Industry Evaluation of Radio Frequency Lamination

Shawn M. Allan*, Inessa Baranova, Gibran Esquenazi, Morgana Fall, Dr. Holly Shulman

Ceralink Inc.

Rensselaer Technology Park Troy, New York

Joseph Poley, Scott Chambers

Pilkington North America

Materials Science & Technology 2011 Innovative Processing and Synthesis of Ceramics, Glass and Composites

Advanced Processing and Characterization

Columbus, Ohio October 17, 2011, 2:40 PM

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Outline

Types of flat glass & product applications

FastFuse™ RF lamination

Industry quality evaluation

Industry energy evaluation

Ceralink Celebrating 10 years of Ceralink!

Focus on innovative manufacturing technologies

Materials processing and technology development

Specialize in microwave & RF heating

FastFuse™ support from

DOE-ITP Industrial Grand Challenge

NYSERDA Industrial Process & Product Innovation

DOE-ITP Inventions & Innovations

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Flat Glass Types

1 Source: http://chicagowindowexpert.com/wp-content/uploads/2009/06/shards.jpg

4 2 Photo source: http://en.wikipedia.org/wiki/Tempered_glass 3 Photo source: By Daniel Ramirez www.creativecommons.org/licenses/by/2.0, via Wikimedia Commons

Annealed1 Tempered2 Laminated3

Lowest strength Dangerous shards Least processed High strength

Safer fragmentation Special cooling process

High strength composite 2 or more glass sheets

Plastic interlayer prevents shards

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Glass Lamination State-of-the-art Methods

Autoclave 130-140 °C, 100-300 psi

Features Batch only 1.5 to 18 hour processes Slow process development Prevents continuous processing Energy Intensive

Interlayers

PVB - Polyvinyl butyral – Autoglass Clear, printed

TPU - Thermoplastic polyurethane – Armor

EVA - Ethylene vinyl acetate – Solar, Decorative

Clear, colored, opaque

Glass Autoclave

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FastFuse RF Lamination Laminates faster and more efficiently

0.5 to 3 minute cycles – most products 5 minutes for thick armor panels Cuts energy over 90% vs. Autoclave Heats interlayer directly New process using existing equipment Allows fast development

50+ experiments in 1 day Custom one-off manufacturing Rapid quality feedback

Thermex Thermatron RF Press with shuttle

Process Flow

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Autoclave Lamination • Lone batch process • Break in continuous process • Prelamination heat is lost • Heat energy lost in storage

FastFuse Lamination • Semi-continuous • No break in process flow • Prelamination heat used in RF • No storage of work-in-process

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RF Heating & Press

Rapidly alternating electric field creates friction – Dielectric Heating

Polar “lossy” materials heat vinyls, polyurethanes,

epoxies, phenolics

Non polar materials don’t heat polyethylene, polypropylene,

PTFE, ETFE

Intermediate materials acrylics, polycarbonate, glass, nylons, polyesters

Conductive materials transmit RF capacitive coupling

RF Laminated Products: Transparent Armor, Solar Panels, Lighting

Armor thickness compared to single-pane

“windshield” laminate

Armor

Single pane

5 minutes in RF press

18 hours in Autoclave

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FastFuse Test Plan 70 samples made identically: visibly good – Pass ASTM C1172

12” x 12” panels Flat autoglass with Sekisui automotive PVB 40 second RF press Nip roller de-airing

Run battery of industry standard tests

Narrow designed experiments on problem areas

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FastFuse Quality Testing 16 different industry quality tests at Pilkington North America

ANSI/SAE Z26-1996 Pilkington Indicative Test Protocol

Optical Haze Light stability Luminous transmission

Mechanical

Abrasion resistance Dart impact, 7 oz, 30 ft Ball impact, 8 oz, 30 ft Pummel adhesion

Environmental

Humidity Cyclic humidity Thermal cycling QUV 2000 hours Boil Bake 120 °C 2 hours Bake 90 °C 4 days 24 month exposure – Florida 24 month exposure – Arizona

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FastFuse Quality Testing 16 different industry quality tests at Pilkington North America

ANSI/SAE Z26-1996 Pilkington Indicative Test Protocol

Optical Haze Light stability Luminous transmission

Mechanical

Abrasion resistance Dart impact, 7 oz, 30 ft Ball impact, 8 oz, 30 ft Pummel adhesion

Environmental

Humidity Cyclic humidity Thermal cycling QUV 2000 hours Boil Bake 120 °C 2 hours Bake 90 °C 4 days 24 month exposure – Florida 24 month exposure – Arizona

Optical testing Haze

PASS! Target < 1% RF <0.10% RF completely eliminated PVB surface pattern

ANSI Z26.1-1996 Light stability and luminous transmission

PASS!

