Recent Developments in Canadian Nanotechnology Measurement ...

Recent Developments in Canadian

Nanotechnology Measurement Science and

Nanotechnology Measurement Science and

ISO Standards Initiatives

Je

nn

ife

r E

. D

ec

ke

r

Tri-National Workshop on Standards for Nanotechnology

Queretaro, Mexico

12 Feb 2009

Intr

od

ucti

on

•Elements required to enable

the platform

of

nanotechnologies:

©2009 NRC-INMS, Decker

–Traceability to the SI

–Reference

Materials/Artefacts

–Documentary Standards

Nan

ote

ch

no

log

y

Norio Taniguchi, Tokyo Science University

–First to use the term

in 1974, C

olle

ge

In

tern

atio

na

l p

ou

r la

Re

ch

erc

he e

n P

rod

uctiq

ue

(C

IRP

)

"Na

no

-te

ch

no

log

y m

ain

ly c

on

sis

ts o

f th

e p

roce

ssin

g o

f

©2009 NRC-INMS, Decker"N

an

o-t

ech

no

log

y m

ain

ly c

on

sis

ts o

f th

e p

roce

ssin

g o

f

se

pa

ratio

n, co

nso

lida

tio

n, a

nd

de

form

atio

n o

f m

ate

ria

ls b

y

on

e a

tom

or

on

e m

ole

cu

le."

D.M. Eigler, E.K. Schweizer

“Positioning single atoms with a

scanning tunneling microscope”

Nature 344524-526 (1990)

Nan

ote

ch

no

log

ies

•>800 nano-Consumer Products

–N

an

o-o

bje

cts

in

clu

de

: p

art

icle

s, tu

be

s,

rop

es,

su

rfa

ce

s. .

.

–O

EC

D ‘sh

ort

lis

t’ o

f 1

4 m

an

ufa

ctu

red

na

no

ma

teri

als


–O

EC

D ‘sh

ort

lis

t’ o

f 1

4 m

an

ufa

ctu

red

na

no

ma

teri

als

•How to characterize them?

–S

ele

ct so

me

ou

t o

f m

an

y s

cie

ntific m

eth

od

s

Nanotechnology Consumer Products Inventory, Woodrow

Wilson International Center for Scholars

R&

D +

Sta

nd

ard

s f

or

Man

ag

ing

Ris

k

•U

niq

ue

id

en

tifica

tio

nof these nanomaterials is e

sse

ntia

lfor

relia

ble

scientific investigation

1.Establish a n

am

efor the unique nano-object

(ISO/TC229 JWG1, JWG2)


(ISO/TC229 JWG1, JWG2)

2.Establish a b

ody o

f R

&D(identification, characterization,

predictive toxicology, etc.) to indicate if this object is safe or

toxic (international R&D cooperation, OECD)

3.Establish s

tandard

meth

odsto identify and report the

characteristics of this entity (ISO)

4.

Inte

rnational consensusagreement on t

esting p

roto

colsis

required for trade (ISO/TC229 W

G3, OECD)

Do

cu

men

tary

Sta

nd

ard

s

•Standards promote levels of quality, safety, reliability, efficiency

and interchangeability

•ISO/TC229, IEC/TC113 Nanotechnologies


•ISO/TC229, IEC/TC113 Nanotechnologies

–JWG1 Term

inology & Nomenclature: Canada

–JWG2 Measurement & Characterization: Japan

–WG3 Health, Safety, Environment: USA

–WG4 Product Specifications: China

Iden

tifi

cati

on

of

a

Measu

ran

d

•IS

O/T

C 2

29 W

G 3

/PG

5 P

roje

ct:

Gu

idan

ce o

n p

hysic

o-c

hem

ical

ch

ara

cte

rizati

on

of

en

gin

eere

d n

an

o-

ob

jects

fo

r to

xic

olo

gic

assessm

en

t

Leader: Dr. Richard Pleus (USA)


•Purpose:What is theintended application

of the m

easurement?

