![Page 1: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/1.jpg)
Cellulose Nanocrystal Cellulose Nanocrystal Characterization by AFMCharacterization by AFM
RoyaRoya LahijiLahiji Post Doc @NINTPost Doc @NINTX. X. XuXu Mechanical EngMechanical EngRyan WagnerRyan Wagner Mechanical EngMechanical Eng
Arvind RamanArvind Raman Prof. Mechanical EngProf. Mechanical EngRon ReifenbergerRon Reifenberger Prof. PhysicsProf. Physics
Robert MoonRobert Moon Forest Products LabForest Products LabPurduePurdue-- Materials EngMaterials EngBirck Nanotechnology CenterBirck Nanotechnology Center
2009 2009 IntnIntn’’ll Conf. on Nanotechnology for the Forest Products Industry, Conf. on Nanotechnology for the Forest Products Industry, June 24June 24--26, 2009, Edmonton, Alberta, Canada26, 2009, Edmonton, Alberta, Canada
![Page 2: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/2.jpg)
OutlineOutline
MotivationMotivationAtomic Force Microscopy (AFM)Atomic Force Microscopy (AFM)ResultsResultsSummarySummary
![Page 3: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/3.jpg)
Crystalline
Disordered
Aci
d H
ydro
lysi
s
Cellulose Nanocrystals (CNCs)Cellulose Nanocrystals (CNCs)
Wood cellulose nanocrystals, Wood cellulose nanocrystals, LiaLia StanciuStanciu
![Page 4: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/4.jpg)
Cellulose NanocrystalsCellulose Nanocrystals
BeckBeck--CandanedoCandanedo et al., et al., BiomacromoleculesBiomacromolecules, 2005, 6, 1048, 2005, 6, 1048
CNC Source Length Cross-Section Algal >1000nm 10-20nm
Bacterial 100 to >1000nm 5-10nm by 30-50nm
Cotton 200-350nm 5nm
Tunicate 100 to >1000nm 10-20nm
Wood 100-300nm 3-5nm
CottonCotton TunicateTunicate WoodWood
400nm
![Page 5: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/5.jpg)
Cellulose NanocrystalsCellulose NanocrystalsPropertiesProperties
![Page 6: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/6.jpg)
Cellulose NanocrystalsCellulose NanocrystalsPropertiesProperties
Encouraging Reinforcement Material
![Page 7: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/7.jpg)
CNC Functional UnitCNC Functional Unit““uniformuniform”” building block building block High Aspect ratioHigh Aspect ratio““GoodGood”” Mechanical propertiesMechanical properties““ReactiveReactive”” surfacesurface
Ideal Ideal GREENGREEN NanoparticleNanoparticle
Function
AvailabilityAvailabilitySustainabilitySustainabilityBiodegradableBiodegradableNonNon--petroleum Basedpetroleum BasedRenewableRenewableCarbon NeutralCarbon NeutralCarbon SequesteringCarbon SequesteringLow Health RiskLow Health Risk
EnvironmentEnvironmentAnimalAnimal
Green
Source: Ikkala, 2004.
![Page 8: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/8.jpg)
CNC CompositesCNC Composites
Composite PropertiesComposite PropertiesThermal StabilityThermal StabilityElastic ModulusElastic ModulusElongationElongationTensile StrengthTensile Strength
CNCCNC--Matrix InterfaceMatrix InterfacePercolation ThresholdPercolation Threshold
L. Oksman, Wood fiber 2007 conference
T. Zimmermann, Wood fiber 2007 conference
Not Reaching Full PotentialCNCs
No CNCs
![Page 9: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/9.jpg)
Percolation ThresholdPercolation Threshold
( )m
f
f
fE
VEVcE −+
= 11 ( ) mfffc EVEVE −+= 1
E
Volume Fraction Fiber
E1
E2
Capadona et al., Science, 2008.
