PHI nanoTOF II TOF-SIMS Unique features of the PHI nanoTOF II TOF-SIMS: • Elemental, isotope and...

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PHI nanoTOF II TOF-SIMS

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25+ Years of TOF-SIMS at PHI

PHI has a long history of developments to support new applications.

1507 08 09 10 11 1204 05 0601 02 0399 0093 94 95 96 97 9890 91 928988 13 14

LMIG

PHI Purchased

CE&A TOF-SIMS

business

Pulsed Cs Gun

Direct Imaging

VUV

Laser

Pulsed Ar

Excimer

Laser

New Cs gun

200 mm

300 mm

Stopped

Development

On 7200In Emitter

TRIFT I TRIFT II

7000/SALI 7200

Dual Source Column

Larger Analyzer FOV

DEM

Detector Scanning

3D Imaging

Au Emitter

Stage Mapping

New LMIG

Improved Au Performance with HR2

Auto / Batch Data Processing

Topo-Strip Data Processing

TRIFT III TRIFT IV

New 5-axis Stage

Dual-Beam Charge Comp

20 kV C60

Auto / Unattended Analysis

FIB-TOF

GCIB

Bi Emitter

New LMIG

Improved HR2 Imaging

TRIFT VnanoTOF

Auto Startup

Auto ShutdownNew Bi Emitter

New FIB

New Cs Gun

New GCIB

2016

Introduction of

Parallel Imaging

MS/MS

nanoTOF II

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Unique features of the PHI nanoTOF II TOF-SIMS:

• Elemental, isotope and molecular fragment with high mass resolution and high sensitivity

• 16,000 m/Δm mass resolution with ~ m/z 10,000 mass range

• > 1 part per million detection limits (Detection Limits ~109 at/cm2)

• 70 nm Spatial Resolution with 2 nm surface sensitivity

• The large angular acceptance and depth-of-field characteristics of the TRIFT analyzer provide high

sensitivity for chemical visualization of samples having rough surfaces.

• HR2 chemical / molecular imaging enables the acquisition of data with simultaneous high lateral

resolution and high mass resolution while also using a high analysis beam current, i.e. ≥ 1 nA, so that the

analysis times remain short, e.g. ≤ 10 minutes.

• The patented dual-beam charge neutralization system for ease-of-use in turn-key insulator analysis.

• The metastable rejection characteristic of the TRIFT analyzer generates data sets with high dynamic

range and low spectral background.

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Highlights of the PHI nanoTOF II

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TOF-SIMS Imaging

Total Area Spectrum

Primary Ion Beam

Total Ion Image

m/z

Sample

One imaging data file of a few minutes acquires a spectrum at every pixel of the image.

The computer can reconstruct a total ion image or total area spectrum from this file.

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Total Area Spectrum

Primary Ion Beam

Total Ion Image

m/z

m/z

Chemical Map 2

Chemical Map 1

m/z

Region 2 Spectrum

Region 1 Spectrum

Sample

TOF-SIMS Imaging

Spectra from selected areas of the total ion image or images from selected peaks of

the total area spectrum can also be obtained for complete analysis after data acquisition.

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Positive TOF-SIMS Spectrum of PET

Fragments allow the molecular structure of the polymer repeat unit to be defined.

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Positive TOF-SIMS Spectrum of PET

The repeating peak patterns confirm the polymerization structure

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Full Mass Spectrum at Every Depth

0 50 100 150 200 250 300 350Depth (nm)

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30Si-

MoSi-

Sample: 120 nm MoSi2/Si

Objective: To measure determine the

impurities at the interface.

