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LED Analysis at EAG

Tim Chang and Gary Mount

Specialists in Materials Characterization

EAG Background in Semi and LED


Established in 1978, Silicon Valley California EAG Taiwan established in 2000 Now over 15 locations in 7 countries 30+ analytical techniques Over 150 instruments Over 300 scientists and engineers Career scientists, many with Ph.D. Foundation in semiconductor industry Very active in LED space
Process monitoring and R&D analysis for 20 years.

Copyright 2011 Evans Analytical Group

MOCVD Reactor Capacity by Region

Courtesy of Yole Development

Copyright 2011 Evans Analytical Group

Barriers to Adoption

price

5x price

40x price

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Costs for LED Light Source

Source: US Department of Energy


Copyright 2011 Evans Analytical Group

MOCVD Epitaxy Big Effect on Cost : Big Effect on Performance


Alternative Substrates: #2: Si Epitaxy: Cluster tools New Epi technologies. Large Diameter Substrates: 4, 6, 8. Lithography: Dedicated tools, higher throughput. Epitaxy MOCVD: Higher yields and throughputs Improved material quality.

Manufacturing Cost

Wafer Level Packaging: Silicon TSC, Wafer level optics.

Testing and Binning: Wafer level Higher throughputs.

Phosphors: Conversion Phosphors: Quantum dots efficiency, Color rendering phosphors IP Free phosphors. Substrate Separation: Laser Lift Off, other separation techniques.

Mirrors: Resonant Cavities.

Die Singulation: Increased throughputs and yields. Encapsulation Materials and Optics: Ageing and optical properties. Mirrors: Improve reflectivity electrical properties.

Alternative Substrate: #1: GaN, AnO, Si, Engineered substrates.

Thermal Management: New materials for packaging.

Contacts & Electrodes: Transparent contacts / Electrode materials and patterns.

Contacts & Electrodes: p to n layer VIAS.

Surface Texture: Patterned substrates/ Roughening.

Surface Texture: Photonic and Quasi Photonic Crystals.

Current Droop: Green Gap LED Structures.

Courtesy of Yole Development


Copyright 2011 Evans Analytical Group

LED Performance
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MOCVD Reactors

Its somewhat of an art [operating an MOCVD reactor]. You cant make decent stuff [LEDs] without epitaxial active layers. Every machine has its own identity. You need R&D."
Aldo Kamper, president and CEO of Osram Opto Semiconductor Interview with Greentechsolar: March 7, 2011

Copyright 2011 Evans Analytical Group

Testing and Binning


Each part is binned for 3 parameters Color Forward Voltage Brightness
Flux

Example: 8 color bins 4 Vf bins 3 flux bins

Color

Forward Voltage

For a customer that wants warm white, highest brightness and mid-range Vf, only 5% of the bin space qualifies.

A lot of this variability is created at the epitaxy stage: Within Wafer Wafer to Wafer Run to Run Reactor to Reactor
Courtesy of Yole Development
Copyright 2011 Evans Analytical Group

LED Evaluation
Binning can only be done by testing LED performance for finished devices. Much of the LED performance is determined by the device microstructure as grown by MOCVD epitaxy.
MOCVD is really the weak point in LED manufacturing. Good die yields after binning are about 35% industrywide. Manufacturers really need some feedback loop on actual dopant concentration homogeneity to fine tune their tools. (Source: Yole Development)

SIMS is an excellent way to monitor epitaxy microstructure and it can be done before any devices are made!

