Silicon as mechanical material

Toshiyuki Tsuchiya
Department of Micro Engineering
Kyoto University
 2

Outline
Introduction
Basics of Silicon
Properties of Silicon
Electrical properties
Elastic properties
Thermal properties
Piezoresistive (Electromechanical) properties
Strength & Fatigue

Silicon
 3

Introduction to MEMS
MicroElectroMechanical Systems
"MEMS" means batch-fabricated miniature devices that convert physical
parameters to or from electrical signals and that depend on mechanical
structures or parameters in important ways for their operation.
http://www.wtec.org/loyola/mems/abstract.htm

Integrated device fabricated

using (silicon) micromachining

MEMS
Control
circuit Readout Mechanical
Transducers
circuit structures

Silicon
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MEMS is

Silicon
 5

MEMS everywhere

Silicon
 6

MEMS in automobile

http://www.mstonline.de/microsystems/industrial_applications_I/automotive
http://www.designnews.com/article/13464-Sensors_make_cars_smarter.php
Silicon
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Pressure sensors
Manifold pressure
Barometric pressure
Blake oil pressure
Engine combustion
Fuel tank pressure
Injection pressure
Tire pressure monitor

Silicon
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Basic structure of piezoresistive sensor

Deformable structure against inertia force or pressure

Strain gauge
Placed around the maximum stress position

Silicon
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Automotive pressure sensor

Denso Review
Silicon
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Inertial sensor in car

Accelerometer
Airbag
Antilock brake system (ABS)
Active suspension
Security

Angular rate sensor

Safety (Roll over)
Navigation
Vehicle dynamics control

Silicon
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Capacitive accelerometer
SAE Paper 2004-01-1116

Silicon
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Capacitance change
0: permittivity
2n 0 hlc
DC x 2
w0 d0 : gap
d0 lc : overlap of fingers
n : number of finger

F Mass
(Movable)
Supporting Beam

Anchor

lc
FX

C0+DC- C0+DC+

Fixed-2 Fixed-1 Wiring

Silicon
 13

Angular rate sensorvibrating gyroscope

Coriolis force Fc Velocity V
Coriolis force Fc
Fictitious force Mass m Rotation W

Proportional to Angular rate WVelocity Vmass m

2DOF Vibration system

Vibrating axis: kx
Mass: m Constant vibration
kx frequencyamplitude

W Sensing axis: ky
Detect Colioris force

ky Mass: m

Silicon
 14

MEMS vibrating gyroscope

Tuning fork
U Hyogo

Linear vibration
In-plane rotation
ADI Murata
Out-of plane rotation
Rotational vibration Bosch
In-plane rotation
Out-of plane rotation
Ring vibration NASA/JPL

U Michigan Motorola
Silicon
Silicon as a mechanical material

Question No. 1
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Silicon as Mechanical Material

Silicon is used as mechanical materials in MEMS.
High elastic constant
High yield stress (= strength)
Compatibility to circuit
Well developed fabrication process

New material as structural material

Lack of knowledge as mechanical properties at small scale
Most of materials in ICs are brittle
Si, SiO2, SiN3

Silicon
 17

Polycrystalline silicon (polysilicon, poly-Si)

Analog Devices ADXL Series

1993~

Analog Devices ADXRS150/300

2002~

Silicon
 18

Single crystal silicon

Lateral Accelerometer (Denso) SAE Paper 2004-01-1116

Vibrating Gyro (Toyota Motor) SAE Paper 2004-01-1113

Silicon
 19

What are they making?

Silicon
 20

Si spring in watch

http://www.youtube.com/watch?v=EoTHE
WhhVWQ

http://www.youtube.com/watch?v=MZ9j-MYDs9Y
Silicon
 21

Spiromax silicon spring

http://www.timezone.com/library/rdnotebook/200603208093
Silicon
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Silicon gears for wrist watch

Question No. 2 Proc. MEMS 2004 p. 1-4

Silicon
 23

Silicon
Atomic number14
Atomic weight28.0855
Density2.33103kg/m3
Melting point1420

Silicon occupies 25.8% of earth crust weight.