Approach: Interleaved Depth Profile

1 keV Cs+/15 keV Ga+

Raw-data-stream acquisition

Extract spectrum at interface

Application: Interface Analysis

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0 20 40 60 80 100 120

Spectrum from interface (118 nm)

MoSi

Si3Si2

30Si

O

C

SiC

SiO2

0 50 100 150 200 250 300 350Depth (nm)

30Si-

MoSi-


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0 50 100 150 200 250 300Nanometers

• Reconstructed Depth Profile showing

some of the interface impurities

• Interleaved depth profiling ensures

that the interface will not be missed

30Si

O

C

SiO2

F

MoSi


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Superior imaging of rough & high topography surfaces

Unique HR2 capability… high mass resolution with high spatial

resolution at high beam current

Optional C60 & GCIB sources for exceptional depth profiling & 3D

imaging capabilities across a wide variety of materials

Unique 3D chemical imaging by FIB-TOF tomography

Superior Signal/Background organic spectra with metastable

rejection due to TRIFT analyzer

With a Triple Ion Focusing Time-of-Flight (TRIFT) Mass Analyzer


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Cluster GunsAr2500

+, C60q+

Gas GunAr+, O2

+

FIB Gun

Cesium

Gun LMIGGa+, Aun

q+, Binq+

High Mass

Blanker

SE Detector

Ion Detector

Imaging

Aperture

Post-ESA

Blanker

ESA 3

ESA 2 ESA 1

Energy Slit

Sample

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Superior Imaging & Characterization of Rough, High

Topography Surfaces

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“Most Samples are Not Flat.”

TRIFT Analyzer Design Philosophy

If you can’t image a feature,

you can’t determine the

chemistry of that feature.

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IC Bump Digitizer Trace Nozzle HD Head

Many samples of complex shapes produce a distortion of the ion extraction fields causing difficulties for

chemical imaging.

Delayed extraction reduces these effects in other instruments, but limits the mass range and produces

spectra with a non-linear mass scale.

The TRIFT has both a large angular acceptance and a large depth-of-field to overcome these difficulties

without using delayed extraction.

High Aspect Ratio Samples

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Large Angular Acceptance of TRIFT Analyzer

Three spatial crossovers refocus divergent ions to

generate a wide angular acceptance which is key for

high topography samples.

Sample

Immersion Lens

Detector

Energy Slit

Total Ion Image

Step

Edge

Triple Ion Focusing Time-of-Flight Mass Analyzer

Flexible

Substrate

Primary Ion Beam (40)Metal interconnect

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Large Depth-of-Field for TRIFT Analyzer

Higher energy ions travel a longer distance through the

spectrometer and arrive at the detector at the same time

as lower energy ions. The default position of the energy

slit provides a 240 eV bandpass filter for excellent

depth-of-field on high topography samples.

Poly Ethyl Methacrylate

Acrylic Adhesive

~ 100 µmSample

Immersion Lens

Detector

Energy Slit

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Large Depth-of-Field Nonwoven Fiber Example

Exceptional imaging depth-of-field of > 150 µm

(8 fibers each ~20-25 µm in diameter). Excellent spectral quality and

high sensitivity is maintained at each fiber layer.

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j

k

l

m

n

p o

Total Ion image, -SIMS, 200 µm field of view (FOV)

100 200 300 400 500

100 200 300 400 500m/z

149

163

197 223

473

493

297

149

163

197

223

473

493

297

-SIMS ROI spectrum from fiber j

-SIMS ROI spectrum from fiber o

q

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New & Unique HR2 Analysis Mode:

Simultaneous High m/Δm and Small Δl

at High Beam Current

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HR2 chemical / molecular imaging with the new PHI LMIG enables the acquisition of

data with simultaneous high lateral resolution and high mass resolution while also

using a high analysis beam current, i.e. ≥ 1 nA, so that the analysis times remain

short, e.g. ≤ 10 minutes.

Unbunched vs. Bunched (HR2) Imaging

Unbunched Imaging: Best Lateral Resolution, Δl

pw

high V

low V

(rep. rate = 1/t)

sample

ion pulses

(Δl) < 70 nm

(Δt) typ. > 10 ns

Bunched HR2 Spectrometry: Best Mass Resolution, m/Δmbuncher sample

(Δl) < 500 nm

(Δt) < 1 ns

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t

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HR2 Imaging of Organic Micro-Droplets+SIMS; 25 µm FOV

lateral resolution (Dl) < 400 nm

0.5 nA beam current, 6 min. acq.

56.95 57.00 57.05 57.10 57.150

C3H5O

C4H9

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Superior HR2 imaging due to performance of new PHI LMIG.

