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Nano-additives for Intumescent Materials. Jeffrey W. Gilman Materials and Products Group Fire Science Division NIST. Outline. Background Nano-additives for intumescent materials High Throughput Methods Image analysis – confocal Flammability of polymers Gradient coatings. - PowerPoint PPT Presentation
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Jeffrey W. GilmanMaterials and Products Group
Fire Science DivisionNIST
Nano-additives for Nano-additives for Intumescent MaterialsIntumescent Materials
• Background Background • Nano-additives for intumescent materialsNano-additives for intumescent materials• High ThroughputHigh Throughput MethodsMethods
• Image analysis – confocalImage analysis – confocal• Flammability of polymersFlammability of polymers• Gradient coatingsGradient coatings
OutlineOutline
Gasification of Polystyrene Layered-silicate NanocompositesGasification of Polystyrene Layered-silicate Nanocomposites
Char or
Coke Formation
0
200
400
600
800
1000
1200
1400
1600
0 120 240 360 480 600
PP intercalated + delaminated (mass fraction 2 % silicate) PP-g-MA (mass fraction 0.4 % MA)
PP intercalated + delaminated (mass fraction 4 % silicate)
Hea
t Rel
ease
Rat
e (k
W/m
2 )
Time (seconds)
Flux = 35 kW/m2
Nano-additivesNano-additives
Layered Double Hydroxide
Mg(OH)64-
Al(OH)63
-
POSSCarbon nanotubes
Coughlin-U Mass
Bellayer - NIST
Zammerano-Chimteclab
Layered Silicates
Nano silica
Kashiwagi - NIST
New additives for intumescent New additives for intumescent materialsmaterials
Layered Layered Double HydroxidesDouble Hydroxides
Imidazolium Imidazolium DicyanamideDicyanamide
New Char Forming New Char Forming SystemsSystems
Epoxy LDH nanocomposite coating
Polyurea LDH nanocomposite coating
Parameter Space (~ 10Parameter Space (~ 106 6 Experiments) for Polymer Experiments) for Polymer NanocompositesNanocomposites
Fluorescence Monitoring of ExfoliationFluorescence Monitoring of Exfoliation
Laser Scanning Confocal Microscope; Laser Scanning Confocal Microscope; 100s of images, 200-1000 nm slices100s of images, 200-1000 nm slices
Charles Wu, Lipiin SungCharles Wu, Lipiin Sung
0 20 40 60 80 100 120 140 160 180Distance (µm)
0
50
100
150
200
250
Intensity
Profile
20 μm
Distance (μm)
0
20
40
60
80
100
120
140
0 50 100 150
Inte
nsity
(a.u
.)
PS + 0.5% MWNT (NB) 1 min
+ 2σ x
x
- 2σ
x
x
Confocal Laser Scanning Fluorescence MicroscopyConfocal Laser Scanning Fluorescence Microscopy
PC Mg6Al/DBS+MO Daca 7 min – Step size Confocal 0.40 micron
Projection
Confocal Imaging of LDH NanocompositesConfocal Imaging of LDH Nanocomposites
EVA(18%VA)/DBS+MO Daca 7 min – Step size Confocal 0.4 micron
Projection
0 20 40 60 80 100 120 140 160 180Distance (µm)
0
50
100
150
200
250
Intensity
Profile
20 μm
Distance (μm)
0
20
40
60
80
100
120
140
0 50 100 150
Inte
nsity
(a.u
.)
0 20 40 60 80 100 120 140 160 180Distance (µm)
0
50
100
150
200
250
Intensity
Profile
20 μm
Distance (μm)
0
20
40
60
80
100
120
140
160
0 50 100 150
Inte
ns
ity
(a
.u.)
0 20 40 60 80 100 120 140 160 180Distance (µm)
0
50
100
150
200
250
Intensity
Profile
20 μm
Distance (μm)
0
20
40
60
80
100
120
0 50 100 150
Inte
nsity
(a.u
.)
0 20 40 60 80 100 120 140 160 180Distance (µm)
0
50
100
150
200
250
Intensity
Profile
20 μm
Distance (μm)
0
20
40
60
80
100
120
140
0 50 100 150
Inte
nsi
ty (a
.u.)