Earth crust Earth Universe

http://stw.mext.go.jp/data/shuuki2_nophoto.pdf
Silicon
 24

Crystal structure
Lattice constant0.54nm
Diamond structure

Filling factor: 34%

High diffusion coefficient

Silicon
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Si(100)

Silicon
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Si(110)

Silicon
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Si(111)

Silicon
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Manufacturing of Silicon
Reduction of Silica Sand Wafer fabrication flow

Silica sand(SiO2)
Purification
Reduction, Purification

Crystal growth
Crystal growth
FZ (floating zone method)
Cutting
CZ (Czochralski method)
Polishing
Wafer fabrication
Silicon Wafer
Cutting
Polishing
Silicon
 29

Purification to EGS
Raw material: Silica sandSiO2
Reduction of silica sand
SiO2 + 2C Si + 2CO (g) Purity: 98
MGS (Metallurgical grade silicon)

Purification by distillation
Si 3HCl SiHCl3 + H2(g)
Impurities FeCl3, BCl3, PCl3/PCl5
Boiling pointFeCl3, PCl3/PCl5 > SiHCl3 (BP31.8) > BCl3

Decomposition
2SiHCl3 + 2H2(g) 2Si 6HCl
EGS (Electronic grade silicon): poly crystalline

Silicon
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Czochralski method (CZ method)
EGS(+ dopant) -> silica crucible
heated to 1420C in a vacuum
~10 rpm Vacuum chamber

Ar
Seed crystal with known crystal
orientation is dipped to molten Seed

silicon and pulled up quickly in Necking

the beginning and then slowly. Ingot

Diameter depend on the speed melt

Crucible
MCZ method
Graphite
Apply magnetic field to the Heater

molten silicon to suppress

convection flow ~20 rpm
Reduction of oxygen impurities.

Silicon
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Impurities incorporation
Segregation coefficient k0= conc. (in solid)/conc. (in melt)
Dopants k0 < 1Higher concentration at the bottom
Radial distribution caused by rotation
Non uniformity of temperature
AsSbO may evaporate
Oxygen concentration decreases during growth
Amount of melt, convection change, temperature

Dopants k0 Impurities k0
Boron 0.8 Iron 6.410-6
Phosphorus 0.35 Copper 810-4
Arsenic 0.3 Nickel 1.310-4
Antimony 0.023 Gold 2.2510-5
Gallium 0.0072 Oxygen 1.25

Silicon
 32

Floating zone method

Segregation
Same as CZ method Polysilicon ingot
No crucible
Heater is moved along the ingot
Impurities are segregated to the
melting part.
Molten silicon
20kW-cm possible
CZ: 100~1000Wcm
Low impurities
Low strength Heater
Upto 6 inch available
Single crystal
silicon ingot
Doping
Gas flow at melting part(PH3, B2H6)
Neutron radiation: P doping
n + 28Si 29Si 29P+e- Seed crystal
n-type high resistivity silicon
Silicon
 33

Wafer fabrication process

1. Crystal orientation determination using XRD
Axial orientation is defined by seed crystal
Cut by 50cm
2. Orientation Flat or Notch formed: (100) wafer [110] direction for (100)
wafer
3. Cutting
4. Polishing
Using alumina abrasive
Remove damaged layer and surface roughness: 0.1~0.3mm
5. Edge rounding
6. Etching
Remove damage on polishing
7. Anneal
600-800
8. Final polishing
10nm Silica abrasive in alkaline solution
Polish 20m, surface roughness 0.1~0.2nm
9. Inspection

Silicon
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Orientation of wafer
(100) Wafer (110) wafer

(110)

(100)
35.3

Orientation Flat

<110> <110>

Silicon
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Specification of wafers
IC MEMS
Growth method CZ, MCZ, FZ CZ CZ
Conductor type p/(B), n/(P, As) P/Boron P/Boron
Orientation (100), (110), (111) (100) (100)
Misalignment 0.01.0 0.00.2
Resistivity 10m ~ 100 cm 16-24 cm 1-10 cm
Diameter ~12inch (300mm) 1000.5 mm 1000.5 mm
Thickness 100 ~ 675 m 52525 m 38010 m
Surface finish Mirror Mirror
Backside finish Etched Mirror
Flat orientation <110> <110>1.0 <110>0.2
O2 impurities 13-16 ppma 11-15 ppma
Particles <20@0.3 m <20@0.3 m
Silicon
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Deposition of silicon film

