Reliability of Advanced Interconnect

Structures:
New Materials and Length Scale Challenges

Christopher Litteken
Daniel Maidenberg
Sven Strohband
Louise Wang
Eric Guyer

Reinhold H. Dauskardt
(dauskardt@stanford.edu)

Work supported by the DOE, SRC, MARCO, and ATP Dept. of Commerce.
Industry support from INTEL, IBM, TI, AMAT, JSR, Hitachi Chemical.
Mechanical Reliability of Thin-Film Interconnect Structures

Issues:
• Measurement of thin-film adhesion
• Subcritical debonding (moisture,
temperature, mechanical fatigue)
• Relationship to processing and
composition (interface chemistry and
morphology, surface treatment, seed layers)
debonding • Integration of new materials
• Simulation and reliability modeling
1 µm
applied mixed mode K-field
Device (KI, KII)

elastic
Solder Interconnect Polymer Underfill
cohesive zone elastic
layer
Substrate (Ceramic or Polymer)
plastic
ductile layer zone
100 µm
Multi-Scale
elastic substrate
Simulations
BC domain dia 25 – 50 µm
 Outline
• Adhesion and Fracture Involving Brittle Dielectric Layers
– barriers and dielectrics in interconnect structures (TiN, TaN, SiNx, SiO2)
– new low-k dielectric materials (e.g. CDO, MSSQ, SiLK, porosity)

• Moisture and Implications for CMP

– moisture assisted subcritical debonding
– kinetic models and understanding

• Multi-Scale Simulations of Adhesion

– interface cohesive zones and plasticity in ductile layers
– barrier layer stiffness, thickness and effects of pre-stressed thin films

• Patterned Structures
– elastic constraint and stress state
– effect of line geometry
 Interface Fracture Resistance and Reliability

Adsorbed Elastic Layer Fracture Process

layer Zone, Go

Surface Barrier
Roughness, λ Plastic Zone Layer, hb
Ductile Layer, hD

Elastic Substrate
Of interest….
• New materials
Interface Fracture Energy • brittle glasses
• ductile polymers
interface chemistry • porosity (density)
• Length scales effects
Gtotal = Go + Gzone • mechanical properties
• adhesion
frictional contact
• 1-D, 2-D, complex
ductile adjacent layer
structures
 Thin-Film Adhesion Testing
Environmental
Low Profile Test Frame Chamber
(use with microscopy)

Thin films sandwiched between elastic substrates

4-pt. Delaminator Tool

Subcritical Debonding
Interface Fracture Energy, Gc (J/m2)

Delamination Resistance (temperature and moisture effects)

Debond Growth Rate, da/dt (m/s)

12.0 10-3

10-4 Ta
8.0 m ~ 80
-5
10

10-6
4.0

da
TaNx
10-7 = C Gm m ~ 14
dt
0.0 10-8
Ta
1.00
TaN 1 10
Sample Type Debond Driving Force, G (J/m2)
Lane, Krishna, Hashim, Dauskardt - J. Mater. Res. 15 [1] 2000
 Research Activities in Low K Materials
Dielectric
Material Class Feature Examples Constant
Silica (SiO2) Silicon dioxide glass Thermal 3.9 – 4.1
TEOS
Modified Silica Fluorinated silica CVD fluorinated silica (FSG) 3.5
Carbon doped silica SiCOH < 3.0
Porous Silica Nanoporous silica Aerogel 1.0 – 3.0
Zerogel

Inorganic Polymer Organically modified Polysilesquioxanes (SSQ) 2.5 – 3.5

silicate
Porous Hybrids Phase separated PCL/SSQ hybrids 2.3 – 3.0
organic/inorganic

Organic Polymers Fluorinated and non- Polyimide, parylene and 1.8 – 3.5
fluorinated polymers polynaphthalene families
Benzocyclobutene (BCB) 2.7
Aromatic Hydrocarbon (SiLK) 2.6
Amorphous carbon films 2.7 – 3.5
 Effect of Carbon Doping on Adhesion of CDO
10
8.5
Cu 9