10 µm10 µm

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HR2 High Mass Resolution of Micro-Droplets+SIMS; sum over entire image area, 6 minutes data acquisition

42.96 42.98 43.00 43.02 43.04 43.06 43.08 43.10 43.12

C3H7

C2H

5N

CH

3N

2

C2H

3O

118.92 118.94 118.96 118.98 119.00 119.02 119.04 119.06

C2F5

660 662 664 666

C45H59O4C45H58O4

m/Δm = 9,292 (FWHM)

m/Δm = 11,860 (FWHM)

m/Δm = 12,100 (FWHM)

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Use imaging mass spectrometry (TOF-SIMS) to:

– Investigate the similarities and differences in epicuticular wax composition of intact plant organ

– Interrogate the variance in composition among epicuticular cells

Targeted organs and cells:

– In general, all major organs..

• Stem

• Leaf (abaxial & adaxial)

• Flower

– Specialized cells…

• Pavement (epidermal cell)

• Stomate (guard cell)

• Trichome (“hair” or “whisker”)

• Pollen (spore)

Biological Sample: Arabidopsis Thaliana

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dev.biologists.org botanicalgarden.ubc.caplanttrichome.org

spores stomata trichomeS

EM

Im

ag

es

TO

F-S

IMS

Im

ag

es

10 mm 10 mm 100 mm

Arabidopsis Thaliana: Specialized Cells

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High spatial resolution total ion imaging of specialty cells

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Total Ion Image (-SIMS)

ROI-3

ROI-1

ROI-2

200 300 400 500

239209493

Nonacosanoic Acid421367223

1-Tricontanol

479

507

395-SIMS from ROI-3: pavement cells

200 300 400 500

491447437349339

463395367

1-Tricontanol

200 300 400 500

517423 507451435

479463

367

395

1-Tricontanol

Nonacosanoic Acid

-SIMS from ROI-1: inside the stomate

-SIMS from ROI-2: guard cells

Stomates have sizes of

approximately 1 x 7 µm.

Arabidopsis Thaliana:Surface Lipid Composition of Cells

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Low noise, high signal-to-background for stomate cell due to superior TRIFT analyzer with metastable ion

rejection.24

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Total Ion Image (+SIMS)

ROI-2

ROI-1

200 300 400 500

209435407237 491

507463

223 395 479453

423

1-Tricontanol

Nonacosanoic Acid+SIMS from ROI-1 of the trichome

200 300 400 500

213 437 453367

423

395

Nonacosanoic Acid

+SIMS from ROI-2 of the underlying pavement cells

Requires > 200 µm depth-of-

field for chemical imaging.

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High signal-to-background for trichome with high depth of field due to superior TRIFT analyzer.

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Arabidopsis Thaliana:Surface Lipid Composition of Cells

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Optional C60+ Molecular Lipid Imaging of Mouse Brain

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m/z 734

m/z 760

700 750 800 850Mass [m/z]

2.0E+4

4.0E+4

6.0E+4

8.0E+4

1.0E+5

1.2E+5

866

850810

826789734

782772

760

798

m/z 772 m/z 782

m/z 788

m/z 798

m/z 184

(phospholipid head group)

m/z 369

(cholesterol)

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Focused

Primary Ion Beam

Insulating Sample

Low

Energy

Electron

Source

Negative Static

Charge

+ + + + +

-

-

-

-

-

-

-

-

-- -

-

-

-

-

-

-

-

--

Sample Platen

Low Energy

Positive Ion

Source

Focused

Primary Ion Beam

Insulating Sample

Low

Energy

Electron

Source

+ + + + +

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

Collection of high quality data quickly without any tuning of the neutralization settings, the

spectrometer, or recalibration of the mass spectrum. Easy single parameter insulator analysis is

accomplished with only adjustment of the sample bias since the spectrometer is grounded.

Dual Beam Charge NeutralizationFor Insulators like Polymers and Life Science Samples

* US Patent 5,990,476, JP Patent P3616714, EP Patent 0848247B1

An electrostatic charge on the insulating sample

surface may repel electrons from a low energy flood

gun and prevent effective charge neutralization.