Sputtering
Polycrystalline Si target
CVD/Epitaxy
Thermal decompositionSiH4Si+2H2
ReductionSiCl4+2H2Si+4HCl

http://lnf-wiki.eecs.umich.edu/wiki/Low_pressure_chemical_vapor_deposition
Silicon
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Etching (patterning) of silicon

Phase Direction Etching reagent Remark

Liquid Isotropic HF+HNO3+CH3COOH Profile changes by mixing ratio

Liquid Anisotropic Strong Alkaline Sol. KOH, TMAH, etc.

Gas Isotropic XeF2

Gas Isotropic SF6 Reactive ion etching

Gas Anisotropic SF6/C4F8 Bosch process

Silicon
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Microfabrication process

UV light
Photomask

Resist Thin
(photosensitive polymer)
film
Silicon wafer

Silicon
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Microfabrication process

Reactive gas, ions,

plasmas, chemical solutions

Silicon
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Thin film structure by wet etching

Accelerometer DMD
(Analog Deives) (Texas Instruments)
poly-Si thin film structure Al thin film structure

Silicon
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Deep reactive ion etching (DRIE)

100 mm

600 mm 15 mm

Accelerometer
TSV
(Transducers 07)
(through-Si-via)

Silicon
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Bosch process

Silicon
 Issues in Deep RIE
Scallops
J. Micromech. Microeng. 22 045019 (2012)

Loading effect

Footing
Sensors and Actuators A: Physical
114 (2004), 236243

Silicon Black
Journal of Chromatography A
819 (1998) 312
Silicon 43
 44

Anisotropic etching of silicon

Appl. Phys. Lett. 89, 173120

(2006)

Probe

Needle array
Sensors and Actuators A: Physical
Volume 116, pp. 264271

Silicon
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Crystallographic anisotropic etching

3D structure fabrication using etching rate anisotropy for single
crystal materials caused by dependence on crystallographic
orientation.

Reaction
Reaction of silicon to alkaline solution
Si+2OH-Si(OH)2+++4e- (Oxidization)
Si(OH)2+++ 4H2O+4e- Si(OH)6--+2H2 (Reduction)

Mask materials
SiO2
Si3N4
p-type Si

Silicon
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Si Anisotropic Etching

Silicon
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Parameters
Input Output
Etching solution Etching rate
Alkaline materials Direction
Concentration, Temperature Non-uniformity
Etched material In wafer, between wafers
Crystallographic orientation Between batchs
Dopant and its concentration Non-uniformity in the opening
Additives and Impurities Surface roughness
Alcohol (IPA), Surfactant pits
Silicon Micro pyramids
Oxidant Undercutting the mask
Metals
Apparatus
Wafer placement
H2 bubble
Silicon
 48

Mechanism
Relationship to crystal structure
Arrangement of four bonds of silicon in respect to surface
plane is good explanation???
(100)Dangling bond 2, bonded to Si 2
(110)Dangling bond 1, bonded to Si 3
2 of 3 are on the surface plane
(111)Dangling bond 1, bonded to Si 3

There are many mysteries

KOH, TMAH Rate (110) >> Rate (100)
Low repeatability in some case

Silicon
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Etchant for anisotropic etching of Si

KOH TMAH EDP N2H4H2O
Composition KOH solution (CH3)4NH4 H2O 320ml Hydrazine
40% 20~25% solution Ethylene diamine 1l monohydrate
Pyrocathechol 320g
Pyradine 6g

Temperature (C) 60~80 70~90 90~120 80~100

Etching rate(m/min) 0.5~2.0 0.5~1.2 0.3~1.0 1.0~3.0
R(100)/R(111) 400 20 35 50
R(100) vs R(110) R(100) < R(110) R(100) < R(110) R(100) > R(110) R(100) > R(110)
Selectivity to SiO2 250 5000
Alkali metals
Surface roughness
Aluminum tolerance (with Si) (with Si)
Toxicity