Interface Fracture Energy Gc (J/m )

2
Sample Set 2
8
Sample Set 1
SiNx
7
5.57 5.35
CDO 0.5 µm
debond 6
4.61
4.5
5
SiNx 3.8
3.57
4 3.2
SiO2 2.8
3 2.41

Si 2

0
O O Si 0% 10% 20% 30% 40% 50% Graded

O
Si
O O Si-CH3 / Si-O FTIR ratio
O O
Si O Si
O O
Si H3C
O Si O Si
Si O O
O O O O
O
H3C Si CH3
Si J. Rim, F. Shi and R.H. Dauskardt - 2000
silica O Si
O
O CH3
Si O
H3 C
O carbon-doped
 SoG Porosity Effects on Properties
1.6

fracture MSQ

Density (g/cm3)
1.4
(Hitachi Chemical)

1.2

3.0 1.0
Fracture Energy (J/m2)

2.5 0.8
2.0 0 10 20 30 40 50
Initial Content of Porogen (wt%)
1.5

Dielectric Constant k (at 10KHz)

1.0 3.6
3.4
0.5
3.2
0.0 3.0
0 10 20 25 30 40 50 2.8
Initial Content of Porogen (wt%) 2.6
2.4
L. Wang, J. Rim, and R.H. Dauskardt - 2002 2.2
2.0
0 10 20 30 40 50
Initial Content of Porogen (wt%)
 SoG NaOH Promoter Effects on Properties
L. Wang, J. Rim, and R.H. Dauskardt - 2002
0.995
Fracture Energy (J/m2)
3.0

Density (g/cm3)
2.5 0.990

2.0 0.985
1.5
0.980
1.0
0.5 0.975
0 20 40 60 80 100
0.0 NaOH Promoter Content (ppm)
0 10 25 50 75 100

Dielectric Constant k (at 10KHz)

Promoter Content (ppm)
3.4
• Step 1: Hydrolysis
NaOH 3.2
Si(OR')3R + H2O ------Æ Si(OR')2ROH + HOR'
NaOH 3.0
Si(OR')4 + H2O ------Æ Si(OR')3OH + HOR'
2.8
• Step 2: Condensation
2.6
Si(OR')2CH3OH + Si(OR')3OH
0 20 40 60 80 100
Æ CH3(OR')2Si-O-Si(OR')3 +H2O NaOH Promoter Content (ppm)
 SoG Composition Effects on Fracture Properties
Constant CH3, Varying H Functional Group Size
Fracture Energy, Gc (J/m2)

Fracture Energy, Gc (J/m2)

10
SiO2 Methyl
8 “Rule of Mixture” 4 Vinyl
Models Phenyl
6 3

4 CH3 2

2 CH3/H 1

0 0
0 1 2 3 0 20 40 60 80
(Effective Functional Group Content) x (Size)
Si-O Bond Ratio, SiOx

H R=H increasing functional group size

HC
3
Si O Si
O O
R = CH3 O
O O Si Si
O Si
HC
Si 3 Si CH
O 3
O C2H3
Si
O
Si O H Methyl Side Groups C6H5
HC (R = CH3) CH3
3
O
Hydrogen Side Groups Methyl Vinyl Phenyl
(R = H)

L. Wang, J. Rim, F. Oota and R.H. Dauskardt - 2001

 Porous Brittle Dielectrics (MSSQ)
Elastic and Fracture Properties Porous MSSQ/Resin-1/Porogen DMAEMA-MMA

Isostrain

50% 200 nm

Isostress …but some surprises!