•Measurements to be compared with each

other should betraceable to the same

reference (SI units)

•Available m

easuring instrumentsand

reference m

aterials

ISO FDIS 9276-6 Descriptive and

quantitative representation of particle

shape and m

orphology

Recen

t D

evelo

pm

en

ts

•M

etr

olo

gic

al C

on

ten

t

ISO

/TC

22

9 S

tan

da

rds

:Two

documents to steer towards

more comprehensive

metrological content

•Category A Liaison with BIPM

–Definition of the base SI units

+ realization at the nanoscale

–International comparisons for

validation of measurements


metrological content

–Check List: Used prior to

accepting draft standard for

ballot

–Guidance on M

etrological

Content: harm

onize content &

term

inology

validation of measurements

Lin

e S

cale

s:

IEC

/TC

113


•Artificial gratings used in nanotechnology: description and

measurement of dimensional quality parameters

•Refers to latest international comparisons of national metrology

institutes:

–C

CL

-S3 (

Nan

o3), CCL-S1 (Nano4 1D gratings), CCL-S5 (Nano5 2D grids)

NR

C-I

NM

S In

itia

tives

•Chairman of Metrology Study Group + participate in Strategy Group of

ISO/TC229 JWG2

•Canadian Advisory Committee Mirror Chairmanship of JWG2

•Negotiated Category A Liaison between ISO/TC229 & International


•Negotiated Category A Liaison between ISO/TC229 & International

Bureau of Weights and Measures (BIPM)

•Pre-treatment protocols for single-walled carbon nanotubes

–Canada-US-UK collaboration

•Liaison with Canadian delegation to OECD

•Primary M

etrology = Direct traceability to the SI

•Development of metrological instrumentsand methods

•Client calibration services andreference m

aterials; intrinsic

NR

C-I

NM

S P

rog

ram

of

Acti

vit

ies


•Client calibration services andreference m

aterials; intrinsic

standards

•Rigorous validation of measurements impacts ability to interpret

results

–international round-robin comparisons with other national

metrology institutes

NR

C-I

NM

S R

&D

Pro

jects

•Reference standard artefacts for length

calibration

•Metrological Atomic Force Microscope for

traceable custom shape/size

•Quantum-based Voltage standards


•Quantum-based Voltage standards

•Optical Characterization of Nanomaterials

•Dielectric measurements of

nanocomposites

•FTIR Spectroscopy & thickness

measurement

•Molecular imaging: Detection of

nanoparticles in biological systems

1-D

imen

sio

nal G

rati

ng

Pit

ch

•Measurements traceable to the

definition of the metre through

wavelengths of light by:

–Optical diffraction technique

–Interferometer coupled to


–Interferometer coupled to

microscope stage translation

•Important characteristics

–Spatial uniform

ity of grating pitch

–Flatness of substrate

–Accurate angle measurement

Ato

mic

Fo

rce

Mic

rosco

pe (

AF

M)

•“Feeling” the surface with a

mechanical probe

–Topography (mechanical

contact)

–Electrostatic force


–Magnetic force

–Measure additional quantities

e.g. therm

al microscopy

•Develop techniques & m

ethods

for accurate measurement with

commercial AFMs

–Reference m

aterials: grating

pitch, step height, line width

Metrological

Ato

mic

Fo

rce M

icro

sco

pe

•Measurement errors in measured points of

a grid in relationship to a perfect ‘true’ grid

(dashed lines)

•Advance technological developments in

metrological SPM instrumentation and in so


metrological SPM instrumentation and in so

doing, provide highest accuracy and

precision measurement capability to clients

•In-house development project:

–motion control stage built on 2-D flexure

stage

–x,y,z co-ordinates read using homodyne

interferometers

–autocollimators sense sample

orientation

Inte

rnati

on

al

Co

mp

ari

so

ns

•Two Comparisons:

–National Metrology

Institutes: Canada,

Taiwan, Germ

any,

Switzerland

Lab3

Lab4

Lab6

2468

Deviation from Nominal Pitch /nm

350 nm Pitch

Industry Comparison


Switzerland

–Industry Labs: Canada +

Taiwan

•R

ep

rod

ucib

ility& g

lob

al

co

mp

ara

bili

tyachieved

through traceability to the SI

Lab1

Lab2

Lab4

Lab5

-4-20

Deviation from Nominal Pitch /nm

Rig

oro

us S

tati

sti

cal

Meth

od

s f

or

An

aly

sis

of

Co

mp

ari

so

n R

esu

lts

Resampled Lab Values' PDFs and Pool: Not constrained by null hypothesis

1.E-01

1.E+00

PDFs and Pool

Lab1

Lab2

Lab3

Lab4

Lab5

Lab6

Pool

Gaussian(-4.1508,4.2608,0.9)

