the use of dispersed nanosized functional materials in ... · water borne coating to fiberglass...
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John DuBYK USA
2008 International Conference on Nanotechnology for the Forest Products Industry
The use of dispersed nanosized functional materials in Coating applications
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•Relationship between preparation and shape
•Why dispersion of nano particles is important.
•How Al2O3 and SiO2 influence scratch resistance
•What types of coatings can benefit from nano.
•Improvement of UV protection in Paint and Plastic using nano
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Unique Nanoparticles
Sol-GelFlame Pyrolysis
Precipitated Milled
Plasma
• Nanoparticles from other methods may overlap, but do not share the same particle properties
• Plasma-produced nanoparticles have unique properties
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Comparative Processes Alumina
Flame SynthesisAlumina
Plasma Vapor Alumina
Precipitated Alumina
Spherical & discrete particles
Irregular, aggregated & agglomerated
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How toDisperse?Stabilize?
Functionalize?
NANOPARTICLES
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Wetting and Dispersing Process
2Dispersion
1Wetting
3Stabilization
Displace air and
wet particleEnergy input
Prevent re-flocculation
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July 2007 Page 7, Robert McMullin Manager Nanotechnology NAFTA
Wetting Additives
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July 2007 Page 8, Robert McMullin Manager Nanotechnology NAFTA
Dispersing Additives
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W&D Additives vs. Covalent Surface Treatment
Covalent Surface Treatment
W&D Mechanism
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Impact of W&D–additive on deflocculation / stabilization
System: 2 Pack Acrylate / NCO
No W&D–additive W&D–additive
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Functionalized Nanoparticles
Nanoparticle Coremechanical, chemicalelectrical
Nanoparticle ShellSolubility
Resin Compatibility
• Nanoparticle Shellreactivity ↔ compatibility
Nanoparticle CoreMechanical Prop.Chemical Prop.Electronic Prop.Biological Prop.
• Tailored Interface
Nanoparticle Boundary Phase
SolubilityReactivity
Compatibility
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Role of Boundary Phase
Expansion of boundary phase on Nanoparticles provides •compatibility•extends functionality (e.g. scratch resistance) •lower loading requirements
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Dispersing NanomaterialsExample “Baytubes®”
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Dispersing Carbon NanotubesCooperation with Bayer Material Science
1% MWCNTs in PMA
Without dispersant
1% MWCNTs in PMA
With dispersant
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0,1% CNT in PMA0,05% W&D
0,1% CNT in PMA0,1% W&D
0,1% CNT in PMA0,15% W&D
Wetting & Dispersing – Key Factor in Stabilization
Increasing Stability
Pictures weretaken 2 monthsafter dispersing
Microscopicimages
Decreasing Agglomerate Size
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Dispersing NanomaterialsExample ZnO
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Dynometer Testing – 5% ZnO dispersions to estimate the time of settlement Crystal density 5.6g/cc
0
0.05
0.1
0.15
0.2
15 M 30 m 45 m 1 HR 1 1/2Hr
2 Hr
5% 60 nm nottreated5% 60 nm
5% 40 nm
5% 20 nm
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Hot box testing – 7 days at 140o F
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Why Nano Dispersions Work for Scratch and Wear Resistance
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Mechanisms of Scratch Resistance - Boundary Phase Properties
homogeneously distribution of NP in coating system• good improvement of scratch resistance properties• good long time stability• good elasticity
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Nanotechnology Advantage
1 wt% particles dispersed in a coating:
1 um diameter = 4 particles
20 um
20 um 20 nm diameter = 10,000 particles
Nanotechnology enables more particles per unit area, and significantly decreases particle-particle separation
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Scratch Damage of Polymeric Materials
Visibility
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0 % 0.75 % 1.75 % 3 %
Scratch Profiles at 49 mN for Filler B systemNB-3610 / 20 nm Alumina / ST 2
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Unfilled
NB-3650
NB-3610
~ 2 % NanoparticlesScratch Results – Images
Control 25 nm Al2O3
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Scratch Resistance of Aqueous Acrylic AD Coating High Gloss over time Gloss 20 ° [%], ASTM D 2486 abrasion tester, 100 cycles 00 steel wool
01020304050607080
No Rubs 24 hr 48 hr 72 hr 96 hr
Control 1% 40nm Al2O3 1% 25 nm Al2O3
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Effect of Nano-particles in Aqueous AD Coatings