Copyright 2011 Evans Analytical Group

EAG Services for LED


EAG Taiwan Can Provide: Process Monitoring Research & Development Failure Analysis Construction Analysis (Reverse Engineering)

Copyright 2011 Evans Analytical Group

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Process Characterization and Monitoring


Characterizing the performance of MOCVD reactors using SIMS is one of our most popular analysis. SIMS is a powerful process characterization tool. We use SIMS depth profiling to look at layer structure and thickness, n and p type doping levels in all layers, and contaminants in all layers. Customers can compare center and edge growth on a wafer, can compare wafer to wafer, compare wafers from the center and edge of the platen, compare lot to lot from the same reactor, and compare reactors. As wafers get larger these comparative measurements will only become more important.
Copyright 2011 Evans Analytical Group

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Si and Mg Profiles
Measure Peak Concentration Average Concentration

Layer Thickness

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Long Term Precision for Si in GaN

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Value of SIMS for Process Monitoring


We currently have 2 major LED manufacturers who use EAG SIMS for MOCVD process monitoring. EVERY COMPANY THAT HAS USED SIMS FOR MOCVD PROCESS MONITORING IN A SERIOUS WAY HAS CONTINUED TO DO SO. a very strong endorsement of the value of the measurements.

Copyright 2011 Evans Analytical Group

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EAG Services for LED


EAG Taiwan Can Provide: Process Monitoring Research & Development Failure Analysis Construction Analysis

Copyright 2011 Evans Analytical Group

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Research & Development


SIMS: Dopant and contaminant concentration and distribution TEM: Layer thickness / uniformity > primarily QW region Growth quality defects dislocations type and number QW interface sharpness STEM: Layer composition EBIC: Junction and junction defects

Copyright 2011 Evans Analytical Group

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III-V Layer Structure


1E+21 1E+06

InP HBT
1E+20 1E+05

CONCENTRATION (atoms/cc)

Ga->
1E+19

The layer structure can be seen and thickness measured


Counts per Second
InGaP InP InP InGaP InP InGaP InGaP Si: 3E19 Si: 3E19 undoped C: 3E19 undoped C: 3E19 undoped

1E+04

1E+18 1E+03 1E+17

1E+02 1E+16

1E+15

1E+01

InGaP

Si: 4E18

1E+14 0 0.5 1 1.5 2 2.5 3

1E+00

InP

substrate undoped

DEPTH (microns)
Copyright 2011 Evans Analytical Group

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III-V Dopants
1E+21 1E+06

InP HBT
1E+20

Si

C Ga->

1E+05

CONCENTRATION (atoms/cc)

Dopant concentrations can be profiled and quantified in multiple layers.


Counts per Second
InGaP InP InP InGaP InP InGaP InGaP Si: 3E19 Si: 3E19 undoped C: 3E19 undoped C: 3E19 undoped

1E+19 1E+04

1E+18 1E+03 1E+17

1E+02 1E+16

1E+15

1E+01

InGaP

Si: 4E18

1E+14 0 0.5 1 1.5 2 2.5 3

1E+00

InP

substrate undoped

DEPTH (microns)
Copyright 2011 Evans Analytical Group

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III-V Contaminants
1E+21 1E+06

InP HBT
1E+20 1E+05

CONCENTRATION (atoms/cc)

Ga->
1E+19

Performance destroying contaminants can be measured and quantified


Counts per Second
InGaP InP InP InGaP InP InGaP InGaP Si: 3E19 Si: 3E19 undoped C: 3E19 undoped C: 3E19 undoped

1E+04

1E+18 1E+03 1E+17

H
1E+02

1E+16

1E+15

1E+01

InGaP

Si: 4E18

1E+14 0 0.5 1 1.5 2 2.5 3

1E+00

InP

substrate undoped

DEPTH (microns)
Copyright 2011 Evans Analytical Group

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SIMS for Structure and Doping


p-GaN
1E+21

p-AlGaN

InGaN MQWs

n-GaN

Mg
1E+20

In (a.u.)

C NC TRA N (atom O EN TIO s/cc) Concentration (atoms/cm3)

1E+19

Si Al (a.u.)
1E+18

1E+17

Powerful analysis tool


Depth profiling dopants and impurities in III-V heterostructures Surface, layer, substrate and interface
0

1E+16

1E+15

Stoichiometry in some cases


0.1 0.2 0.3 0.4

0.5

0.6

0.7

0.8

DEPTH (microns) Depth (micron)

Copyright 2011 Evans Analytical Group

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Quantum Well Dopant


PCOR-SIMSSM

5.0E18

0.100

Si CONCENTRATION (at/cm3)

In Ga,In Atomic Fraction


4.0E18 0.080

3.0E18

0.060

Si
2.0E18 0.040

1.0E18

0.020

0 0 50 100 150

0 200

DEPTH (nm)

High depth resolution SIMS can reveal the doping profile within the quantum well. Best quantification is achieved using PCOR-SIMS, a protocol that provides accurate quantification in all matrix layers.