Student(0.3513,0.0853,134,0.899)

NRC Monte Carlo Toolkit

http://inms-ienm.nrc-

cnrc.gc.ca/qde/montecarlo/


Lab1

Lab2

Lab3

Lab4

Lab5

Lab6

⟨En2⟩ j

P({Claims} exceed experiment by chance)

Lab1

2.6

87

1.96

-1.44

4.83

2.53

-0.70

7.2

21

P( ⟨E

n2⟩ j=1 > 7

.221 ) = 3.24%

Lab2

-1.96

1.9

20

-2.41

-1.77

-1.29

-2.00

3.6

85

P( ⟨E

n2⟩ j=2 > 3

.685 ) = 6.37%

Lab3

1.44

2.41

1.8

24

1.77

2.35

0.32

3.3

27

P( ⟨E

n2⟩ j=3 > 3

.327 ) = 10.29%

Lab4

-4.83

1.77

-1.77

2.5

94

1.77

-0.95

6.7

26

P( ⟨E

n2⟩ j=4 > 6

.726 ) = 3.46%

Lab5

-2.53

1.29

-2.35

-1.77

1.9

47

-1.49

3.7

89

P( ⟨E

n2⟩ j=5 > 3

.789 ) = 13.09%

Lab6

0.70

2.00

-0.32

0.95

1.49

1.2

40

1.5

38

P( ⟨E

n2⟩ j=6 > 1

.538 ) = 24.77%

Experimental pair-difference

En i

j = (x

i- x

j) / (u

i2+

uj2)1/2

4.3

81

P( (2APD > 4

.381 ) = 5.78%

RM

S E

n j = [ ( i=1N (

En ij)2 / (N

-1) ]1/2

564.261

P( (2SM > 564.261 ) = 33.60%

7.212

P( (2WM > 7.212 ) = 3.24%

81.916

P( (2MED > 81.916 ) = 31.84%

1.E-03

1.E-02

-100.00

-50.00

0.00

50.00

100.00

La

b V

alu

es

for

Re

sa

mp

led

Me

asu

ran

ds

PDFs and Pool

cnrc.gc.ca/qde/montecarlo/

NR

C-I

NM

S R

&D

Co

llab

ora

tio

ns

•NRC Cross Institute Metrology for Nanotechnology

(INMS-IMS-NINT-SIM

S)

•Interfacial Force M

icroscope

•Nanoimprint Lithography applied to artefact standards

•Intrinsic length standards


•Intrinsic length standards

•Soft materials

•NRC-NSERC-BDC Quantum Candela

•Metrological photon counting to support calibrations (single-photon

detectors)

•Nanodielectrics & DiagnosticsElectrical + Electronics Industries

(INMS-IMI)

•Reference Materials for Single-walled Carbon Nanotubes

(INMS-SIMS-IRC)

Inte

rnati

on

al

Co

llab

ora

tio

ns

•Canada-USA Reference Materials for

Single-W

alled Carbon Nanotubes

–Sample preparation protocols for

reproducibleresults


•Canada-USA-UK Sample Preparation

Protocols for Single-W

alled Carbon

Nanotubes

–Multiple methods

–Precursor to international

comparison for validation +

documentary standards

•Molecular Imaging

NR

C S

imard

et

al.

Up

co

min

g M

eeti

ng

s

•T

ri-N

ati

on

al W

ork

sh

op

Sta

nd

ard

s

& N

an

ote

ch

no

log

y

–NRC (Ottawa) 2010: Reference

Materials

Chairs: Sturgeon & Simard


Chairs: Sturgeon & Simard

–North American Partnership

Platform

(NAPP)

•In

tern

ati

on

al c

on

fere

nc

e o

n t

he

sc

ien

ce

an

d a

pp

lic

ati

on

of

na

no

tub

es(NT10) –Satellite

Meeting on Reference Materials

Sta

nd

ard

s &

Metr

olo

gy

Su

pp

ort

Nan

ote

ch

Develo

pm

en

t•

Na

no

scie

ncecan only evolve into

na

no

tech

no

log

yonce the

measurement problems and

metrology are under control

–T

race

ab

ility

to

th

e S

I


–T

race

ab

ility

to

th

e S

I

–R

efe

ren

ce

ma

teri

als

•Economic impacts from product

development and commercialization

demand d

ocu

me

nta

ry s

tan

da

rds

•Workplace safety, environment and

health are key drivers

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