25
actual Untreated

Interfacial Adhesion, G (J/m2)

Treated

Porosity, ρ 20
Fracture path:
MSSQ-Silica

15
…anticipate fracture problems
in complex structures… 10
All others show
fracture at
MSSQ-chromium

film stress: σ f ≈ Ef ∆α ∆T 5

driving “force” for thin film cracking: 0

0% 10% 20% 30% 40% 50%
βσ h 2
Porosity
G≈ f
∝ Ef
Ef Maidenberg, Miller, Volksen, and Dauskardt - 2002
 Moisture Assisted Subcritical Debonding
applied stress
Pressure
strained debond
tip bonds

chemical reaction
with H20

Aqueous solution
Wafer
crack velocity

H20
l ao

Subcritical debonding
important for reliability copper transport limited zone
during CMP barrier
dielectric
Require Gc > 5 J/m2 to survive
CMP.
Block, Scherban, et.al. INTEL
debond
Proc. IEEE 2001 Int. Interconnect Tech.
Conf., June 2001
M. Lane and R. H. Dauskardt - Proc. MRS, 1999.
 Moisture-Assisted Debonding
• Interaction of moisture with strained debond tip bonds applied stress

nH 2 O + B (debond tip) → B * (activated complex)

strained debond
tip bonds

chemical reaction
• Chemical reaction rate theory: with H20

rate = k r [H 2O ] [B ]
n

Wiederhorn et. al. model (1980)

n Region III
da  PH2O   − E * + bGtip 
= A o  exp 
dt  
 P   RT 

GC
• Atomistic crack-growth models: Region II
(Transport-controlled)
  − U +*   − U −* 
TH

rate = fo exp   − exp  

  kT   kT  Region I
(Reaction-controlled)
Lawn and Cook model (1990)
da  G − 2γ 
= v o sinh tip 
dt  η  Crack Driving Energy, G
 Subcritical Delamination Behavior in Moist Environments:
Temperature and Humidity Effects

Crack-Growth Model
da  G − 2γ  Debonding in CDO Dielectrics
= vo sinh 

Delamination Growth Rate, da/dt (m/s)

J. Rim, F. Shi and R.H. Dauskardt - 2000
dt  η  -4
10

debond TaN/SiO2
5 at.% C (25oC and 50% RH)
Delamination Growth Rate, da/dt (m/s)

-3 -5
10
10
20 at.% C
10 -6
10
-4 SiO2/TaN/Cu
T = 50oC 10 -7
-5
10
-8
10

-6
10 10
-9

-10
90% RH
-7
10 10
95% RH
30% RH
-11
-8 10
10
1 10
-9 Debond Driving Energy, G (J/m2)
10 50% 20%
5%
-10
10
3 10 15 threshold values crucial for
Debond Driving Force, G (J/m2) reliability
M. Lane and R. H. Dauskardt - Proc. MRS, 1999.
Effect of CMP Solution on Subcritical Debonding
Materials:
-4 JSR - LKD6103 with Poly X Cap
10

T = 30oC Bulk Silica Glass

Delamination observed in MSSQ
Debond Growth Rate, da/dt (m/s)

Crack Growth Rate, da/dt (m/s)

10
-5 2 H 2O ↔ H 3O + –+1973)
(Wiederhorn OH −
2 lone pair 1 lone pair 3 lone pairs
Increasing pH 10-4 orbitals
(shields) (accelerates)
10
-6
accelerates
delamination
pH
10-63.0 solution (e.g. dielectric slurry)
growth rates
1.0 wt.% potassium hydrogen phthalate, hydrogen
-7
10 chloride 0.07 wt.%, formaldehyde 0.05 wt.%, methanol
0.02
-8 wt.%, balance H2O
10

-8 HCl + H 2O ↔ H 3O + + Cl −
10
10-10 1 lone pair
pH 11.0
(shields)
10
-9
H2O pH-1211.0 solution (e.g. barrier metal slurry)
10
0.3 0.4 0.5 0.6 0.02 wt.%
pH 3.0 0.08 wt.% Glycine, 0.03 wt.% sodium chloride,
sodium hydroxide, 0.01 wt.% disodium (MPa√m)
Stress Intensity Factor, K
-10 ethylenediaminetetraacetate anhydrous, balance H2O
10
1 2
Applied Strain Energy Release Rate, G (J/m2) NaOH ↔ OH − + Na +
3 lone pairs
(accelerates)
E. Guyer, M. Patz and R. H. Dauskardt - 2002
 Effect of CMP Solution on Subcritical Debonding
Materials:
10-4 JSR - LKD6103 with Poly X Cap
Debond Growth Rate, da/dt (m/s)