Analysis with high depth resolution SIMS

Copyright 2011 Evans Analytical Group

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Research & Development


SIMS: Dopant and contaminant concentration and distribution TEM: Layer thickness / uniformity > primarily QW region Growth quality defects dislocations type and number QW interface sharpness STEM: Layer composition EBIC: Junction and junction defects

Copyright 2011 Evans Analytical Group

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Example: Commercial GaN LED Dislocation Density XS & PV


1

XS
2 1 2 3

PV
3 1 2 3

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Rapid Typing of Dislocations


The character of dislocations can be quickly determined using STEM imaging. By utilizing specific sample tilts, threading dislocations can be identified as having screw, edge, or mixed character.

Copyright 2011 Evans Analytical Group

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Quantum Well and Superlattice


Quantum well and superlattice layer thicknesses can be measured using high resolution TEM imaging.

1.11 nm

2.71 nm

Copyright 2011 Evans Analytical Group

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Research & Development


SIMS: Dopant and contaminant concentration and distribution TEM: Layer thickness / uniformity > primarily QW region Growth quality defects dislocations type and number QW interface sharpness STEM: Layer composition EBIC: Junction and junction defects

Copyright 2011 Evans Analytical Group

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Quantum Well Composition


1 2 3 4

STEM/EDS (at%) Location 1 2 3 4 5 Al 9 In 6 3 2

Epi-layer Structure

STEM/EDS can determine composition of the quantum well layers with 2-3nm spot size.

Copyright 2011 Evans Analytical Group

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Research & Development


SIMS: Dopant and contaminant concentration and distribution TEM: Layer thickness / uniformity > primarily QW region Growth quality defects dislocations type and number QW interface sharpness STEM: Layer composition EBIC: Junction and junction defects

Copyright 2011 Evans Analytical Group

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Finding Defects using EBIC


EBIC
Defect

SEM

Electron Beam Induced Current (EBIC) imaging is compared with standard SEM imaging. An EBIC bright spot reveals a defect that is not seen in standard SEM.

Copyright 2011 Evans Analytical Group

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Analysis of EBIC Discovered Defect


A closer view of the defect site shows large and small bright spots in the EBIC image. A cross section was prepared using FIB at the red line. A TEM image of the defect cross-section is shown aligned on the same scale as the EBIC image. A pit defect is present under the small bright spot Magnifying the TEM cross-section image vertically reveals a disruption in the quantum well epi-layer growth. The EBIC image is brighter where the quantum well is closer to the ITO layer.
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Copyright 2011 Evans Analytical Group

Locate Junction by EBIC


Top and bottom contacts are required. A current is passed through the sample. An electron beam is rastered over the sample and where it touches the electrical junction, current is induced.

Copyright 2011 Evans Analytical Group

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EAG Services for LED


EAG Taiwan Can Provide: Process Monitoring Research & Development Failure Analysis Construction Analysis

Copyright 2011 Evans Analytical Group

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Failure Analysis
Mainly chip but also some full package RTX: delaminations / cracks / voids / line breaks OBIRCH: defect localization FIB : cross-section and find defect STEM / Auger: FIB follow up for defect ID composition metal migration > Auger works well in FIB crater. GC-MS: Gas bubbles inside package.

Copyright 2011 Evans Analytical Group

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Package and Wire Integrity

Real Time X-ray (RTX) looks into the package providing images in real time. Examination of this LED reveals an open wire.

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Curve trace results show a difference when compared with the good device:

Bad

Good

Reverse Bias

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Defect Detection by OBIRCH


OBIRCH reveals a defect location. We can use the OBIRCH image to locate the defect for Dual Beam FIB.

