction to MEMS
ECE@ Duke University
Semiconductor on Insulator
Device layer ~ 1µm High energy particle
Buried oxide (BOX)
e-
h+
substrate
e-
e- h+
- h+
e -e h+
h+
e-
h+

Radiation hardened
High speed circuits

Coupling through the substrate


increases RC delay

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Wafer bonding & wafer fusion
Definition:

The permanent attachment of two ultrasmooth surfaces without any kind of glue.

“Wafer bonding” " bonding of two wafers with an oxide inbetween them.
“Wafer fusion” " bonding of two wafers without an oxide between them.

• Can be used to combine materials


with different lattice constants and
thermal expansion coefficients.
• Can be used to get monocrystalline
layers on top of amorphous layers.
• Applications : SOI, heterogeneous
integration, Si-InGaAs APD, MEMs

P. Mages, Ph.D. Thesis, UC San Diego (2003)

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Bonding chemistry

After Tong and Gösele, Semiconductor Wafer Bonding,


John-Wiley & Sons, 1999

After P. Mages, Ph.D. thesis, (2003)

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Hydrophobic bonding
IR Transmission Si-Si wafer bonded interface
One example of this is bonding a
III-V piece to Si.
III-V piece is ~10× more expensive that Si so we
don’t want to use the whole wafer.

Artifacts from poor cleaving

Pictures from P. Mages, Ph.D. thesis, 2003

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
High thermal stress bonding

After P. Mages Ph.D. Thesis, UC San Diego, 2003

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Low thermal stress bonding

After P. Mages Ph.D. Thesis, UC San Diego, 2003

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Hydrophilic bonding
Cleaning procedure:

For Si with thin oxide: Acoustic microscope images of plasma


activated bonded Si-OX 4” wafers.
Spin cleaning with solvents
Dilute HF (1%) dip
Modified RCA-1 (1:1:38)

For Si with thick oxide:


Spin cleaning with solvents Si with native oxide : Si with native oxide :
Si with native oxide Si with thick oxide
Modified RCA-1 (1:1:38) (5000 Å)

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Bond strength

! 1.1 µm

IR camera

E = Young’s modulus
tw = wafer thickness
tb = blade thickness
Important to measure L accurately
L = crack length since small changes in L = large
" = bond energy changes in "!

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Plasma activation of the surface
plasma activated Si/OX wafers
(30 s, 150 W)
RCA-1(45 s), DI water (2 min)

3500

3000

Bond strength (mJ/m )


2
2500

2000

1500

1000
oxygen plasma + RCA1
500 Oxygen plasma + DI water
Argon plasma + DI Water
Nitrogen plasma + DI Water
0
0 100 200 300 400 500 600
Anneal Temperature (°C), 2 hr. in air

From T. Suni, Master’s thesis, Helsinki Institute of Tech., (2001)

How does plasma activation increase OX


et
e the bond energy so much? Water from
pl t Si oxide
m a is
co l th th - general concensus : surface surface
o de ns OX
N o ai becomes more porous Possible
m xpl Water diffuses
e t… - water may be trapped in the pores Si to gaps during model
ye annealing
OX Wet oxidation of Si
- wet oxidation of Si wafer to close
up gaps ! increase contact area. Si Gaps close

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Layer transfer techniques
Oxygen ion implantation
~1022 cm-2

Bond wafers

Try to Anneal out defects

Grind and
polish

SIMOX BESOI
Silicon implanted with oxygen Bond and Etch back SOI

See also http://www.mse.berkeley.edu/~pzhang/MSE225/TICS5GRP7.pdf

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Unibond® (a.k.a. Smart-Cut®, Ion-cut®)
• Initial motivation
Re-use of expensive wafers.