PHI’s patented* dual beam charge neutralization

method uses a low energy ion beam to eliminate

electrostatic charges on the sample surface and a

low energy electron beam to neutralize the charge

created by the primary ion beam.

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Optional Ion Guns for

Depth Profiling

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O2+ Ion Gun Sputter Depth Profiling

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▬ D-SIMS

▬ TOF-SIMS

Excellent Comparison between TOF-SIMS vs D-SIMS Layer (Depth Resolution)

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Nickel (60 nm)

Silicon (substrate)

Chromium (60 nm)

Depth Resolution Test Sample: Optional Cs+ Gun

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Dual-Beam Interleaved Depth Profiling with Cs+ Gun

Negative SIMS

1 keV Cs+; 250 x 250 µm2

15 keV Ga+; 25 x 25 µm2

Oxygen enhancement

of Ni at interfaces

100 200 300 400 500 600 700Depth (nm)

Cr

Ni

Cr/Ni Multi-layer Analysis

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Positive SIMS (CsM+)

1 keV Cs+; 250 x 250 µm2

15 keV Ga+; 25 x 25 µm2

More uniform Relative Sensitivity

Factors

100 200 300 400 500 600 700Depth (nm)

CsCr+

CsNi+

Dual-Beam Interleaved Depth Profiling with Cs+ GunCr/Ni Multi-layer Analysis

CsM+ improves quantification

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Optional Gas Cluster Ion Beam (GCIB) Depth Profiling

Si substrate

9 delta layers of P2VP~ 225 nm PS

PS: polystyrene

P2VP: poly(2-vinylpyridine)

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GCIB Depth Profile

+SIMS; 60 keV Bi3++ analysis; 5 keV GCIB (Ar2,500

+) sputtering

0 100 200 300 400 500Depth (nm)

Total Ion

Si

C3H9Si

C7H7

C7H8N

The depth profile of the P2VP

delta layers are clearly observed

by the C7H8N+ monomer signal in

the PS matrix. The polymer

signals are stable throughout the

multilayer film. There is some

signal fluctuation at the Si

substrate interface as a result of

the presence of the native oxide.

NOTE: The depth scale is

estimated based on the analysis

conditions and against the

previous analysis.

The Si arises from both the substrate

and the silicone contamination

(predominantly at the surface). It is not

observed to increase as a function of

depth until the substrate is reached.

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+) sputtering

0 100 200 300 400 500Depth (nm)

C7H7

C7H8N (x1.8)

The P2VP and PS profiles

are shown overlayed on a

linear intensity scale. A total

of 18 layers (9 bi-layers)

were measured before

reaching the Si substrate.

NOTE: The depth scale is

estimated based on the

analysis conditions and

against the previous

analysis.

9 bi-layers (18 total layers).

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GCIB Depth Profile of PS/P2VP

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3D Iso-Surface Imaging of PS/P2PV


+) sputtering

C7H7+ (PS, 91m/z); C7H8N

+ (P2VP, 106m/z); Si+ (28m/z)

surface surfaceSi from silicone

(i.e. PDMS)

Si from

substrate

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0 2000 4000 6000 8000Depth (nm)

Total Ion

C

Si

Al

Cu

Mg

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Optional C60+ vs. Ar+ Profiling of Sol-Gel

+SIMS; 5 keV Ar+ sputtering

The Si/Al stoichiometry appears

to change as a function of depth.

The C signal also varies as a

function of depth.

There is substantial Cu at the

surface and again at the sol-

gel/Al interface.

The sol-gel/Al interface appears

thick and disordered; however,

the nonuniformity may be a result

of roughness induced by the

sputter beam.

The depth scale is estimated; the

sputtered depth was not

measured by profilometry.

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Sputter Crater

www.phi.com0 2000 4000 6000 8000

Depth (nm)

Total Ion

CSi

Al

Cu

Mg

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+SIMS; 40 keV C60++ sputtering The interface transients are essentially

nonexistent which improves the

capability for quantitative data

analysis.

The ion signals are relatively constant

indicating a uniform Si/Al

stoichiometry. There is no C build-up

from the C60 sputter beam.

The sol-gel/Al interface appears more

sharp indicating either a more uniform

sputter crater produced by the C60

beam or a more homogeneous film.

