PHI 710 Scanning Auger Nanoprobe

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PHI 710 Scanning Auger Nanoprobe

Complete Auger Compositional Analysisfor Nanotechnology, Semiconductors,

Advanced Metallurgy and Advanced Materials

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PHI Auger 710 Superior Analytical Capabilities

Nanoscale image resolution

Image registration for high sensitivity

Constant sensitivity for all sample geometries

High sensitivity at low tilt angles for insulator analysis

Nano-volume depth profiling

Chemical state analysis: spectra, imaging, depth profiling

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PHI 710 Secondary Electron Imaging (SEI)3 nm from Au Islands on Carbon

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PHI 710: High Spatial Resolution Auger

Ga Map 25kV; 1nA 256x256 pixels Line Analysis Al Map 25kV; 1nA 256x256 pixels Line Analysis

Locations for Line Scans Area Analyzed4 nm Al LineAlGaAs Line Width (nm)

AugerLine

Scans

Sample provided by Federal Institute for Materials Research and Testing (BAM)Berlin, Germany

BAM-L200 Standard Sample

1

2

3

4

24 Hour stability test demonstrating exceptional image registry

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PHI 710: High Spatial Resolution Auger

4 nm Line

Line Scan #4

0 0.05 0.1 0.15 0.2 0.25 0.3 0.35Distance (µm)

Inte

nsity

Ga

Al (X3)

BAM-L200 Standard Sample

24 hour analysis demonstrating exceptional image registration

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Constant Sensitivity for All Geometries

0

200

400

600

800

1,000

1,200

1,400

1,600

1,800

2,000

-90 -75 -60 -45 -30 -15 0 15 30 45 60 75 90

Tilt Angle (degree)

Sen

sitiv

ity (k

cps)

Sensitivity vs. Sample Tilt

Coaxial CMA

Non-Coaxial SCA

The CMA with a coaxial electron gun provides high sensitivity at all sample tilt angles which is essential for insulator analysis

Minimum Beam DiameterField

Emission Electron Source

Cylindrical Mirror

Analyzer

Multi-ChannelDetector

Sample holder with high energy resolution optics

Ar+ Ion Gun

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CMA with Coaxial Electron Gun

Poly-Si/W Deposition and PatterningAuger Analysis of ex situ FIB cut

Auger Maps:Si oxideSi elementalW

Auger maps show: Defect is sub-micron Si oxide particle Surrounded by elemental Si Introduced during poly-Si deposition Covered with W

Only the PHI 710 can image samples such asFIB sections with uniform, high sensitivity

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PHI CMA High Energy Resolution Mode

How does the high energy resolution mode work?– The CMA energy resolution is given as:– ΔE / E = 0.5%– An optics element placed between the sample surface and

the entrance to the standard CMA retards the Auger electrons, reducing their energy, E

– From the energy resolution equation, if E is reduced, ΔE is also reduced and so is the Auger peak width; energy resolution is improved

– The CMA is not modified in any way and retains a 360º coaxial view of the sample relative to the axis of the electron gun

– US Patent 12 / 705,261

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710 Energy Resolution Specification

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0 500 1000 1500 2000 2500

Auger Peak Kinetic Energy (eV)

ΔE

/ E (%

)

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Auger KLL spectrum of native oxide on Al foil measured on PHI CMA at 0.5% (blue) and 0.1% (red) energy resolution, after background subtraction.