1.0% Loading of Nano Alumina• improves scratch resistance (gloss retention)• 20nm alumina imparts early resistance properties (24 hrs)• 40 nm requires longer dry time 96 hours for same
properties
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Scratch Resistance of Aqueous Acrylic/Urethane AD Satin over time 25% PUD 75% Acrylic
Gloss 60 ° [%], ASTM D 2486 abrasion tester, 100 cycles 00 steel wool
048
12162024
No Rubs 96 hr 100 cycles
Control Wax 1% 40nm Al2O3 1% 60 nm Al2O31% 60 nm Al2O3 + wax 1% 40nm Al2O3 + wax
Best
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Taber Abrasion
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Abrasion Resistance of Aqueous Acrylic/Urethane AD Satin Finish 25% PUD 75% Acrylic
CS 10 Abrading wheel, 1000g load, 3X4 mil WFT coats
020406080
100120140
weight loss 100 cycles weight loss 1000 cycles
Control Wax 1% 40nm Al2O3 1% 60 nm Al2O31% 60 nm Al2O3 + wax 1% 40nm Al2O3 + wax
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Effect of Nano-particles in Aqueous AD Coatings
1.0% Loading of Nano Alumina
• improves scratch resistance (gloss retention)• 20nm alumina imparts early resistance properties (24 hrs)• 40 nm requires longer dry time 96 hours for same
properties
• Improves burnish resistance of matted coatings• Nano-Alumina with wax for best burnish resistance• Nano-Alumina with wax for best Taber Abrasion resistance
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Adhesion and Scratch Resistance of Acrylic Water borne Coating to Fiberglass
Control
1% 60 nm Al2O3
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Effect of Nano-particles in Aqueous AD Coatings
1.0% Loading of Nano Alumina
• improves scratch resistance (gloss retention)• 20nm alumina imparts early resistance properties (24 hrs)• 40 nm requires longer dry time 96 hours for same
properties
• Improves burnish resistance of matted coatings• Nano-Alumina with wax for best burnish resistance• Nano-Alumina with wax for best Taber Abrasion resistance
• Improves stress relief resulting in better adhesion
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AFM Control Gloss 20 ° [%] Haze, modified abrasion scrub tester, ASTM D2486
No Rubs 1000 Rubs
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AFM 1.2% (40nm) Nano Alumina
No Rubs 1000 Rubs
Gloss 20 ° [%] Haze, modified abrasion scrub tester, ASTM D2486
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AFM 1.2% Nano Alumina (25 nm) Gloss 20 ° [%] Haze, modified abrasion scrub tester, ASTM D2486
No Rubs 1000 Rubs
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July 2007 Page 37, Robert McMullin Manager Nanotechnology NAFTA
UV Clear
500 rubs Control
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July 2007 Page 38, Robert McMullin Manager Nanotechnology NAFTA
UV Clear w/ 1.2% Nano Alumina
500 rubs Control
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Effect of Nano-Partucles on Scratch resistance
• Prevents gloss loss in high gloss systems• Prevents burnishing in flatted and satin systems• Smaller nano-particles provide greater scratch resistance
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UV light damages surfaces
Surfaces exposed to direct sunlight usually suffer from thesolar UV radiation that destroys organic compounds such as
- dyes and pigments- binders- polymers- organic substances in wood
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Types of UV-Absorbers for Coatings
Organic UV absorbers and HALS• Absorbers
• Hydroxyphenylbenzotriazoles• Hydroxybenzophenones• Hydroxyphenyl-S-triazines• Oxalic anilides
• HALS (Hindered Amine Light Stabilizers)
Inorganic UV absorbers • Zinc oxide• Cerium oxide• Titanium dioxide• Transparent iron oxide
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The Ideal UV Absorber
0
10
20
30
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60
70
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90
10024
026
028
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060
0
Wavelength [nm]
Tran
smitt
ance
[%]
UV Visible
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Nanoadditives for UV protection
o≈ 350 nm
+
+
+
+
+
CeO2
-++No Migration
-++Long Term Stability
+≈ 375 nm
+
-
-
TiO2
+oAbsorption Efficiencyvaries≈ 375 nmUV-Absorption Edge
+-Chemical Stability
++No Photoactivity
+oClarity
Organic AbsorbersZnO*Property
*: ZnO was listed in Europe as Biocide until 2005
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Nanoadditives for UV protectionComparison of ZnO, Ceria and Titania
200 250 300 350 400 450 500 550 600 650 700 750 800 850 9000
10
20
30
40
50
60
70
80
90
100
Tran
smis
sion
[%]
Wave length [nm]
60 nm ZnO40 nm ZnO20 nm ZnO10 nm Ceria15 nm Titania2% Nano
50 µm Film Thickness
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Uniform distribution of the proper particle size ZnO ensures maximum substrate and coating protection
The smaller and finer the ZnO particle distribution the greater the protection!
