Introduction to Semiconductor microfabrication technology
Felix Lu
Introduction to MEMS ECE@ Duke University
Overview
I. Raw materials to wafers
I. II. III. Si refinement from sand Si boule growth techniques Wafer preparation
II.
Doping
I. II. III. Diffusion Oxidation Ion implantation
III.
Material growth and Deposition
I. II. III. Material deposition Epitaxy Wafer bonding
IV.
Device processing
I. II. III. Etching Contacts Device fabrication overview
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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)
Fractional distillation increases purity.
Impurity chlorides
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Silicon refinement from MGS
Electronic grade Si (EGS) ~ 99.999999% pure
SiHCl3+ H2 (g)
Very pure
2Si + 3HCl
Polycrystalline Si
Re-melt and recrystallize into single crystal. Czochralski 2 examples: Float Zone
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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 Quartz ampule GaAs melt
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; FloatZone 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
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Introduction to MEMS ECE@ Duke University
Si wafer process
http://smtbook.com/instructor_guide.pdf
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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 _ (01 1) _ (01 1) 90 90
Si
(100) p-type (100) n-type
Sometimes flat is here
GaAs
90 _ (01 1)
Fall 2005
135 _ (01 1)
1230
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.
Microfabrication Technology
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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
zygo
Optical profilometer
Nomarski differential interference contrast
http://www.zygo.com/?/products/nv6000/
http://www.microscopyu.com/articles/dic/reflecteddic.html
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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
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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) RCA2 (SC2) removes metallic contaminants HCl:H2O2:H2O (1:1:5) Dry
70 C for 10 minutes
oxygen plasma: reactive oxygen ions convert hydrocarbons to CO2 and H2O. UV/Ozone: reactive O3 oxidize hydrocarbons.
Mechanical Ultrasonic megasonic
Small scale mechanical agitation
http://www.techsonic.fr/megatheory.htm
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Doping of Semiconductors
Metals : ~10-7 to ~10-8 Ohmm Resistivity of Semiconductors : ~10-6 to ~107 Ohmm (including semi-insulating III-Vs) Insulators : ~1010 to ~1015 Ohmm
http://www.geokem.com/images/pix/periodic.gif
http://www.astro.virginia.edu/class/oconnell/astr511/lec11-f03.html
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Doping considerations
Doping vs. alloying
~ 1ppm or less Si:P ~.1 99% SixGe1-x
Selective etching of layers and dopant selective etching Mostly for III-Vs 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))
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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
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Thermal oxidation of Si
H2O amorphous SiO2 O2
Diffusion through oxide Reaction with Si Reaction with Si
H2O amorphous SiO2
O2
Diffusion through oxide
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 compressive stress from the substrate. substrate
Top layer is under tensile stress from the substrate.
substrate
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The oxide surface
H HF dipped Si surfaces tend to be hydrophobic :
H termination minimizes water interaction with Si.
H Si
H Si
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) 9195
After Tong and Gsele, 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. Si wafer with oxide mask
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
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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/ELEC2002_11Apr02_3_PDF.pdf
After F. Lu, Ph.D. thesis, (2004)
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Material deposition and growth
deposition amorphous or polycrystalline layer
Contact metal Insulating layer
growth - single crystal layer - epitaxy : MBE, CVD
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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 which form a eutectic with the boat cannot be thermally evaporated.
http://www.haanappel.net/ryan/resume/experiencedielectric.php
Adhesion layers for Au to Si:
Electron beam evaporation
http://www.mpi-halle.mpg.de/~mbe/si.html
Ti, Cr
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Sputtering
What is sputtering? (a.k.a. physical vapor deposition)
Why sputtering? Whats 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 heat up target. - Adhesion of sputtered films is often better. - Deposition is different from evaporation- which is from a point source. - changes in composition easy to do. photoresist or
Layer stoichiometry = target stoichiometry (source) Fall 2005
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Electroplating
Typically to make thick layers of metal (>~1m) 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
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Chemical Vapor Deposition
a.k.a. CVD, VPE, and for III-Vs : 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
Flourescent screen
http://www.ece.utexas.edu/projects/ece/mrc/groups/street_mbe/mbechapter.html
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 Medieval Brain Extractor http://www.ece.utexas.edu/projects/ece/mrc/groups/street_mbe/mbeacronym.html
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Lattice mismatched epitaxy
a1
a2
Misfit dislocation
a2
Separate layers
thickness of epilayer < critical thickness
thickness of epilayer > 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).
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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 Lattice mismatch 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?