Copyright 2011 Evans Analytical Group

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Defect Analysis by Dual Beam FIB


Localized defect from OBIRCH

After localizing by OBIRCH the defect is cross-sectioned by FIB and imaged with SEM. Examples: Metal migration FIB cross-section and investigation by Auger. Voids FIB cross-section and investigation by SEM. Particles surface or FIB cross-section and investigation depending on size and possible organic content Cracks FIB cross-section and investigation by SEM Delaminations FIB cross-section and investigation by SEM
Copyright 2011 Evans Analytical Group

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Failure Analysis
Mainly chip but also some full package RTX: delaminations / cracks / voids / line breaks OBIRCH: defect localization FIB : cross-section and find defect STEM / Auger: FIB follow up for defect ID composition metal migration > Auger works well in FIB crater. GC-MS: Gas bubbles inside package.

Copyright 2011 Evans Analytical Group

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LED Discoloration
Gas bubble that appear inside LED packaging can be extracted and analyzed by GC-MS.

Copyright 2011 Evans Analytical Group

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EAG Service Offerings


EAG Taiwan Can Provide: Process Monitoring Research & Development Failure Analysis Construction Analysis (Reverse Engineering)

Copyright 2011 Evans Analytical Group

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FTIR Identification of Polymer Materials


LED Encapsulant 100 3523

1382

95

90 2868

85 2950

Package material in this case identified as a modified epoxy.

1608

1129

1455

1086

1041

75

70

65

60

3500

3000

2500 Wavenumbers (cm-1)

2000

1736

1500

1509

1182

%T

80

1301

1235

1000

Copyright 2011 Evans Analytical Group

830

761

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Construction Analysis Package Level


Measurement of the materials, structure, composition and doping profiles that comprise an LED

phosphors

wire chip reflector

Structure
Materials and layout of the package and support structures can be examined in cross-section using SEM imaging and EDS analysis.

heat-sink/support

Phosphors
SiO2 Au GaN Gd doped YAG Sapphire
Materials identification in and around the LED chip includes and evaluation of the phosphors. In this case STEM/EDS identified the phosphor as Gd doped YAG. Lattice imaging and d-space measurements confirm YAG identification.

Silicone

Cu

Ag

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Construction Analysis Die Level


100 90

Au W

N-contact W Rh

Au

80

W Rh ITO
O In ITO

n contact
Auger depth profile

70

60 Atomic Concentration (%)

GaN
Ga N

50

40

n and p contact evaluation by Auger depth profiling

30

20

10

Sn

Contacts

0 100

50

100

150 Sputter Time (min)

200

250

300

350

Au
90

Au
W

Rh

80

W Rh ITO
ITO In

p contact
Auger depth profile

P-contact

70

SiO2
O

GaN
Ga N

60 Atomic Concentration (%)

50

Au

40

Si
30

Rh ITO

20

SiO2

10

Sn
0 350

TEM cross-section of p contact

Copyright 2011 Evans Analytical Group

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Quantum Well Composition


1 2 3 4

STEM/EDS (at%) Location 1 2 3 4 5 Al 9 In 6 3 2

Epi-layer Structure

STEM/EDS can determine composition of the quantum well layers with 2-3nm spot size.

Copyright 2011 Evans Analytical Group

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Construction Analysis Die Level


Deprocessed

Polished

Decapped LED may need to be polished to remove leads. The LED may need to be etched to remove passivation prior to SIMS analysis.
Mg
1E+20 Concentration (Atoms/cm3) 1E+21

Al (intensity)
1E+19 1E+18 1E+17

Si

1E+20

1E+19

Crater

1E+18 1E+16 1E+15 0 200 400 600 800 1E+17 1000

Depth (nm)

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INTENSITY (arbitrary units)

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Summary

Why Use EAG Taiwan?


1. Experts in LED Analysis 2. Special Instruments for LED 3. Fast Turnaround Time 4. All Types of LED Analysis

Copyright 2011 Evans Analytical Group

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End

Specialists in Materials Characterization

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