UV-Radiation
20 - 60 nm > 100 nm > 1µm
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Optimum Stabilization of Nanoparticles is necessary to see benefits of Nanotechnology
UV-radiation
no agglomerates agglomerates
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The smaller the particles the lower the haze!
Transparency of NANOBYK-3800 seriesInfluence of particle sizes
92 97113
240
0
50
100
150
200
250
300
control 20 nm 40 nm 60 nm
HA
ZE [a
.u.]
20 µm film1% dosage
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Transparency of NANOBYK-3800 seriesInfluence of particle concentration
The lower the particle concentration the lower the haze!
9297
115
148 150
0
20
40
60
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100
120
140
160
0% 1% 2% 4% 6%
Concentration of ZnO particles
HA
ZE [a
.u.]
20 µm film20 nm ZnO
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A B C D E F G H L
A: ControlB: 0,5% Organic Absorber C: 1,0% Organic AbsorberD: 0,5% 40 nm ZnO E: 1,0% 40 nm ZnOF: 0,5% 15 nm TiO2 G: 1,0% 15 nm TiO2H/L: Competitive ZnO Samples
Nanoscale ZnO for UV protectionThin Film (30 µm) Coating – 2000 h QUV-A TestingFurniture & Parquet Coating
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Results in Water Borne CoatingsThin Film Glazing (Bayhydrol 2342 Aqueous Aliphatic) 750h QUV-B Dry Testing
Control 2.5% 40nm ZnO 2.5% 20nm ZnO
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Latest’s Results from Water Based CoatingsThick Film (120 µm) Coating – 1000 hrs QUV-A Dry Testing Furniture & Parquet Coating
Reference 2,5% NANOBYK-3840Control 2% 20nm ZnO 2% 40nm ZnO 2% 60nm ZnO
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Douglas fir (1% on active matter)
Ceria Conventional organic UV absorber
Organic UV absorber +
Hals
Reference
Nanoadditives for UV protection Aqueous-based Acrylic PUD Formula – Natural Exposure: 15 months – 10 nm Ceria*
*: Patent Protected Technology
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Conventional organic UV absorber
Nanoadditives for UV protection Aqueous-based Acrylic PUD Formula – 1600 h Xenon Test – 10 nm Ceria*
Red Cedar (1% on active matter)
Ceria ReferenceConventional mineral UV absorber
*: Patent Protected Technology
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Transparency and functionality is the key driver for nanotechnology in paint application• Synthesis, Material, Particle size, and Boundry Phase determine nanomaterials
performance benefits• Low refractive index and high efficiency are key in nanotechnology for paint
application.
Nanoparticles improve• Scratch resistance of high gloss high transparent coatings to low gloss
transparent coatings • UV Coatings: 0,3 – 2,0% Nanoparticles• 2K Coatings: 1,0 – 2,0% Nanoparticles• Air-Drying solvent based coatings: 0,3 – 2,0% Nanoparticles• Air-Drying water based coatings: 0,3 – 3,0% Nanoparticles• Forced-Dried solvent based coatings: 1,0 – 4,0% Nanoparticles
UV-Protection in transparent and pigmented coatings 1,0 – 6,0% NP
Conclusion The Difference Dispersion Brings
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July 2007 Page 56, Robert McMullin Manager Nanotechnology NAFTA
NANOBYK–3650: Handling Ease
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July 2007 Page 57, Robert McMullin Manager Nanotechnology NAFTA
Nano ?