pH 11 Delamination observed in MSSQ

10-5 Buffered
NaOH
10-6
pH 4.5
3%H2O2
10-7 Hydrogen peroxide effects on
pH 3 reaction kinetics
-8
10 Buffered
HCl H 2O2 + H 2O ↔ H 3O + + O2 H −
10-9
5 lone pairs
(accelerates)
10-10
T=30oC
10-11
1 2
Applied Strain Energy Release Rate, G (J/m2)

E. Guyer, M. Patz and R. H. Dauskardt - 2002

 Moisture and Loading Effects during CMP
• chemically-active species in aqueous slurries crucial for
survival through CMP
Engineer interfaces immune to stress corrosion?
• barrier-oxide effect on steric hindrance
-3
10

Debond Growth Rate, da/dt (m/s)

-4
SiO2 10 Ta
adsorbate
-5
10
H2O 2uop ao
oxide -6 premature
10
Ta threshold
Cu -7
TaNx
10
SiO2
-8
10
1 10
Competing rate effects: crack growth rate and Ta oxidization rate
Debond Driving Energy, G (J/m2)
Multi-Scale Simulations of 3-D Interconnect Structures
elastic
Cohesive elastic
zone layer
Use simulations to predict
Gate plastic
n+/p+ n+/p+
Cu zone adhesion and mechanical reliability
elastic of more complex structures
substrate

debond
Computational Model (developed from Klein and Gao - 1999)

Gate
• finite deformation elasticity (FEM)
n+/p+ n+/p+
• large strain elastic/plastic (with hardening)
• VIB debond layer or cohesive zone

Gate σmax ~ E/60

Stress, σ
n+/p+ n+/p+

Microprocessor

Go ~ 5 J/m2 δmax
Reliability of Complex 3-D Structures
Separation, δ
Multi-Scale Simulations of Interface Fracture Resistance

Ductile copper layer, hCu

Elastic barrier layer, D
Interface Fracture Energy, Gc (J/m2)

100
measured yield properties

Copper Yield Stress, σys (MPa)

500
80
Copper layer
σ ys  1 
debond ~ β + 
α  h
Barrier layer
450
Dielectric layer
60 Si wafer 400
simulated yield properties
350 σ ys  1
40 Cu layer thickness ~ β + 
300 Å - 16.4 µm 300 α  h
20
250

0
-2 -1 1 10 20 0 2 4 6 8
10 10
Copper Layer Thickness, h (µm) Copper Layer Thickness, h (µm)

Lane, Vainchtein, Gao, R.H. Dauskardt - J. Mater. Res. 16 [1] 2001

 Ductile Organic Dielectrics:
Thickness Effects on Adhesion
Cu (0.4 µm)
60
Interfacial Adhesion, Gc (J/m2)

Cr (0.02 µm)
SiXy (0.2 µm)
50
SiLK/SiO2 SiLK (0.25 – 5.12 µm) debond
(ozone clean)
40 SiO2

800
30
Cu

Yield Stress, σys (MPa)

600
20
FLARE/SiN SiLK/SiO2 400
10
Cu metal 200

0 SiLK
0.01 0.1 1 10 0
0 2 4 6
Organic Dielectric Thickness, h (µm)
Film Thickness-1, 1/h (µm)-1

Litteken and Dauskardt - 2000

 Barrier Layer Thickness Effects on Adhesion
S. Stroband and R.H. Dauskardt - 2002

Technologically Relevant Values:

hb ~ 5 – 100 nm 1µm Cu
debond barrier
σ c ≈ E / 60 ≈ 1.66 GPa  σc
 ≈ 3 .2 - 8 .0 SiO2 dielectric
σ YS ≈ 200 - 500 MPa  σ YS
silicon
Interface Fracture Energy, Gss/Go