1350 1360 1370 1380 1390 1400 1410 1420-50

0

50

100

150

200

250

300

350

1393.4 (Al metal)1386.9 eV (Al oxide)

Kinetic Energy (eV)

N(E

) cps

0.5%0.1%

Al KLL Spectra of Native Oxide on Al Foil

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970 980 990 1000 1010 1020 10300

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

Kinetic Energy (eV)

Nor

mal

ized

Inte

nsity

Zn LMM Spectra of Sputter Cleaned Zn Metal0.5% Energy Resolution0.1% Energy Resolution

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0.1% Energy Resolution

Si oxide

Si plasmons

Si elemental

1580 1590 1600 1610 1620 16300

20

40

60-2

0

2

4

6

8

x 104

Kinetic Energy (eV)

c/s

Depth Profile of Native Oxide on Si

10 kV - 10 nA20 µm defocused beam4 minutes per cycle

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Zn oxide Zn metal

970 980 990 1000 1010 1020 10300

5

10

8.4

8.6

8.8

9

9.2

9.4

9.6

9.8

x 105

Kinetic Energy (eV)

c/s

Depth Profile of Zn Oxide on Zn

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PHI 710 Spectral Window Imaging

IC412_256.map: Pad 41 PHI

2012 Sep 22 10.0 kV 10 nA FRR 0.00 s

Si4/-1 RSF

32297

746520 µm

20 µ

mSi4.ls3

IC412_256.map: Pad 41 PHI2012 Sep 22 10.0 kV 10 nA FRR 0.00 sSi4/-1 RSF

47.0

0.020 µm20

µm

Si4.ls1+Si4.ls2+Si4.ls3

Panel A shows a 200 µm FOV SEI of a semiconductor bond pad. Panel B shows the Si KLL peak area image from the area of panel A. Panels C, D and E show the chemical state images of silicide, elemental Si and Si oxynitride respectively. Panel F shows a color overlay of elemental silicon, silicide and silicon oxynitride images.

A B

ED

SEI

Elemental Si Si Oxynitride

SilicideC4094

892.8

IC.401.sem: Pad 41 PHI

2012 Sep 21 10.0 kV 10 nA FRR

SEM/-1 RSF

20 µm

20 µ

m

SEM


2012 Sep 22 10.0 kV 10 nA FRR 0.00 s

Si4/-1 RSF

3462175

113732920 µm

20 µ

m

Si4

Si KLL Peak Area


2012 Sep 22 10.0 kV 10 nA FRR 0.00 s

Si4/-1 RSF

32297

746520 µm

20 µ

m

Si4.ls1


2012 Sep 22 10.0 kV 10 nA FRR 0.00 s

Si4/-1 RSF

32297

746520 µm

20 µ

m

Si4.ls2

F Si Chemical States

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PHI 710 Spectral Window ImagingA B

C

Composite Si KLL


2012 Sep 22 10.0 kV 10 nA FRR 0.00 s

Si4/-1 RSF

3462175

113732920 µm

20 µ

m

Si4

Elemental Si

SilicideSi Oxynitride

Si KLL image with ROI areas

Si KLL Basis Spectra

1604 1608 1612 1616 1620 1624Kinetic Energy (eV)

Inte

nsity

1605 1615 1625Kinetic Energy (eV)

Inte

nsity

Panel A shows the Si KLL spectrum from the sum of all pixel spectra in the Si KLL Auger image shown in panel B. Panel B shows the three Regions Of Interest (ROI) selected for creation of the basis spectra for Linear Least Squares (LLS) fitting of the Si KLL image data set. Panel C shows the three basis spectra with their corresponding chemical state identifications.

PHI App. Note: Chemical State Imaging WithThe PHI 710 Scanning Auger NanoProbe

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Nanocone Imaging

N Map 256 x 256 pixels SEI HR Si-oxide Map at 0.1% Energy Resolution

Only the larger Nanocone contains N Both the large and small features contain Silicon oxide

The composition suggested by the images is confirmed with high energy resolution analysis

Smaller Silicon Oxide Feature Smaller Silicon Oxide Feature

Auger Images SuggestLarger Nanocone Surface Composed of Silicon Oxide and Nitride

2O kV – 10 nA

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Nanocone Chemical Analysis

Si NitrideStandard

Large Nanocone Base 0.1% Energy Resolution

Nanocone base is mixture of silicon oxide and silicon nitride

Si OxideStandard

1600 1605 1610 1615 1620 1625 16300

0.2

0.4

0.6

0.8

1

Kinetic Energy (eV)