The depth scale is estimated; the

sputtered depth was not measured

by profilometry.


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Sputter Crater

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0 2000 4000 6000 8000Depth (nm)

Si / Al (x104)

C60+/C60

++ profile

Bi3++/Ar+ profile

The C60 sputtering produces a

better profile result. The stable

Si/Al stoichiometry is likely the

result of (a) uniform sputter rates of

the various matrix elements, and

(b) a flat bottom sputter crater.


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Ion Gun Ar+ / O2+ Cs+ C60

+n Arn+ Cluster

Sample Type

Metals Preferred for

+SIMS

More uniform ion

formation yield

> 20 kV minimizes

carbide formation

Very slow sputter

rates, material

dependent

Ceramics

Glasses

Oxides

Differential

sputtering and

chemical changes

Preferred for

negative SIMS like

Cl-, F- and

MetalOx-

Excellent for

glasses, metalloid

alloys and many

oxides

Very slow sputter

rates, with damage

of TiO2, HfO2 and

some other oxides

Organics

Polymers

Severe chemical

damage

Severe chemical

damage

Excellent for chain

scission polymers

Excellent for chain

scission and cross-

linking polymers

Mixed Organics

and

metals/oxides

Severe damage of

organic

components

Severe damage of

organic

components

Excellent sputter

rates of all

components

Very slow sputter

rates of inorganic

components

Semiconductors Preferred for

+SIMS

Preferred for

-SIMS

Not preferred Not applicable

Preferred Sputter Gun Options: Material Dependent

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Ion Gun Advantages Disadvantages

20 kV C60q+ • Bunched m/Δm > 5,000 FWHM

• Small spot size (Δl < 2 µm)

• Consistent sputtering of inorganic

specimens

• Best sputter gun for mixed

composition materials

• Ideal for single-gun analysis of

chain scission polymers and

biological specimens

• Not ideal for sputtering of cross-

linking polymers

• Slow organic sputter rates

compared to GCIB

20 kV Arn+

(n = 400 to 4,000)

• Efficient sputtering for organic and

biological specimens

• Very high organic sputter rates

• Large spot size (Δl > 25 µm)

• Very low inorganic sputter rates

• High differential sputter rates

between organic and inorganic

phases

C60+ and Gas Cluster+ Ion Gun Comparisons

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Optional FIB for FIB-TOF Tomography

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3D Imaging by FIB-TOF Tomography

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sample preparation FIB sectioningTOF-SIMS ion &

electron imaging

Tomography

image processing

x

y

z

FIB

LMIG

Imaging

Plane

Sample stage is not moved between sectioning and ion/electron imaging.

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3D FIB-TOF Imaging of Solid Oxide Fuel Cell:

SOFC

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Full Chemical Characterization of a SOFC

With the TRIFT mass analyzer, the full mass spectrum is collected at every image pixel. There is no

need to use delayed extraction in order to obtain high collection efficiency or uniform signal for

imaging.

Ion-Induced SE Image

PrS

rCo

Ox

Gd

-do

ped

CeO

x

Sc-s

tab

ilize

d Z

rOx

All 14 elements present in the matrix (not including 69Ga/71Ga) are detected.

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Isotopic abundances are used to confirm peak assignments.

Example showing isotopic identification of Sr, Y and Zr.

There is high confidence for the identification of Sr, Y and Zr based on the

expected isotopic distributions. There is also high confidence for the

identification of Li, B, Na, Mg, Al, Si, K, Sc, Ni, Co, Ce and Pr.

Minor isotopes of Gd were used for imaging due to interferences.

84 86 88 90 92 94 96

ôòSr ôóSr

ôôSr

Y

õìZr

õíZrõîZr õðZr

õòZr84Sr

Identification of Matrix Components

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direction

of FIB

sectioning

Sr+, Ce+, Zr+ and K+ iso-surface overlay.

Note K+ decorating the void surfaces.

Imaged volume is 50 mm x 50 mm x 10 mm.

3D FIB-TOF Imaging of a SOFC

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Optional MS/MS for High Mass, Unambiguous

Peak Identification

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Practical mass resolution of polymers/tissue ~ 10,000 m/Δm.