If not matched well enough:
high dislocation density at the interface
Si on Insulator (SOI)
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Semiconductor on Insulator
Device layer ~ 1m
Buried oxide (BOX)
High energy particle
eh+
substrate
eeeee-
h+ h+ h+ h+
h+
Radiation hardened High speed circuits
Coupling through the substrate increases RC delay
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Wafer bonding & wafer fusion
Definition:
The permanent attachment of two ultrasmooth surfaces without any kind of glue. Wafer bonding Wafer fusion bonding of two wafers with an oxide inbetween them. 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)
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Bonding chemistry
After Tong and Gsele, Semiconductor Wafer Bonding, John-Wiley & Sons, 1999
After P. Mages, Ph.D. thesis, (2003)
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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 dont want to use the whole wafer.
Artifacts from poor cleaving
Pictures from P. Mages, Ph.D. thesis, 2003
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High thermal stress bonding
After P. Mages Ph.D. Thesis, UC San Diego, 2003
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Low thermal stress bonding
After P. Mages Ph.D. Thesis, UC San Diego, 2003
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Hydrophilic bonding
Cleaning procedure: For Si with thin oxide: Spin cleaning with solvents Dilute HF (1%) dip Modified RCA-1 (1:1:38) For Si with thick oxide: Spin cleaning with solvents Modified RCA-1 (1:1:38)
Si with native oxide : Si with native oxide Si with native oxide : Si with thick oxide (5000 )
Acoustic microscope images of plasma activated bonded Si-OX 4 wafers.
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Bond strength
1.1 m
IR camera
E = Youngs modulus tw = wafer thickness tb = blade thickness L = crack length = bond energy
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Important to measure L accurately since small changes in L = large changes in !
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
Bond strength (mJ/m )
3000 2500 2000 1500 1000 500 0 0 100 200 300
oxygen plasma + RCA1 Oxygen plasma + DI water Argon plasma + DI Water Nitrogen plasma + DI Water
400 500 600
Anneal Temperature (C), 2 hr. in air
From T. Suni, Masters thesis, Helsinki Institute of Tech., (2001)
e et pl t m a is - general concensus : surface co l th th o e s N od ain becomes more porous m xpl e t - water may be trapped in the pores ye
How does plasma activation increase the bond energy so much?
OX
Si Water from oxide surface Water diffuses to gaps during annealing Wet oxidation of Si
OX Si OX Si
Possible model
- wet oxidation of Si wafer to close up gaps increase contact area.
Gaps close
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Layer transfer techniques
Oxygen ion implantation ~1022 cm-2
Bond wafers
Try to Anneal out defects
Grind and polish
SIMOX
Silicon implanted with oxygen
See also http://www.mse.berkeley.edu/~pzhang/MSE225/TICS5GRP7.pdf
BESOI
Bond and Etch back SOI
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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)
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Device processing
Start with layered structure Etching patterns for current and/or optical isolation/confinement
Semiconductor optical waveguide
SOI MOSFET
http://www.compoundsemiconductor.net/articles/magazine/9/ 6/2/1/csbipolar3_6-03
BJT
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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
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Wet etching
Pros
Cheap and easy to set up Can be highly selective Often does not damage substrate
Cons
Can be sensitive to temperature (affects repeatability) Etch rates may be a function of stirring and stirring rate 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:
HF (hydrofluoric acid)
~1200 /min at RT
BOE buffered oxide etch (buffered HF)
Al etchant:
H3PO4: H2O: HNO3 (16:4:1)
Produces bubbles during 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
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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
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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.
Example: etch Si using HNO3:HF:H2O
The nitric acid changes Si to SiO2, and HF etches the SiO2:
Often, CH3COOH is used because it wets the surface better, better wetting results in smoother surfaces.
SiO2 + 6HF
SiF6 + 2H2O
Electrolytic etching, light induced etching Extra electrons speed up reaction
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SiF6 is soluble in water
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Contacts to devices
Purpose: fulfill electrical specs and resist contact degradation. I I
V Ohmic junction
metal isolation Highly doped layer
V Rectifying junction
Metal-semiconductor junction typically rectifying Metal-highly doped semiconductor typically ohmic substrate Backside contact acts ohmic due to large size.
Acts like a lot of resistors in parallel.
Backside contact
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Fabrication of a MOSFET
1. Clean n-Si wafers:
RCA1, HF dip, RCA2, BOE dip.
2. Wet oxidation of Si (~2000 )
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 )
Heat wafers up to 1000 C in ultra pure oxygen.
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MOSFET fab (contd)
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 cant 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 ) 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.
Answer: since youre going to put Al on the backside for a body contact, you can use the backside as a gauge to see when to stop etching the windows.
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