recent developments in canadian nanotechnology measurement
TRANSCRIPT
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
©2009 NRC-INMS, Decker
–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)
©2009 NRC-INMS, Decker
(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
©2009 NRC-INMS, Decker
•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)
©2009 NRC-INMS, Decker
•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
©2009 NRC-INMS, Decker
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
©2009 NRC-INMS, Decker
•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
©2009 NRC-INMS, Decker
•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
©2009 NRC-INMS, Decker
•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
©2009 NRC-INMS, Decker
•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
©2009 NRC-INMS, Decker
–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
©2009 NRC-INMS, Decker
–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
©2009 NRC-INMS, Decker
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
©2009 NRC-INMS, Decker
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/
©2009 NRC-INMS, Decker
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
©2009 NRC-INMS, Decker
•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
©2009 NRC-INMS, Decker
•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
©2009 NRC-INMS, Decker
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
©2009 NRC-INMS, Decker
–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
©2009 NRC-INMS, Decker