Mass accuracy is limited to ~ 10 - 50 ppm.

Given the practical mass resolution and mass accuracy limits, it is not possible to

unambiguously determine the chemical formula of an ion above ~ m/z 200.

Additionally, there is no way to resolve overlapping peaks and isobaric (same nominal

mass) molecular ions at high mass.

Why is MS/MS Required in TOF-SIMS?

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TOF-SIMS Parallel Imaging MS/MSTrue Parallel and SynchronousMS1 and MS2 Data Acquisition

Pulse counting TOF provides greatest

speed and sensitivity

Full MS1 and MS2 mass spectra collected

at every image pixel

Narrow mass precursor selection window

(m/z 1 at m/z 500) for user selection of12C vs 13C composition

Parallel Imaging MS/MS available for

imaging, mosaic mapping, and depth

profiling

High conversion efficiency of precursors

with high energy collision induced

dissociation (CID)

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PET (poly (ethylene terephthalate)) film heated to 150-170 oC for 2 hours.

Surface features appear as surface crystals in optical microscope and secondary

electron and secondary ion images.

What is the chemical composition of these features which have a common peak at

+m/z 577?

Analysis conditions

• 40 mm FOV; 256 x 256 pixels

• 6 nA Bi3+; unbunched

• 4.82 x1012 Bi3+/cm2; 13 min

Analysis of PET Surface Features

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Precursor Ion Selection of +m/z 577

MS1 Spectrum with Precursor Selector OFF

MS1 Spectrum with Precursor Selector ON

Precursor = m/z 577.13

MS1 Spectra Without and With 100% Precursor Ion Selection

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MS2 Compositional Peak Assignments

The +m/z 577 peak of heat-treated PET is confirmed to be ethylene terephthalate trimer.

The MS2 results are accomplished at < 5 mDa RMS mass deviation,

and 3.8 ppm mass accuracy at the precursor.

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MS2 Spectra are Generated with > 25% CID Precursor Ion Fragmentation

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High Lateral Resolution Parallel Imaging MS/MS

The +m/z 577 peak arises almost exclusively from the surface crystals, as emphasized in the parallel MS1

and MS2 images; the MS2 images are free of chemical noise.

C8H5O3+ (m/z 149)

Total Ion (+SIMS)

Total Ion (+SIMS)

C8H5O3+ (m/z 149)

C7H4O+ (m/z 104)

C7H4O+ (m/z 104)

MS

1M

S2

10 mm

10 mm

10 mm

10 mm

10 mm

10 mm

40 mm FOV; 256 x 256 pixels; 6 nA Bi3+; PIDD = 4.82x1012 Bi3

+/cm2; 13 minutes

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Measured Lateral Resolution at +m/z 577

MS1 Measured Lateral ResolutionDl80/20 = 172 nm

MS2 Measured Lateral ResolutionDl80/20 = 148 nm

40 mm FOV; 256 x 256 pixels; 6 nA Bi3+; 13 minutes

Unbunched (MS1 spectra) LIMG with < 100 nm beam size

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50 100 150 200 250 3000

0.5

1.0

1.5

2.0

Tota

l C

ounts

(x10

5)

70

58

42

336

21085 236 264

250 319196

126

182

168140

154

150x

98112

222 278 292306

[M - H]-

318

320

[M - CH4]-

[M - H2O]-

C4H7ON-

C3H4ON-

C2H4ON-

CON-

C5H8ON-

[M - NH3]-

MS2 (m/z scale)

208 224

-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2 -CH2-CH2-CH2

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Tandem MS of Erucamide -m/z 336

The MS2 results are accomplished at < 5 mDa RMS mass deviation.

CID of M-H precursor shows complete structure with possible C=C bond position.

www.phi.com 57


Comprehensive TOF-SIMS Options for Real World Samples

PHI nanoTOF II TOF-SIMS Unique features of the PHI nanoTOF II TOF-SIMS: • Elemental, isotope and...

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Transcript of PHI nanoTOF II TOF-SIMS Unique features of the PHI nanoTOF II TOF-SIMS: • Elemental, isotope and...