3D Printing: From Molecules to Manufacturing

1/22/2015

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Pacifichem 2015 www.pacificchem.org THE INTERNATIONAL CHEMICAL CONGRESS OF PACIFIC BASIN SOCIETIES Honolulu, Hawaii DECEMBER 15 - 20, 2015

Abstract submission is open from January 1 – April 3, 2015 Learn more about the technical program and subject areas covered visit: www.pacifichem.org

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“3D Printing: From Molecules to Manufacturing”

Dr. Mark Jones Executive External Strategy and Communications Fellow, Dow Chemical

Dr. Timothy Long Professor of Chemistry and Director of Macromolecules and Interfaces Institute, Virginia Tech

Dr. Chris Williams Associate Professor of Mechanical Engineering and Asst. Director of Macromolecules and Interfaces Institute, Virginia Tech

Slides available Now! Recordings will be available to ACS members after one week

www.acs.org/acswebinars Submit Your Abstracts to Pacifichem 2015 today! Find out more at www.pacifichem.org

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3D Printing: From Molecules to Manufacturing Timothy E. Long

Christopher B. Williams

Director, Macromolecules & Interface Institute

Associate Director, Macromolecules & Interface Institute

Department of Chemistry Virginia Tech

Department of Mechanical Engineering Virginia Tech

[email protected]

[email protected]

The Virginia Tech Team

Tim Long The Long Group http://www.tlong.chem.vt.edu/

Chris Williams DREAMS Lab http://www.me.vt.edu/dreams @DREAMSlab

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http://fineprintnyc.blogspot.com/2013/05/3d-printed-implant-saves-babys-life.html

http://www.dezeen.com/2013/05/29/3d-printed-robohand-helps-children-bornwithout-fingers/

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http://thehightechsociety.com/3d-printing-change-face-poverty-stricken-nations/ http://www.the-scientist.com/?articles.view/articleNo/37270/title/Organs-on-Demand/

https://www.solidconcepts.com/content/images/selective-laser-sintering-sls-015.jpg

http://www.newscientist.com/data/images/ns/cms/dn20737/dn20737-1_300.jpg

Challenge, Opportunity & Invitation Additive Manufacturing needs:  Larger catalog of working materials  Structure-Property-Process understanding

 Chemistry opportunities:  Tailoring rheology/viscosity for AM platforms with new macromolecular architectures  Understanding intermolecular interactions at interfaces, surfaces, and interfacial phenomena  Physical properties of layered architectures  New orthogonal synthetic methods and photo-reactive monomers/oligomers

http://wohlersassociates.com/road map2009.html

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Molecules to Manufacturing

Opportunity to realize breakthrough products via concurrent design of novel polymer chemistry, part geometry, and manufacturing process.

Structural Parameters for Polymeric Materials in Additive Manufacturing  Molecular Weight and Molecular Weight Distribution  Chemical Composition  Chain Isomerism/Stereochemistry  Morphology  Topology  Rheology (solution and melt)  Surface Features  Polymer Additives

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Webinar Outline Additive Manufacturing Overview Additive Manufacturing Materials & Processes Extrusion Photopolymerization Vat-based & Jetting

Powder Bed Fusion Binder Jetting

Summary

Additive Manufacturing

http://www.compassdude.com/i/topographic-map.jpg

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vs.

http://www.compassdude.com/i/topographic-map.jpg

http://upload.wikimedia.org/wikipedia/commons/6/68/Fotothek_df_n-20_0000140_Zerspannungsfacharbeiter.jpg

Subtractive

Additive ASTM F2792-10

Instantaneous Audience Question When was the first “3D printing” technology commercialized?  1970s  1980s  1990s  2000s  2010s

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AM Technologies: Classification

ASTM F2792:12a


ASTM F2792:12a

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Material Extrusion Processes

media1.wmv

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Entering the Viscous Melt State  Provide heat to induce polymer flow  Need to maintain constant temperature  Avoid overheating:  Polymers degrade at high temperatures and can leave residue

Thermoplastic Polymers for Extrusion Any thermoplastic material with proper melt viscosity is potentially suitable for extrusion Polymer Type

Chemical Structure

Acrylonitrile-Butadiene-Styrene (ABS)

Properties High toughness and impact resistance

Polysulfones

Heat/chemical resistance, dimensional stability

Polycarbonates

High impact resistance/tensile strength, low scratch resistance

Polyetherimides

High temp applications (Tg = 216 °C), similar to PEEK

Polyesters

Biocompatible and biodegradable

http://blog.lib.umn.edu/thors394/3701/assets_c/2 013/10/DSC_2569-thumb-800x529-167617.jpg

Gibson, I.; Rosen, D. W.; Stucker, B.; Springer: New York, 2010, pg. 159 Images - http://en.wikipedia.org/wiki/Fused_deposition_modeling

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Morphology of Thermoplastics: Study of Structure What are the details of the structure of the solid?

Crystalline

Semicrystalline

Melting @ Tm Heat of Fusion Stronger Forces Correlated Structure

Amorphous

Glass Transition No Heat of Fusion Free Volume Amorphous Form

Melt Rheology Considerations

Viscosity of Polymers as a Function of Molecular Weight

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Relationship of Molecular Weight to Mechanical Properties and Rheology  Properties increase, then essentially plateau with MW at Me, entanglement MW  Melt Viscosity proportional to 3.4 power of weight average MW.



0 “Property” e.g., Tg

(Zero shear melt Viscosity)

Me  M.W.