Thin film of Si on Corning 1737F glass.

http://www.mpi-halle.mpg.de/~waf_bond/cut.html

After F. Lu, Ph.D. thesis (2004)

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Device processing
• Start with layered structure
• Etching patterns for current and/or
optical isolation/confinement
Semiconductor optical
waveguide

http://www.compoundsemiconductor.net/articles/magazine/9/
SOI MOSFET 6/2/1/csbipolar3_6-03

BJT

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Isotropic/anisotropic etching

http://www2.nano.physik.uni-muenchen.de/~schoeff/RR_Web_01/images/Anlagen/RIE/IsotropicEtchPix.jpg

www.memsnet.org/mems/processes/etch.html

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Wet etching
Pros Cons
• Cheap and easy to set up • Can be sensitive to temperature
(affects repeatability)
• Can be highly selective
• Etch rates may be a function of
• Often does not damage stirring and stirring rate
substrate • Can have particulates in solution (may
not be very clean)
• Large amounts of chemical waste

Ambient
temp.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Common etchants in Si processing
Si etchants:
KOH (potassium hydroxide)
TMAH – Tetramethylammonium hydroxide
EDP – Ethyylene diamine pyrocatechol
HF:HNO3:Acetic acid

SiO2 etchant:
~1200 Å/min at RT
HF (hydrofluoric acid)
BOE – buffered oxide etch (buffered HF)

Al etchant:
Produces bubbles during
H3PO4: H2O: HNO3 (16:4:1) etching – shake wafer to
remove bubbles

Etch masks:
photoresist, thermal SiO2, deposited SiOx, SiNx
Source: Kurt E. Petersen, Silicon as a mechanical material, Proceedings of the IEEE, vol. 70, no.5, May 1982, pp. 420

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Dry etching
Chemical and/or physical process using a plasma for etching substrates.

Etch rates: much slower than wet etching

Parallel plate configuration Barrel configuration

Plasma has no
directionality

vertical sidewalls
www.ulvac.com/foundry/index.asp

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Etching mechanics
Etching of single crystal :
– Diffusion
• Movement of etchant to sample surface
– Reaction
• If sample is not directly soluble in etching solution, change it.
– Typically done by oxidizing the surface (e.g. H2O2, HNO3), oxidizing the
sample is another name for removing electrons, or injecting holes.

• Use another component of the etching solution to remove the new


product.
Often, CH3COOH is used because it wets
the surface better, better wetting results in
Example: etch Si using HNO3:HF:H2O smoother surfaces.

The nitric acid changes Si to SiO2, and HF etches the SiO2: SiO2 + 6HF ! SiF6 + 2H2O

Electrolytic etching, light induced etching


Extra electrons speed up reaction SiF6 is soluble in water

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Contacts to devices
• Purpose: fulfill electrical specs and resist contact
degradation. I I

V V
Ohmic Rectifying
junction junction

metal

isolation Metal-semiconductor junction typically rectifying


Highly doped layer Metal-highly doped semiconductor typically ohmic
substrate
Backside contact Backside contact acts ohmic due to large size.
Acts like a lot of resistors in parallel.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
Fabrication of a MOSFET
1. Clean n-Si wafers:
RCA1, HF dip, RCA2, BOE dip.

2. Wet oxidation of Si (~2000 Å)


Heat wafers up to 1000 °C, bubble oxygen
through 95 °C DI water into furnace.
3. Pattern S and D through holes in wet oxide.
Photolithography, cover backside with resist. BOE through the wet
oxide. Result: only front side holes go through to Si.
4. Boron doping of S and D.
Activate Boron Nitride (BN) wafers,
Predep: anneal Si with oxidized BN in N2 at 1050 °C
Drive-in: anneal Si without BN wafer in wet oxygen.

5. Strip off wet oxide.


BOE dip until wafer is hydrophobic.

6. Grow dry (gate) oxide (~1000 Å)


Heat wafers up to 1000 °C in ultra pure oxygen.

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University
MOSFET fab (cont’d)
7. Pattern gate oxide to open up windows for metal to
contact S and D.
BOE dip (since S and D windows are so small, you can’t use the hydophobic test to
see if oxide has etched through), how do you know when to stop?

8. Evaporate Al over front side of wafer. (~1000 Å)

9. Etch Al, leaving only contacts to S and D.


H3PO4:HNO3:Acetic acid – shake the wafer to remove bubbles.

10. Evaporate Al on the backside of the wafer.

11. Anneal Al for good contacts.


450 °C in nitrogen for 10 min.
when to stop etching the windows.
Answer: since you’re going to put Al on the backside for a body contact, you can use the backside as a gauge to see

Fall 2005 Microfabrication Technology Introduction to MEMS


ECE@ Duke University