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Profilometry NNUM thematic seminar Analysis Wednesday 10 May 2017 Børge Holme SINTEF [email protected]

NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

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Page 1: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Profilometry

NNUM thematic seminar

AnalysisWednesday 10 May 2017

Børge Holme

SINTEF

[email protected]

Page 2: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Outline

•What is topography?

•Techniques for measuring topography

•White Light Interferometry (WLI)

• Atomic Force Microscopy (AFM)

•Summary: When to use which technique

2

Page 3: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Topography

New Zealand

and surrounding sea bed

100 µm100 km

Surface of a tooth with an amalgam filling

Topography can be measured on different scales!3

Page 4: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Techniques for measuring topography

Optical

Profilometry

1 m

1 mm

1 µm

1 nm

1 pm

Vert

ica

l m

easure

ment

ran

ge

Lateral measurement range

1 m1 mm1 µm1 nm1 pm

Projected

Stripes

Stylus

Profilometry

0.1 nm

1 cm

Atomic

Force

Microscopy

4

Page 5: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Profilometry (measuring topography)

•Stylus Profilometry• 2D systems [Mitutoyo]

• 3D systems [Dektak]

•Optical Profilometry• Chromatic Confocal Sensing [Stil, me]

• Confocal microscopy [Leica, Nikon]

• Focus variation [Sensofar]

• White Light Interferometry [Wyko, Zygo, Sensofar]

• Digital Holographic Microscopy [Lyncée Tec]

• etc.

me

Nikon

Mitutoyo

Sensofar

Dektak

5

Page 6: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Availability of instruments near you

Location Stylus ProfilometerAtomic ForceMicrosopes

OpticalProfilometer

NTNU NanoLab Dektak 150

Lund Nano Lab Dektak 6M

Chalmers (NFL) Tencor P15, Tencor AS500, DektakDimension 3100and ICON

Wyko NT1100

Uppsala (MSL) Dektak 150, Dektak XT Wyko NT1100

DanChip Dektak 8, Dektak XTADimension ICON PT

Sensofar

UiO Dektak

USN Dektak Wyko NT1100

Aalto DektakXT, Alpha

SINTEF DI MultiMode Wyko NT9800

6

Page 7: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

White Light Interferometry (WLI) WYKO (Veeco/Bruker) optical profiler

7

Page 8: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Vertical Scanning Interferometry (VSI)

•Height range: Several millimeters

•Noise level (3 nm) too high for very flat surfaces

8

Page 9: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Phase Shifting Interferometry (PSI)

• Low noise level (0.3 nm), good for flat surfaces

•Can not measure sharp steps

9

Page 10: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Objective lens

CCD

Camera

Upper mirror

Lower mirror

Beam splitter

White or green

LED

Sample surface

Interferometer {

WLI working principle

10

Page 11: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Pixel size vs. Optical resolution

Pixel size: 7.1 µm

Optical res: 3.8 µm

Pixel size: 97 nm

Optical res: 490 nm

Magnification: 2.5*0.55x=1.4x Magnification: 50*2x=100x

Undersampling: Pixels are larger than

optical resolution

Oversampling: Pixels are smaller than

optical resolution

11

Page 12: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Oversampling

Undersampling

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Page 13: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Limit for the surface steepness• If a dark and bright fringe fills the same pixel, the average is grey

so the interference is not detected.

• The practical maximum slope gives the steepest surface tilt that

can be measured:

Inte

nsit

y

Beginning of scan Later in scan

Cylindrical sample surface

Pixel size

on sample

pixelsizexz /nm 134arctan/arctan

13

Page 14: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Practical maximum slope between 2° and 35°

You need a high-magnification lens to see steep facets

If the surface has a high local

roughness, you may be able to

measure steeper slopes

14

Page 15: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Wrong step height if different materials

Be careful when measuring

• Transparent materials on a substrate (May give reflections from both surfaces)

• Different materials within the same image (Phase changes upon reflection)

Mo on Si:

Measuring 169 nm step

Covering the sample

with gold: 56 nm step

Height offset from material:

221

2arctan

40

4

nh

Soffset

n and are real part and

imaginary part of refractive index

15

Page 16: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Beware of artefacts near sharp steps

Step height profile display

batwings due to

• Light diffraction

• Shadowing

• Light reflection

• Lateral translation/tilting

during vertical scanning

A H

ara

sa

ki, J

Sch

mit

& J

C.W

ya

nt,

Ap

plie

d O

ptics,

39

, 2

10

7-2

115

(20

00

)

Measured profile

Real profile

16

Page 17: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Live demo of intermolecular forces

Atomic Force Microscopy (AFM)

17

Page 18: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

AFM working principle

AFM with optical microscope

Piezo for

X, Y, Z

scanning

of sample

Controller

Pie

zo

for

vib

ratio

n o

f

cantile

ver

PC

http://www.uclouvain.be/en-168791.html

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Page 19: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Cantilevers and tips

• Many types exist, for different applications

Particle Ø=9 nm

Magnetic

Electric

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Page 20: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Contact mode vs. Non-contact modehttp://p

ers

o.u

niv

-

lem

ans.f

r/~

bard

eau/laboLP

EC

/afm

/afm

intr

oduction.h

tml

• Contact mode used for hard surfaces

• Non-contact mode for soft surfaces or to detect softness contrast

Probing

repulsive

forces

Probing

attractive

forces

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Page 21: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Non-contact mode gives both Topography and Phase images

•Can study individual dislocations

Topography Phase

Displaying the same data in different ways: The absolute height and its derivative21

Page 22: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Lateral Force Microscopy (LFM)

Measuring topography

Inte

rface P

hysic

s G

roup,

Leid

en Institu

te o

f P

hysic

s

AFM LFM

22

Measuring frictional forces

Page 23: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Useful for distinguishing between polymer materials

http://www.nanotribo.org/research/polymer_blends

AFM LFM

Lateral Force Microscopy (LFM)

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Page 24: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Using AFM to study MEMS device

HiVe Master student Huy Quoc Nguyen came to Oslo to use the AFM at SINTEF Materials and Chemistry

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Page 25: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Using AFM to study MEMS device

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Page 26: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

WLI + AFM on SAPO-34 catalyst grains

• SEM images show nearly cubic grains

• The shape can be related to the crystal structure

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Page 27: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

Relating the pentagonal growth spirals to structural details

Børge Holme, Pablo Cubillas, Jasmina Hafizovic Cavka, Ben Slater, Michael W. Anderson, Duncan Akporiaye

Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy

Crystal Growth & Design 10, 2824-2828 (2010) doi: 10.1021/cg9016118

WLI + AFM on SAPO-34 catalyst grains

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Page 28: NNUM thematic seminar Analysis · 2017-09-14 · Growth mechanisms in SAPO-34 studied by White Light Interferometry and Atomic Force Microscopy Crystal Growth & Design 10, 2824-2828

When to use which technique?

•Use AFM when you

• need to see lateral details < 1 µm

• need info on surface softness or friction

• need info on magnetic or electrical properties

• want to interact physically with the sample

• Use WLI/Stylus when you

• want to measure rough surfaces or step heights >10 nm

• want images larger than 100 µm

• want fast imaging

• want easy quantification of heights

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