Nor

mal

ized

Inte

nsity

Si KLL

20 kV – 10 nA

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PHI 710 Advantages

World’s best Auger depth profiling– Floating column ion gun for high current, low voltage depth

profiling– Compucentric Zalar Rotation™ maximizes depth resolution– Image registration maintains field-of-view

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Low Voltage Depth Profiling

0 10 20 30Sputter Time (min)

Inte

nsity

As

Ga

Al

0 200 400 600 800Sputter Time (min)

Inte

nsity

As

Al

Ga

500 eV Depth Profile 100 eV Depth Profile

Improved Interface Definition with use of Ultra Low Ion Energies

AlAs/GaAs Super Lattice Sample

Improved definition of layers

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Nano Depth Profiling

FOV: 2.0 µm

F

0.5 µm

1

P from the growth gas is detected on the surface of a Si nanowire

20 kV, 10 nA, 13 nm Beam

60 nm Diameter Si Nanowire

100 200 300 400 500 600 700 800-2

-1.5

-1

-0.5

0

0.5

1x 10

4

Kinetic Energy (eV)

c/s

Atomic %Si 97.5P 2.5

O

CSi

P

Surface Spectrum of Nanowire A

SEI

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Non-homogeneous P Doping of Si Nanowires

500 V Ar sputter depth profiling shows a non-homogeneous radial P distribution. The data suggests Vapor-Solid incorporation of P rather than Vapor-Liquid-Solid P incorporation

Depth Profile of Nanowire B

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Compucentric Zalar Rotation Depth Profiling

Ion Beam

Sample

AnalysisArea

Zalar rotation is used to eliminate sample roughening that can occur when sputtering at a fixed angle.

Compucentric Zalar rotation depth profiling defines the selected analysis point as the center of rotation. This is accomplished by moving the sample in X and Y while rotating, all under software control.

Micro-area Zalar depth profiling is possible on features as small as 10 µm with the 710’s automated sample stage.

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0 50 100 150 200 250 3000

20

40

60

80

100

Sputter Time (min)

Ato

mic

Con

cent

ratio

n (%

)

O

Al (oxide)

Al (metal) Si

Compucentric Zalar Depth Profile of 10 µm Via Contact

Secondary Electron Image(Before Sputtering)

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0 50 100 150 200 250 3000

20

40

60

80

100

Sputter Time (min)

Ato

mic

Con

cent

ratio

n (%

)

O

Al (oxide)

Al (metal) Si

Depth Profile Comparison With and Without Zalar Rotation

0 50 100 150 200 250 3000

20

40

60

80

100

Sputter Time (min)

Ato

mic

Con

cent

ratio

n (%

)

Al (metal)

O

Al (oxide)

Si

Without RotationWith Rotation

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Without RotationWith Rotation2500X2500X

SE Images of 10 µm Via Contactsafter Depth Profiling

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Large Area Chemical Depth Profile of Ni/Si WaferAnnealed at 425 ºC

0.1% Energy Resolution 10 kV-10 nA20 µm AverageAs Received

Sputter Conditions:500 V Argon1 x 0.5 mm raster

No Zalar Rotation10° Sample Tilt

Chemical State of Si ? Chemical State of Ni ?