0 1
Transverse Load Transfer
![Page 10: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/10.jpg)
Motivation: CNC CharacterizationMotivation: CNC Characterization
Not much known about CNCsNot much known about CNCsCharacterize Characterize ““building blockbuilding block””
Surface ChemistrySurface ChemistryMechanical PropertiesMechanical PropertiesWater Interaction Water Interaction UniformityUniformityCNC MorphologyCNC Morphology
Insight for Composite Processing & PropertiesInsight for Composite Processing & PropertiesLoad Transfer across Transverse SurfacesLoad Transfer across Transverse Surfaces
CNCCNC--Matrix InterfaceMatrix InterfaceCNCCNC--CNC InterfaceCNC Interface
Necessary for Predictive ModelingNecessary for Predictive Modeling
![Page 11: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/11.jpg)
Modulus of ElasticityModulus of ElasticityBased on Idealized Cellulose Based on Idealized Cellulose IIββ SimulationsSimulations
No Transverse Elasticity
![Page 12: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/12.jpg)
Developing Characterization ProtocolsDeveloping Characterization ProtocolsWhere we are atWhere we are at…….. ……where we need to be!where we need to be!
Approach: Approach: AFM TechniquesAFM TechniquesContinuum ModelingContinuum ModelingMolecular Dynamic ModelingMolecular Dynamic Modeling
Stone AgeF 1
![Page 13: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/13.jpg)
ObjectivesObjectivesDevelop CNC Measurement CapabilitiesDevelop CNC Measurement CapabilitiesAssess Uniformity of CNCsAssess Uniformity of CNCs
Surface ChemistrySurface ChemistryMechanical PropertiesMechanical Properties
InIn--situ with Changes in Relative Humiditysitu with Changes in Relative Humidity
![Page 14: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/14.jpg)
Scanning Probe Microscopy (SPM)Scanning Probe Microscopy (SPM)TipTip--Surface Interactions: Surface Interactions:
Physical contactPhysical contact Electrostatic forceElectrostatic forceLateral forceLateral force CapacitanceCapacitancevan van derder Walls interactionsWalls interactions ThermalThermalMagnetic forceMagnetic force
Ernst-Moritz-Arndt-University, Greifswald
Xintek
Tips Radius Tips Radius ~10nm (typical)~10nm (typical)~2nm (ultra sharp) ~2nm (ultra sharp)
![Page 15: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/15.jpg)
a) contact b) non-contact, small amplitude
c) intermittent contact, large amplitude
d) jumping
a) contact b) non-contact, small amplitude
c) intermittent contact, large amplitude
d) jumping
Imaging Modes Imaging Modes Contact Contact Vibrating (non & intermittent contact)Vibrating (non & intermittent contact)JumpJumpImaging under Gas or LiquidImaging under Gas or LiquidTip Chemical FunctionalizationTip Chemical Functionalization
Atomic Force Microscopy (AFM)Atomic Force Microscopy (AFM)
TopographyTopographyStiffnessStiffnessPullPull--off forceoff force
![Page 16: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/16.jpg)
AFMAFM--PurduePurdueNanotech AFMNanotech AFM
Si tips, 10nm tip radiusSi tips, 10nm tip radiusStiffness 0.65 N/m Stiffness 0.65 N/m (manufacturer)(manufacturer)
measure each tipmeasure each tip0.90.9--2.5N/m2.5N/m
Resonance Frequency: ~40KHzResonance Frequency: ~40KHzAtmosphere ControlAtmosphere Control
30% & 0.1% RH30% & 0.1% RH
Sharp AFM tips Sharp AFM tips (<10nm)(<10nm)Consistent tip shapeConsistent tip shapeDurableDurableLess expensiveLess expensiveImage & Property MeasurementImage & Property Measurement
![Page 17: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/17.jpg)
AFM TipsAFM TipsSharp Sharp (<10nm)(<10nm)
Good
Ultra Sharp Ultra Sharp (<2nm)(<2nm)Inconsistent tip shapeInconsistent tip shapeFragileFragileExpensiveExpensive
Bad
![Page 18: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/18.jpg)
10 nm
CNC: ~4CNC: ~4--10nm10nm
Mica
ArtifactsArtifactsChanging contact curvatureChanging contact curvatureEdge effectsEdge effectsAFM Tip dilationAFM Tip dilationAFM Tip bluntingAFM Tip bluntingAFM TipAFM Tip--toto--Tip changesTip changesMeniscus FormationMeniscus Formation
Idealized TipIdealized Tip--CNC Contact Geometry CNC Contact Geometry
AFM Tip
![Page 19: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/19.jpg)
AFM: ForceAFM: Force--DisplacementDisplacement
A
BC
DE
A
B
C
D E
F
G
H
F
G
H ApproachWithdraw
![Page 20: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/20.jpg)
AFM: ForceAFM: Force--DisplacementDisplacement
IIII -- PullPull--off Force off Force TipTip--Surface InteractionSurface InteractionAdhesionAdhesionCNCCNC--surface Chemistry?surface Chemistry?