Silicon
 50

Etching rate map

KOH 34wt% 70 TMAH 20wt% 70 0.6
1.0
0.3
0.5

0.0 0.0
(mm/min)
(mm/min)

(100) (110) (111) (100) (110) (111)

Orientation KOH 34wt% 70.9 TMAH 20wt% 79.8
(100) 0.629 m/min 0.603 m/min
(110) 1.292 m/min 1.114 m/min
(111) 0.009 m/min 0.017 m/min
Silicon
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KOH 80C (every 20 min)

200mm

Silicon
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TMAH 90C (every 25 min)

200mm

Silicon
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KOH 80C 100min

200mm

40mm
TMAH 90C 125min

Silicon
 54
KOH 80C 20min KOH 80C 120min

400mm

TMAH 90C 25min TMAH 90C 150min

Question No. 3
Silicon
Mechanical Properties
 56

Elastic properties
Strain S as a functions of stress T
S sT
S1 s11 s12 s12 0 0 0 T1
s : compliance matrix
S 2 s12 s11 s12 0 0 0 T2
S1~S3: tensile strain S s s12 s11 0 0 0 T3
S4~S6: shear strain 3 12
T1~T3: tensile stress S4 0 0 0 s44 0 0 T4
T4~T6: shear stress
S5 0 0 0 0 s44 0 T5
S 0 s44 T6
6 0 0 0 0

s11 s12 s44

7.68 -2.14 12.6
unit10-12Pa-1

Silicon
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Elastic propreties (contd.)

Stress T as a functions of strain S
T cS c11 c12 c12 0 0 0
c: elastic constant matrix c12 c11 c12 0 0 0

c c12 c11 0 0 0
c 12
0 0 0 c44 0 0
0 0 0 0 c44 0

0 c44
0 0 0 0

c11 c12 c44

165.7 GPa 63.9 GPa 79.56 GPa

Silicon
 58
Elastic constant of arbitral directions
Compliance s11 for (l,m,n) directions

s11 s11 2s11 s12 12 s44 l 2 m2 m2 n2 n2l 2
Youngs modulus E

E 1 / s11
Poissions ratio

s12 s12 s11 s12 12 s44 l 2l 2 m 2 m2 n 2 n2


s11 s11 2s11 s12 12 s44 l 2 m 2 m 2 n 2 n 2l 2
Shear modulus G
s 44 4s11 s12 12 s 44 l 2 l 2 m 2 m 2 n 2 n 2
1
s 44
G

Silicon
 59

(100) oriented wafer

160 0.3
Si
(100) Ge (100)
140 Si

120
Ge Ge Si
100
0.2

[001]
[001]

80

60
0.1 //
40

20
[010] [010]
0 0
0 20 40 60 80 100 120 140 160
0 0.1 0.2 0.3
Youngs modulus / GPa Poissons ratio

Silicon
 60

(110) oriented wafer

180 0.4
(110) (110)
160

140 Si
0.3
120 Ge

100
0.2
[001]

[001]
80
//
Si

60 Ge

40 0.1

20
[110] Ge Si [110]
0 0
0 20 40 60 80 100 120 140 160 180 0 0.1 0.2 0.3 0.4
Youngs modulus / GPa Poissons ratio

<100>

<110>

Silicon
 61

(111) oriented wafer

In-plane elastic constants
Constant for any in-plane directions

E(111) 168.9 GPa

(111) 0.262

Useful?

Silicon
 62

Elastic constants
Wafer Direction Youngs Direction Poissons
orientation modulus Ratio
(100) <011> 168.9 GPa <011> <0-11> 0.064
(100) <001> 130.2 GPa <010> <001> 0.279
(110) <111> 187.5 GPa <1-11> <1-1-2> 0.182
(110) <100> 130.2 GPa <001> <1-10> 0.279
(111) ----- 168.9 GPa ----- 0.262
J. Appl. Phys. 44 (1): 534-535 (1973).