0 10 20 30 40 50 600

100

200

300

Sputter Time (min)

Inte

nsity

(kcp

s)

Ni LMM

Si KLL

Elemental Depth Profile

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Si in Ni layer

Si inSi substrate

0 10 20 30 40 50 60

0

100

200

Sputter Time (min)

Inte

nsity

(kcp

s)

Si KLL

Si Chemical Depth Profile Created Using Linear Least Squares Fitting

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0.1% Energy ResolutionSi basis spectra for LLS Si basis spectra for LLS (expanded)

1616.5 eV(metal)

1617.2 eV(silicide)

Si in Ni layerSi inSi substrateSi in Ni layer

Si inSi substrate

1570 1590 1610 1630Kinetic Energy (eV)

Nor

mal

ized

Inte

nsity


Nor

mal

ized

Inte

nsity

Si KLL Si KLL

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Ni in Ni layer Ni inSi substrate

0 10 20 30 40 50 60

0

100

200

300

Sputter Time (min)

Inte

nsity

(kcp

s)

Ni LMM

Si Chemical Depth Profile Created Using Linear Least Squares Fitting

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Ni basis spectra for LLS Ni basis spectra for LLS (expanded)

844.8 eV(Ni-silicide)

846.2 eV(Ni-metal)

Ni in Ni layerNi inSi substrateNi in Ni layer

Ni inSi substrate


810 820 830 840 850 860 870 880Kinetic Energy (eV)

Nor

mal

ized

Inte

nsity

830 835 840 845 850 855 860Kinetic Energy (eV)

Nor

mal

ized

Inte

nsity

Ni LMM Ni LMM

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FOV: 5.0 µm 20.000 keV

Fe3C 2/16/2010F

1.0 µm

1

2

SEM 20kV - 1nA Analysis points

Point 1: Ni-silicidePoint 2: Si-metal

After Depth Profile

Auger multi-point analysis shows composition of nano-structures

500 1000 1500 2000

1.0

1.5

2.0

2.5

Kinetic Energy (eV)

Inte

nsity

(Mcp

s)

Si

Ni

||||

Si

Si

Si

NiNi

C

C

Ni Point 1

Point 2

22 nm beam size

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After Depth Profile0.1% Energy Resolution

1616.5 eV(metal)

1617.2 eV(silicide)

Point 2Si inSi substrate

Point 1Si in Ni layer

Point 1Si in Ni layer

Point 2Si inSi substrate

1570 1580 1590 1600 1610 1620 1630 1640Kinetic Energy (eV)

Nor

mal

ized

Inte

nsity


Nor

mal

ized

Inte

nsity

Si KLL

22 nm beam size

Si KLL (expanded)22 nm beam size

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Ni/Si Annealed at 425 °C

FOV: 5.0 µm 20.000 keV

Ni/Si 425C 3/30/2010F

1.0 µm

1

2

1

2

SEM 20 kV - 10 nA Analysis points Auger Color Overlay 20 kV - 10 nA 256 x 256 pixels

12 nm Removed

Nano-areas selected for depth profiling

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Nano Area Chemical Depth Profile of Ni/Si WaferPoint 1 – Ni Layer

10 kV – 10 nAPoint 1LLS Profile

Sputter Conditions:500 V Argon1 x 0.5 mm raster

No Zalar Rotation10° Sample Tilt

Nano area depth profile shows nickel silicide at the nickel / silicon interface Large area depth profile included heterogeneous distributions of nickel silicide

that grows through imperfections in Ni film

0 20 40 60 80 100 120 140 160 180 2000

100

200

Sputter Depth (nm)

Inte

nsity

(kcp

s)

Si metal

Si silicide

Ni metal

Ni silicide

Chemical Depth Profile Created Using Linear Least Squares Fitting

22 nm beam size

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PHI 710 Scanning Auger NanoprobeMulti-technique Options

The Complete Auger Solution

Energy Dispersive Spectroscopy (EDS or EDX)

Backscatter Electron Detector (BSE)

Electron Backscatter Diffraction (EBSD)

Focused Ion Beam (FIB)

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PHI 710 Chamber Layout for Options

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PHI 710 Scanning Auger Nanoprobe

Complete Auger Compositional Analysisfor Nanotechnology, Semiconductors,

Advanced Metallurgy and Advanced Materials

Documents

PHI 710 Scanning Auger Nanoprobe