II --Slope Slope CantileverCantilever--CNC stiffnessCNC stiffnessElastic ResponseElastic ResponseCNCCNC--Modulus?Modulus?
II
II
ApproachWithdraw
![Page 21: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/21.jpg)
Force DisplacementForce Displacement
90nm
Topography
Data CollectedData CollectedTopography, PullTopography, Pull--off, Stiffnessoff, Stiffness128 x 128 points128 x 128 pointsResolution based on mapping areaResolution based on mapping area
Maps Maps TopographyTopographyStiffnessStiffnessPullPull--off Forceoff Force
![Page 22: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/22.jpg)
~2wt% CNC suspension 400nm
Deposit ~10 μl of solution on to freshly cleaved mica sheet
DI wash
Sample PreparationSample Preparation
![Page 23: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/23.jpg)
TopographyTopography
Observations Observations Variable heightVariable height
RH influence?RH influence?not likelynot likelyScanScan--toto--scan ~1nm scan ~1nm not not ““exactlyexactly”” same tracesame trace
0.1% RH0.1% RH
012345678
0 20 40 60 80 100 120 140 160 180 200
Distance (nm)
Hei
ght (
nm) 0.1% RH
012345678
0 20 40 60 80 100 120 140 160 180 200
Distance (nm)
Hei
ght (
nm)
30% RH
0.1% RH
40nm
0.1% RH
×
40nm
0.1% RH
40nm
0.1% RH
×
30% RH30% RH
40nm
30% RH
×
40nm
30% RH
40nm
30% RH
×
×mica CNC
![Page 24: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/24.jpg)
StiffnessStiffness
1.4
1.5
1.6
1.7
1.8
1.9
2.0
0 20 40 60 80 100 120 140 160 180 200
Distance (nm)
Effe
ctiv
e St
iffne
ss (N
/m)
30% RH
0.1% RH
mica CNC
43nm
0.1% RH
43nm
30% RH
× ×
××
1.4
1.5
1.6
1.7
1.8
1.9
2.0
0 20 40 60 80 100 120 140 160 180 200
Distance (nm)
Effe
ctiv
e St
iffne
ss (N
/m)
30% RH
0.1% RH
30% RH
0.1% RH
mica CNC
43nm
0.1% RH
43nm
30% RH
× ×
43nm
0.1% RH
43nm
30% RH
× ×
××
Observations Observations Uniform along lengthUniform along lengthEdge effectsEdge effectsNo CNC height effectsNo CNC height effects
RH RH StiffnessStiffnessMica & CNCMica & CNCMeniscus InfluenceMeniscus Influence
30% RH30% RH 0.1% RH0.1% RH
![Page 25: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/25.jpg)
Force Displacement Force Displacement MOEMOEFo
rce
Distance
Cantilever B
ending
d
Nano Crystal
Approach
Tip Contact
Stiffness PlotsStiffness PlotsRemove Cantilever ContRemove Cantilever Contd several locations d several locations
d ~ Indentation Depth
![Page 26: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/26.jpg)
Mechanical Properties: Wood CNCsMechanical Properties: Wood CNCs
“AFM TIP”
Cellulose
RH=0.1% RH=0.1%
Transverse Modulus Transverse Modulus E=18E=18--50 50 GPaGPa, , Mean: 35 Mean: 35 GPaGPaMedian: 39.5 Median: 39.5 GPaGPa Reasonable, but how accurate?