Parameters:
4 H = 10 GPa 5
E = 250 GPa
b
10 Effect of Barrier Stiffness

Interface Fracture Energy, Gss/Go

h = 1.0 µ m
pl

G = 4 J/m
2 3 125
3 0
200
250
25 300
weak interface
500
strong ductile layer
2 50
strong interface 2 Elastic modulus
weak ductile layer
100 Eb (GPa)
barrier thickness
1 typical values hb (nm)
typical values
3 4 5 6 7 8 9 10 11 12 1 3 4 5 6 7 8 9 10 11 12
Normalized Cohesive Stress, σc/σys Normalized Cohesive Stress, σc/σys
Pre-Stressed Metal and Multi-Layer Structures
Films with Residual Stress

Normalized Fracture Energy, Gc/Go

3.0

2.6
σR = -1/3 σys
σR 2.2
plastic zone
barrier 1.8
brittle dielectric
barrier
1.4 σR = 1/3 σys
silicon
substrate -80 -60 -40 -20 0 20 40 60 80
Phase Angle, Ψ (degrees)

Interface Fracture Energy, Gss/Go

20
Multi-Layer Structures bi-layer
18
single layer
ILD (4.0µm) 15 hb = 10 nm
plastic (1.0µm) 13
barrier hb 10 bi-layer
ILD (0.5µm) hb = 20 nm
8
barrier hb
5
plastic (1.0µm)
3 typical values
ILD (4.0µm)
0

2 3 4 5 6 7 8 9 10 11 12
Normalized Cohesive Stress, σc/σys
S. Stroband and R.H. Dauskardt, Interface Science – 2002 (In review)
 Adhesion of Complex Patterned Structures
• Does feature size and aspect ratio effect interface adhesion and reliability?
• Establish guidelines for interface reliability in complex structures

Silicon
Interfacial Adhesion, Gc (J/m2)

14 Metal Layer
SiO2 debond
12 patterned line
adhesion Polymer w h = 1 µm
10

8 Silicon
6 blanket thin-film Optical Micrographs
adhesion
4
shear lip model
2 prediction

0
5 10 15 20
Aspect Ratio (w/h)
C. Litteken and Dauskardt, Int. J. Fracture – 2002 (in review)
top surface bottom surface
 Cu/ILD Patterned Structures (300 mm Wafers)

Landed Trench Hanging Trench

SiC or SiN SiC or SiN

360 nm SiLK or
SiLK or
690 nm Cu CDO
CDO
TaN 690 nm 330 nm
SiC or SiN SiN or SiC
SiO2 SiO2
Si Si
narrow orthogonal wide
features features features
CDO/SiLK
Cu
210 nm
debond
propagation
210 nm

210 nm 210 nm 400 nm 400 nm

C. Litteken, T. Scherban, G. Xu and Dauskardt - 2002

 Landed Patterned Structures –
Etch Stop versus Passivation Cap Debond
6
Interfacial Adhesion, Gc (J/m2)

5 debonded
interface

4 SiC

3 Cu CDO
TaN
orthogonal features
narrow features

2
wide features

SiC
SiO2
1 Si

0
etch stop pattern/passivation
debond debond
 Debond Path Morphology
debond direction

RMS roughness RMS roughness

3.8nm 2.9nm
KI KI
KII KII
 Summary Copper layer

Barrier layer

Dielectric layer

• Adhesion and Fracture Involving Brittle Dielectric Layers Si wafer

– barriers and dielectrics in interconnect structures (TiN, TaN, SiNx, SiO2)

– new low-k dielectric materials (e.g. CDO, MSSQ, SiLK, porosity)
Pressure
• Moisture and Implications for Debonding
– moisture assisted subcritical debonding Aqueous solution
– kinetic models and understanding Wafer

• Multi-Scale Simulations of Adhesion

– interface cohesive zones and plasticity in ductile layers σ
– barrier layer stiffness, thickness and pre-stressed thin films x

• Patterned Structures
– elastic constraint and stress state
– effect of line geometry