Temperature coefficientlinear 150K1000K

1 dc11 1 dc12
9.4 10 5 K 1 9.8 10 5 K 1
c11 dT c12 dT
1 dc44
8.3 10 5 K 1
c44 dT
Silicon
 63

Electrical properties
104
Resistivity as a
function of dopant 103

concentration
102

Resistivity (Wcm)
p-type CZ wafer
101

cf. 1 n-type
i-Si:
1.98105Wcm 10-1

10-2

10-3

10-4
1012 1013 1014 1015 1016 1017 1018 1019 1020
Dopant concentration atom/cm3)
Silicon
 64

Electrical properties
Temperature-resistivity relationship (Solid: calcurated, dotted: measured)
n-type (Sb) p-type (B)

Silicon
 65

Thermal properties
300K

Thermal expansion coefficient 2.61610-6/K

Specific heat 0.713 J/g/K
Thermal conductivity 1.56 W/cm/K
Thermal diffusivity 0.86 cm2/s
5
4
CTE(10-6K-1)

3 Measured values
Equation
2
1 3.725 106 1 exp 5.88 103 T 124 5.548 1010T
0
-1
0 500 1000 1500
Temperature (K)
EMIS Datareviews Series No. 24, Properties of Crystalline Silicon, INSPEC, London (1999).

Silicon
 66

For more accurate simulation

Silicon
Elastic Constants 67

ThermalCond

SpecificHeat
TCE Integral Form

TCE Integral Form

0 Zero stress temp.

Databook: differential

Silicon
 68
Electrical Conductivity
Fit to polynominal

Conductivity (pS/m)
Resistivity (cm)

1017

1018

1019

Temperature () Temperture (K)

Electric Cond

Silicon
Current Temperature
12 2000
Simulation 1800
10
with constant properties 1600
Current [mA]

8 1400

Temperature (K)
Measured
1200
6 1000
800
4
Simulation with 600
temperature dependence 400
2
200
0 0
0 2 4 6 8 10 0 2 4 6 8 10
Voltage (V)
Voltage [V]
Displacement
1400

1200 Measured
Displacement [nm]

1000 Simulation with

temperature dependence
800

600

400 Simulation
with constant properties
200

0
0 20 40 60 80 100
Voltage2 [V2]
 70

Strain gauge (piezoresistive effect)

Resistance L Length L a
R
a2

a
Stress, strain at force F
F T F
T 2 2 DL a+Da
a E Ea
Elongation DL L F

Change in width Da a
Resistance change by dimensions
L DL Da
DRS 2 2 R1 2
a L a
Resistance change by piezoresistive effect
: Piezoresistive coefficient
DRP RT RE G: Gauge factor
Resistance change
DR
1 2 E G
R
Silicon
 71
Piezoresistive effect
Ohms law
E I
Resistivity tensor and its change by stress (cubic crystal)
0 0 11 12 13

0
0 12 22 23
0
0 13 23 33
Relationship between and stress (Engineering notation)
11 11 12 12 0 0 0 T1

22 12 11 12 0 0 0 T2
12 12 11 0 0 0 T3 T1~T3: tensile stress
33 T4~T6: shear stress
23 0 0 0 44 0 0 T4

13 0 0 0 0 44 0 T5
0 0 44 T6
12 0 0 0
11, 12, 44: Piezoresistive coefficient of cubic crystal
Silicon
 72

Vector equation of piezoresistive effect

E I I I T I

Each component
E1 I11 11T1 12 T2 T3 44 I 2T6 I3T5

E1 T2
E1 E1 I2
T1 T1 I1 T6
I1
T2
E2 I 2 1 11T2 12T1 T3 44I1T6 I3T4
E3 I3 1 11T3 12 T1 T2 44I1T5 I 2T4

Silicon
 73
Piezoresistive effect Contd.
Piezoresistive effect along (lmn) direction
Tensile stress along gauge axis
F I F

l 11 2 44 12 11 l 2 m 2 m 2 n 2 l 2 n 2
Tensile stress along orthogonal direction (lmn)
F