Percent transmittance

Specimen No.

Before Irradiation

After Irradiation

Reduction of Transmittance

1 74.48 74.26 0.22

2 74.68 74.39 0.29

3 74.55 74.37 0.18

Mechanical Testing Abrasion Test – PASS

Dart Impact from 30 ft

5 panels PASS – no penetrations

Ball Impact from 30 ft

12 panels PASS – no penetrations

Dart Impact

Ball Impact

Pummel Adhesion Testing Pummel adhesion – FAIL

Subjective rating scale 0-10 Low adhesion in 0-1 range

Identified next stage test plan

High adhesion PVB Low humidity PVB storage

Pummel 0-1 FAIL

Environmental Testing Failure indicated by bubbles, haze, delamination

Cyclic humidity – PASS

12 weeks alternated 2 weeks at 50 °C, 95% RH & ambient

Thermal cycle – PASS 10 cycles 80 °C, 80% RH to -40 °C

UV cycling – PASS 400 hours, no change – target is < 1.5% change in transmission

Bake 4 days, 90 °C – PASS

Boil 2 hours – PASS

Environmental Testing Stepwise bake – FAIL

110 °C bake – fine edge bubbles 120 °C bake – bubbles throughout

Identified next stage test plan

Low humidity conditioning High adhesion PVB Vacuum de-airing Cooling under pressure

Environmental Test Success Significant factors

Vacuum de-airing Cooling under pressure

Combination produced 120 °C, 2 hour bake PASS

25 psi 40 seconds

Nip rolled No cooling

100 psi 55 seconds

Nip rolled 5 minute cool

25 psi 55 seconds Nip rolled No cooling

100 psi 55 seconds Vacuum 5 minute cool

Pummel Adhesion Success Significant factors

PVB adhesion characteristic Automotive PVB contain adhesion inhibitor salts Architectural PVB more pure, higher adhesion

Pummel ratings from 3-7 achieved PASS – automotive target

Same RF parameters as automotive grade Pummel rating of 1

Pummel 3 PASS

Pummel 7 PASS

FastFuse Energy Scale-up

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EVA Interlayers

FastFuse Scale-up vs. Industry Energy Use

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Industry Average 1 kWh/ft2 (DOE MECS)

Windshields 0.45 kWh/ft2 (Pilkington estimate)

FastFuse™ 0.04 kWh/ft2

Autoclave Energy Projections

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Autoclave FastFuse 3 RF Presses

Production Capacity 240 windshields/batch 1 windshield/press

Production Time 90 minutes 1 minute

Energy per ft2 0.45 kWh/ft2 0.04 kWh/ft2

Batch Energy (kWh) 1,729 kWh 154 kWh

Batch Peak Demand (kV)

1700 kV 150 kV

Annual production 22 million ft2 22 million ft2

Annual energy 10,100,000 kWh 896,000 kWh

Annual energy cost $1,010,000 $89,600

FastFuse™ Roadmap Curved side window lamination

In progress with Pilkington Automotive & Thermex Thermatron Curved tooling in development

Transparent armor FastFuse evaluation

Non-destructive ultrasonic adhesion testing

Dr. Henrique Reis, UIUC Correlating NDE results to measured adhesion levels

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FastFuse™ Summary Commercial quality windows produced with FastFuse™

Non-RF prelamination steps critical to quality

High adhesion achieved with current PVB

Quality verifies energy applicability

90% lamination energy reduction

Quality verifications aid industry acceptance

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Acknowledgements U.S. Department of Energy, Industrial Grand Challenge Award No. DE-EE0003453 New York State Energy Research & Development Authority Joseph Poley, Scott Chambers, Pilkington North America Thermex-Thermatron

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Thank you! Questions? Ceralink Inc. develops advanced materials,

green processes, and new products for industry.

Shawn Allan Sr. Materials Engineer

(518) 283-7733 shawn@ceralink.com

www.FastFuse.net

Patent Pending FastFuse™ RF Lamination Technology

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