Forc
e (n
N)
Forc
e (n
N)
Forc
e (n
N)
Forc
e (n
N)
Forc
e (n
N)
Indentation (nm) Indentation (nm)
Indentation (nm) Indentation (nm) Indentation (nm)
![Page 27: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/27.jpg)
Modulus of ElasticityModulus of ElasticityBased on Idealized Cellulose Based on Idealized Cellulose IIββ SimulationsSimulations
Within Range
![Page 28: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/28.jpg)
Mechanical Properties: Tunicate CNCsMechanical Properties: Tunicate CNCs
“AFM TIP”
Cellulose
Hertz ModelHertz Model Continuum ModelContinuum Model Molecular DynamicMolecular Dynamic
Extracting Elasticity:Extracting Elasticity:
Idealized Crystals:Idealized Crystals:
2/3CdF =
![Page 29: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/29.jpg)
Mechanical Properties: Tunicate CNCsMechanical Properties: Tunicate CNCs
806040200
1.41.31.21.1
1
Z[nm]
Nor
mal
forc
e[V
]30 nm
mica
CNC
-0.5 0 0.5 1 1.50
10
20
30
40
50
d (nm)
F (n
N)
Force Indentation Curve
fd cnck*a*(x+b)1.52/3)( bdakL +
0 0.2 0.4 0.6 0.8 10
1
2
3
4R2 Values of Fits
coun
t
R2
Transverse Modulus Transverse Modulus 30 Points along line 30 Points along line HertzHertzMean: 13 Mean: 13 GPaGPa ±± 9 9 GPaGPa (3 STD)(3 STD)
![Page 30: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/30.jpg)
Mechanical Properties: Tunicate CNCsMechanical Properties: Tunicate CNCs
![Page 31: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/31.jpg)
Mechanical Properties: Tunicate CNCsMechanical Properties: Tunicate CNCs
Transverse Modulus Transverse Modulus 100 Points along line 100 Points along line HertzHertzMean: 3 Mean: 3 GPaGPa ±± 5 5 GPaGPa (3 STD)(3 STD)
![Page 32: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/32.jpg)
51nm 706050403020100
10
8
6
4
2
0
X[nm]Z[
nm]
Analysis of Transverse FZ curves
0 0.005 0.01 0.015 0.02 0.0250
0.05
0.1
0.15
0.2
0.25
Doffset (V)
F (V
)
Force Indentation Curve Comparison of Mica vs. Mica FZ curve
![Page 33: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/33.jpg)
9080706050403020100
2
1.5
1
0.5
0
X[nm]Z[
nm]
51nm 302520151050
0.8
0.75
0.7
0.65
0.6
0.55
0.5
0.45
0.4
Z[nm]
Nor
mal
forc
e[V
]-0.01 0 0.01 0.02 0.030
0.05
0.1
0.15
0.2
0.25
0.3
0.35
Doffset (V)
F (V
)
Force Indentation Curve
![Page 34: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/34.jpg)
9080706050403020100
1.4
1.2
1
0.8
0.6
0.4
0.2
0
X[nm]
Z[nm
]
302520151050
0.8
0.75
0.7
0.65
0.6
0.55
0.5
Z[nm]
Nor
mal
forc
e[V
]
51nm
0 0.01 0.02 0.03 0.040
0.05
0.1
0.15
0.2
0.25
0.3
0.35
Doffset (V)
F (V
)
Force Indentation Curve
![Page 35: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/35.jpg)
9080706050403020100
1.5
1
0.5
0
X[nm]Z[
nm]
51nm 302520151050
0.8
0.75
0.7
0.65
0.6
0.55
0.5
Z[nm]
Nor
mal
forc
e[V
]0 0.5 1 1.5 2
