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Failure of Silicon:
Crack Formation and Propagation
Robert O. Ritchie
Materials Sciences Division, Lawrence Berkeley National Laboratory,
and Department of Materials Science and Engineering
University of California, Berkeley, CA 94720
tel: (510) 486-5798, fax: (510) 486-4881, email: roritchie@lbl.gov
with thanks to
C. L. Muhlstein (Penn State) and E. A. Stach (NCEM, LBNL)
Work supported by the U.S. Department of Energy (Basic Energy Sciences), NEDO and Exponent, Inc.
MEMS,
MEMS,Microsystems
Microsystemsand
andMicromachines
Micromachines
R. Conant, 1999
micron-scale
Schmidt et al, MIT microturbine, moveable mirrors
MCNC/Cronos
microhinge
series of gears
Outline
Outline
• Mechanical properties of silicon
• Suppression/prediction of fracture
Ductile
Ductilevs.
vs.Brittle
BrittleProperties
Propertiesof
ofSilicon
Silicon
• crystal structure
- diamond cubic structure (face-centered cubic)
• brittle-to-ductile transition (DBTT at ~500°C) a = 0.534 nm
Indent went to a
peak depth of 216 nm
diamond sample
indenter
In situ sample geometry
• no phase transformations
• large plastic extrusions of the
In situ TEM holder diamond cubic phase
• dislocation nucleation easier
than phase transformation
Wall & Dahmen, 1997 Minor, Stach, et al., Phys. Rev. Lett.., 2003
Modes
Modes of
of Failure
Failure in
in Silicon
Silicon
• Intrinsic factors
- bond rupture
- plasticity, i.e., mobile dislocations
- defect (crack) population
• Toughening mechanisms
- intrinsic mechanisms (ahead of crack tip)
• microstructure, e.g., second phases
- extrinsic (crack-tip shielding) mechanisms (behind crack tip)
• crack bridging (intergranular cracking)
• microcrack toughening (from dilation and reduced stiffness)
• residual stresses (compressive for toughening)
Brittle
Brittle Fracture
Fracture of
of Silicon
Silicon
transgranular
cleavage
fracture
600 nm
{111} cleavage
{110}
cleavage
σ −σ
P (σ ) = 1 − exp − ∫ dV (
V
ln(ln(1/1-Pf))
) N
u m
F
0 σ o
Kc = Q σF (πac)½
microhardness indent
sharp pre-crack
weakest-link statistics
• Probability of brittle fracture
• composition
MUMPs process - LPCVD reactor* low voltage SEM
uncoated sample
n-type – P doped
deposited Si and PSG layers
thermally annealed at ~900°C
• microstructure
nominal grain size ~100 nm
0.8 MeV TEM
low residual stresses ~ -9 MPa 2 µm unthinned
sample
• mechanical properties
E ~ 163 GPa, ν ~ 0.22 Contaminants
bending strength, σF ~ 3 - 5 GPa 1×1019 atoms cm-3 P
2×1018 atoms/cm-3 H
fracture toughness Kc ~ 1 MPa√m 1×1018 atoms/cm-3 O
6×1017 atoms/cm-3 C
*MCNC/JDS Uniphase/Cronos/MEMSCAP
Muhlstein, Brown, Ritchie, Sensors & Actuators, 2001
Microstructure
Microstructure of
of Polysilicon
Polysilicon Films
Films
Cross-section
Plan view
10
Stress Amplitude (GPa)
2
(110) Notched Silicon Beam
30 ± 0.1ºC, 50 ± 2% Relative Humidity
0
5 6 7 8 9 10 11 12
10 10 10 10 10 10 10 10
Fatigue Life (Cycles)
Muhlstein, Brown, Ritchie, J. MEMS, 2001.
Fatigue
Fatigueof
ofThin
Thin(2(2µµm)
m) Polycrystalline
Polycrystalline
Silicon
SiliconFilms
Films
• Micron-scale polycrystalline n-type Si 600 nm
is susceptible to fatigue failure
• Films can fail after 109 cycles at
stresses of one half the (single cycle)
fracture strength
4
MUMPs 18 SN (pres).QPC
1
Notched Polycrystalline Silicon Beam
Laboratory Air
0
5 6 7 8 9 10 11 12
10 10 10 10 10 10 10 10 • slivers and debris on fractures consistent with
some degree of microcracking
Fatigue Life, N (Cycles)
f
Muhlstein, Brown, Ritchie, Sensors & Actuators, 2001
Fatigue
Fatigueof
ofSingle
SingleCrystal
Crystaland
and
Polycrystalline
PolycrystallineSilicon
SiliconThin
ThinFilms
Films
• transgranular cleavage
cracking from notch
under sustained loads
• some evidence of
secondary cracking and
multiple microcracking
200
150
100
50 2024-T4
Smooth Bar Rotating Beam Fatigue
Templin, et al. (1950)
0
4 5 6 7 8 9
10 10 10 10 10 10
Fatigue Life (Cycles)
200
100
50
• native oxide
thickness ~30 nm
• in fatigue, oxide
thickness at notch
root seen to
thicken three-fold
to ~100 nm
• in sustained
loading, no such
thickening is seen
• temperature measured in
situ at various stresses using
a high-resolution IR camera
• IR camera capable of
detecting ∆T to within mK
with lateral positioning within
microns
• small changes in ∆T of the
<1K resonant mass due to friction
with the air
• notch region shows no
change (<1 K) in ∆T during
the fatigue test
• the observed 3-fold
thickening of the oxide film in
the notch region is promoted
by mechanical rather than
thermal factors
film bulk
SiO2/Si
α = -0.5
β = -0.2
Crack -Growth Rates
Crack-Growth Rates and
and Final
Final Failure
Failure
- small-crack effects
- displacement-control conditions
• interfacial
solutions for a
compliant
(cracked) SiO2
layer on a stiff
silicon substrate
max • crack-driving
force K is f (a,h)
• maximum K is
found at ac/h ~
0.8
KI,o is the interfacial K where a/h = 0.05; h = 100 nm Muhlstein and Ritchie, Int. J. Fract., 2003
Interfacial
InterfacialCrack-Driving Force
Crack-Driving Force
• maximum K at
fracture (a/h) ~ 0.8
KIc ~ 1 MPa√m
• in range of fatigue
failure, where σapp~ 2
to 5 GPa, cyclic-
induced oxidation
required for reaction-
layer fatigue
reaction-layer fatigue
• oxide thickness ≥ 46
nm for failure
KIscc ~ 0.25 MPa√m
at σapp< 5 GPa
no cracking
• oxide thickness ≥ 2.9
fatigue loads nm for crack initiation
at σapp < 5 GPa
• behavior dependent
on reaction-layer
thickness
• bounds set by KIscc
and Kc of the oxide
• regimes consist of:
- no crack initiation in
oxide (K < KIscc)
- cracking in oxide but
no failure (KIscc< K < Kc)
- reaction-layer fatigue
(K > Kc)
silicon lattice