I
F
t 12 11 12 44 l 2l 2 m2 m2 n2 n2
Shear stress on normal surface along direction (lmn)
F
I

F
s 44 211 12 44 ll 2 mm2 nn2

Silicon
 74

Piezoresistive coefficient of n-Si

unit 10-11m2/N
(100) (110)

t
t

l
l

Y. Kanda, IEEE Trans. Electron Devices Vol. 29, No. 1, pp 64-70 (1982).

Silicon
 75

Piezoresistive coefficient of p-Si

unit 10-11m2/N
(100) (110)

l l

t t

Silicon
 76

Piezoresistive coefficient
unit 10-12m2/N
type (cm) 11 12 44 [direction]
n-Si 11.7 -1022 +534 -46 -1020 [100]
p-Si 7.8 +66 -11 +1381 +930 [111]

l of major direction
100 100 11
110 110 12 11 12 44
111 111 13 11 212 2 44

type (cm) <100> <110> <111>

n-Si 11.7 -1022 -267 -15
p-Si 7.8 66 718 935
Question No. 4
Silicon
Fracture and fatigue of Silicon
 78
Strength
Theoretical tensile strength (Orowan)
m E a0 32GPa
: Surface Energy (
1.2 J/m2 )
E :Young' s modulus (188 GPa 111 )
a0 : Interatomic distance
Theoretical shear strengthFrenkel
m b hG 2 13.7GPa
G : Shear modulus (57GPa 111 )
b :Atomic distance along the silpping
direction on slip plane
h :Interval of the atom row

Silicon
 79

Actual strength
Measured strength 0.6~10 GPa
Stress intensity factor
KI a f

Fracture toughness
KIC = 0.82 MPa/m0.5
for (111) plane-family orientation
Surface defect: a= 0.5mm~

Defect size is not same, distributes

Statistical expression/analysis is required.

Silicon
 80

Weibull statistics
Cumulative fracture probability

Weibull modulus
F 1 exp m VE
Weibull modulus (shape parameter) m Effective Volume
deviation
Effective volume VE
Size effect: Larger specimen fractures at lower stress

Question No. 5
Silicon
 81

Fatigue
Crack propagation rate: Paris Law


= = , =

Initial strength 0 : initial crack size 0
Crack propagates by cyclic stress and fractures at
=

Lifetime model
2 2
0 2
1 = 1
2 0 0

Silicon
 82

S-N curve of silicon

50%RH

Silicon
 83

Silicon vs. Steel

(Denso Technical Review)

But

Si

Stress
Fe

Strain
Silicon has same or better properties
Reliability?

Silicon
 84

To learn more.
Journals
IEEE/ASME Journal of Microelectromechanical Systems
Sensors and Actuators A; Physical (Elsevier)
Journal of Micromachining and Microengineering (IOP)
Journal of Micro System Technology (Springer)
International Conferences
Transducers (International Conference of Solid-state sensors and
actuators)
Every 2 years 2015/6 Anchorage, 2017/6 Kaohsiung, 2019/6 Berlin
http://www.transducers2017.org/
MEMS (Micro Electro Mechanical Systems Conference)
Every years 2016/1 Shanghai, 2017/1 Las Vegas, 2018/1 Dublin
http://www.mems17.org
uTAS (Micro Total Analysis Systems)
MOEMS (Micro-opto Electro Mechanical Systems)
Silicon
 85

Visit Kyoto (University)

Silicon
 86

Fracture of silicon (Prof. K. Sato)

Brittle BDT Ductile

600

Brittle fracture at-50

Component (Ando et al. 2011) Creep observation
size [m] Fracture mode transition
(Nakao et al. 2008) (T. A. Taylor et al. 1972)
10-3
MEMS (D.S. Walters et al. 2000)

Fracture with necking at 500

10-6 (Nakao et al. 2006)

Ductile Slip-line observed at 100 ( Namazu et al. 2002)

10-9
RT Nano-wire: Plastic deformation at RT (Han et al. 2007)
Fracture mode
brittle -100 100 300 500 700 900 1100 1300
less-brittle Temperature []
ductile
Silicon