0
5
10
15
20
D (nm)
F (n
N)
Force Indentation Curve
fd cncC*k*a*(x+b)1.5
0 0.2 0.4 0.6 0.8 10
1
2
3
4
5
6R2 Values of Fits
coun
t
R2
![Page 36: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/36.jpg)
51nm 80706050403020100
2.5
2
1.5
1
0.5
0
X[nm]Z[
nm]
302520151050
0.75
0.7
0.65
0.6
0.55
0.5
0.45
Z[nm]
Nor
mal
forc
e[V
]0 0.5 1 1.5
0
5
10
15
D (nm)
F (n
N)
Force Indentation Curve
fd cncC*k*a*(x+b)1.5
0 0.2 0.4 0.6 0.8 10
1
2
3
4
5
6R2 Values of Fits
coun
t
R2
![Page 37: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/37.jpg)
51nm 80706050403020100
1.4
1.2
1
0.8
0.6
0.4
0.2
0
X[nm]
Z[nm
]
302520151050
0.75
0.7
0.65
0.6
0.55
0.5
0.45
Z[nm]
Nor
mal
forc
e[V
]0 0.5 1 1.5
0
5
10
15
D (nm)
F (n
N)
Force Indentation Curve
fd cncC*k*a*(x+b)1.5
0 0.2 0.4 0.6 0.8 10
0.5
1
1.5
2
2.5
3R2 Values of Fits
coun
t
R2
![Page 38: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/38.jpg)
51nm 80706050403020100
1.2
1
0.8
0.6
0.4
0.2
0
X[nm]Z[
nm]
302520151050
0.75
0.7
0.65
0.6
0.55
0.5
0.45
0.4
Z[nm]
Nor
mal
forc
e[V
]0 0.5 1 1.5
-5
0
5
10
15
D (nm)
F (n
N)
Force Indentation Curve
fd cncC*k*a*(x+b)1.5
0 0.2 0.4 0.6 0.8 10
1
2
3
4R2 Values of Fits
coun
t
R2
![Page 39: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/39.jpg)
51nm 706050403020100
10
8
6
4
2
0
X[nm]
Z[Å
]
302520151050
0.75
0.7
0.65
0.6
0.55
0.5
0.45
0.4
Z[nm]
Nor
mal
forc
e[V
]0 0.2 0.4 0.6 0.8 1
-5
0
5
10
15
D (nm)
F (n
N)
Force Indentation Curve
fd cncC*k*a*(x+b)1.5
0 0.2 0.4 0.6 0.8 10
1
2
3
4
5R2 Values of Fits
coun
t
R2
![Page 40: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/40.jpg)
Summary Summary Key ObservationsKey Observations
Variable CNC Height ProfileVariable CNC Height ProfileUniform StiffnessUniform StiffnessInfluence of RH on measurementsInfluence of RH on measurements
Elastic Modulus EstimatesElastic Modulus EstimatesComplimentary Experimental & Modeling Complimentary Experimental & Modeling QualitativeQualitative
Wood: 18Wood: 18--50GPa (FEM)50GPa (FEM)Tunicate: 0Tunicate: 0--22 22 GPaGPa (Hertz)(Hertz)
Artifacts need to be accounted forArtifacts need to be accounted for……
![Page 41: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/41.jpg)
AcknowledgementsAcknowledgements
Forest Product Laboratory:Jim Beecher, Chris Hunt, Rick Reiner, Allan Rudie, Ron Sabo
Funding: Cooperative Agreement with Purdue Funding: Cooperative Agreement with Purdue
Funding: Seed Grant Funding: Seed Grant
![Page 42: Cellulose Nanocrystal Characterization by AFM · 2009-07-29 · Cellulose Nanocrystal Characterization by AFM Roya Lahiji Post Doc @NINT X. Xu Mechanical Eng Ryan Wagner Mechanical](https://reader031.vdocuments.us/reader031/viewer/2022011913/5faafc65e39b1949ee0a7eed/html5/thumbnails/42.jpg)
Thank YouThank You
Questions ?