PS + 0.5% MWNT (NB) 10 min
PS + 0.5% MWNT (NB) 1 min
PS + 0.5% DMHDIm-TFB (NB) 10 min
PS + 0.5% MWNT + 0.5% DMHDIm-TFB (NB) 10 min
- The lower intensity regions are possibly due to a MWNTquenching mechanism
-The lower (2/m) the more homogeneous the sample
- Complements the TEM data
2σ/ m = 0.38
Confocal Laser Scanning Fluorescence MicroscopyConfocal Laser Scanning Fluorescence Microscopy
2σ/ m = 0.18 2σ/ m = 0.09 2σ/ m = 0.09
High Throughput Gradient Approaches
Schematic drawings flame spread on homogenous sample exposed to a gradient flux intensity (Workflow 1)
Flame SpreadFlame Spread
Low
High
Different Critical Fluxes for Flame-SpreadDifferent Critical Fluxes for Flame-Spread
PS/APP-PER
50 %50 %40 %20 %
5 %
8
16
24
32
40
48
0 100 200 300 400 500 600 700 800
HIFT mid-line flux (kW/m2)
HIFT flux (kW/m2)
distance mm
50 % 40 % 5 % 20 %
High Throughput Gradient Approaches
Simultaneous flame spread (MFFS)and heat release measurements using the Cone Calorimeter
HeatRelease rate
Flux
Conventional Property Characterization:Tensile testing, DMA, UL94, Cone calorimetry
High Throughput Property Characterization:Nanoindentation, flame spead,, rapid calorimetry
High Throughput Material characterization: on-line sensors,Micro-FTIRMicro-FTIR, COnfocalCOnfocal, UV-Vis spectra
Conventional Material Characterization:TEM, GPC, XRD…
Polymers, catalysts, nano-additives, co-additives, and processing variables
Compare results
Compare results
Gradient and Gradient and
Rapid CoatingRapid Coating
SystemSystem
High Throughput System-2 High Throughput System-2 Gradient CoatingsGradient Coatings
NIST Project team:Cindy Montgomery, Dick Harris
samples
Computer control panel
FluidicSystems (CEO:Bruce Menck)
High Throughput ScreeningHigh Throughput Screeningof Military Aircraft Topcoat Accelerators of Military Aircraft Topcoat Accelerators ProjectProjectGradient #3, 1000, 1600, 32s, (2100- 2551)/(2700-3040)cm-1
Naomi EidelmanNaomi Eidelman
ISO/CH2
target
0.07
0.67
0.39
Accelerator concentration (% x 10-3)
Cu
rin
g t
ime
(hr)
1.50 1.55 1.60 1.65 1.70 1.75 1.8011
21
16
32
42
37
55
65
60
102
112
107
155
165
160
ConclusionsConclusionsNano-additives enhance the performance of Nano-additives enhance the performance of
intumescent systemsintumescent systems
Gradient Spray Coating Facility provides Gradient Spray Coating Facility provides rapid sample preparationrapid sample preparation
FTIR-Microscopy, Optical probes and FTIR-Microscopy, Optical probes and Confocal are inherently High Throughput vs. Confocal are inherently High Throughput vs. alternativesalternatives
Gradient Flux Flame Spread and Tign vs Gradient Flux Flame Spread and Tign vs Flux allows HT evaluation of FRFlux allows HT evaluation of FR
Research TeamResearch TeamRick Davis, Takashi Kashiwagi, Marc Nyden, Richard Harris, Greg Linteris, John Rick Davis, Takashi Kashiwagi, Marc Nyden, Richard Harris, Greg Linteris, John
Shields, Walid Awad, Lori Brassell, Michael Smith - BFRL/NIST; Shields, Walid Awad, Lori Brassell, Michael Smith - BFRL/NIST; David VanderHart, Atsuchi Asano, Anthony Bur - MSEL/NISTDavid VanderHart, Atsuchi Asano, Anthony Bur - MSEL/NIST
Joe Lichtenhan –Hybrid PlasticsJoe Lichtenhan –Hybrid PlasticsPaul Maupin –DOEPaul Maupin –DOEPaul C. Trulove and Hugh DeLong -Air Force Office of Scientific ResearchPaul C. Trulove and Hugh DeLong -Air Force Office of Scientific ResearchDoug Fox – NRL, Naval AcademyDoug Fox – NRL, Naval Academy
Funding ($):Funding ($):Air Force Office of Scientific ResearchAir Force Office of Scientific Research (ISSA - (ISSA - AFOSR- ISSA-01-0001AFOSR- ISSA-01-0001 ) )
AFRL – High Throughput Screening of Military Aircraft AcceleratorsAFRL – High Throughput Screening of Military Aircraft Accelerators - Joel Johnson - Joel Johnson
High Throughput Methods for Materials Flammability ConsortiumHigh Throughput Methods for Materials Flammability Consortium (AFRL, FAA, Rhodia, Dow) (AFRL, FAA, Rhodia, Dow)
FAAFAA, Richard Lyon at William J. Hughes Technical Center (IAA- DTFA03-99-X-90009), Richard Lyon at William J. Hughes Technical Center (IAA- DTFA03-99-X-90009)