Me = MW where entanglements become important Tg ~ Tg - Constant / Mn

Advancements in Extrusion

http://cloudwiser.wordpress.com/2014/09/15/local-motors-3d-prints-a-car-live-at-imts-3d-printing-industry/

http://craft.usc.edu/CC/modem.html

http://www.envisiontec.de/

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Instantaneous Audience Question Which of the following materials often used in 3D Printing are thermoplastics?  Amorphous polymers  Semi-crystalline polymers  Hydrogels  Crosslinked epoxies  Block copolymers


ASTM F2792:12a

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Vat Photopolymerization Stereolithography (3D Systems) Scanning Mirrors

http://www.picastings.co.uk/_includes/images/global/RPQuickCastmodelsRacingCar.jpg

Mask Projection mStereolithography

http://pubs.acs.org/doi/abs/10.1021/mz5006316

Projected UV light selectively cures photopolymer

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Material Jetting: Stratasys PolyJet

Stratasys PolyJet Material Jetting

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UV-Curable Photopolymers for Stereolithography Functional Group Type

Acrylate / Methacrylate

Epoxy

Vinyl Ether

Curing Mechanism

Free Radical

Cationic

Cationic

Chemical Structure

Examples

Polymer backbone can contain any of: - Linear/cyclic aliphatics - Aromatics - Polyurethanes/ureas - Polyesters - Polyethers - Polycarbonates

Most versatile AM method for polymeric materials Any liquid polymeric (oligomeric) material is suitable for stereolithography. Gibson, I.; Rosen, D. W.; Stucker, B.; Springer: New York, 2010, pg. 63-67

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A Smart Swap™ accessory offers rheological characterization of UV curable materials UV Curing Accessory

 High-pressure mercury light source for UV radiation  UV wavelengths in the range of 320 to 500 nm  Smart Swap assembly with light source mount, collimator, and 5 mm light guide

TA Instruments-Discovery Hybrid Accessories http://www.tainstruments.com

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Photo-rheology accelerates discovery for cure time and viscosity optimization 1.E+7

DHR-2: 20 mm parallel plate, UHP, 500 um gap, 10 Hz, 0.05% strain

G’

G' or G'' (Pa)

1.E+6 1.E+5 G’’

1.E+4 1.E+3

L61 20mW/cm2 L61 5 mW/cm2

1.E+2

UV Light 1.E+1 0

50

100

150 200 time (s)

250

300

350

SEM reveals architectural definition for Pluronic L-61 scaffolds

500 µm

1 mm

500 µm

500 µm

SEM: NEO Scope JCM 5000

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SL Materials: Acrylates & Epoxies Acrylate (acrylic monomer + free radical photoinitiator) Faster polymerization Warping Poor material properties

Epoxy (epoxy monomer + cationic photoinitiator) Slow Sensitive to impurities (e.g., water) Viscous Good material properties

SL Materials: Acrylates & Epoxies Commercial materials are combinations of acrylates and epoxies. Acrylates reduces energy required for cationic reaction Epoxy aides free-radical reaction (acts as a plasticizer)

Acrylate and epoxy monomers do not react with one another. Result is interpenetrating polymer network. Variety of additives to stabilize resin, adjust viscosity, etc.

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Instantaneous Audience Question Which of the following parameters does NOT influence the rate of the photochemical curing reaction in a stereo lithographic process?  Glass transition temperature of the final polymer  Photo-initiator concentration  Acrylate concentration  Phase of the moon

Phosphonium monomers displayed ionic liquid behavior with bulky counterions

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Mask projection micro-stereolithography successfully 3D prints phosphonium ILs x

z O

O

O

O Tf N 2

P

y

3D Printer: UV LED 365 nm, build surface intensity 5 mW/cm2, Digital micro image device 1080 p

Poly(PEGDMA90-co -TOPTf2N10) with 0.25 wt% Tinuvin® increases print resolution, printability, and structural definition

0.1 mm

100 mm

0.5 mm

500 mm

1 mm


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Polyester cylinders provide structural advantages in tissue-engineered scaffolds Inner layer: Endothelium Middle layer: Smooth muscle & elastic tissue

lumen

Outer layer: Elastic and collagen fibers


Suspension Photo-polymerization  Emerging research in photo-polymerization of particulate suspensions  Example:  Material Jetting of Quantum Dot acrylate suspension  “Programmable Matter” for anti-counterfeiting applications  Stochastic arrangement of nanoparticles in droplet create unique identifier that cannot be replicated

a

b

Images of jetted QD Nanoink in (a) visible and (b) UV light

Elliott et al., 2013, Advanced Engineering Materials, 15(10), 903-907.

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ASTM F2792:12a

Powder Bed Fusion

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“Powder Bed Fusion Additive Manufacturing;" J. P. Kruth, KU Leuven University, Belgium

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ASTM F2792:12a

Binder Jetting

www.exone.com

• Binder is selectively jetted into powder bed • Powder for next layer is swept onto bed via a roller

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Binder Jetting

Binder Jetting Materials

Starch / Plaster

Foundry Sand

Metals (e.g., steel; Cu)

Ceramics (e.g., B4C)

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Key Takeaway Additive Manufacturing + Novel Polymer Synthesis + Tailored Part Geometry

=

Can displace what is possible with conventional materials and traditional manufacturing processes

Acknowledgements: Sponsors  National Science Foundation  Air Force Research Laboratory  Virginia Center for Innovative Technology  VT Institute for Critical Technology & Applied Science  Army Research Office, ILEAD MURI

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Acknowledgements: Collaborators  Students:  Nick Meisel (PhD Candidate)  Nicholas Chartrain (PhD Student)  Amelia Elliott (PhD 2014)  Nancy Zhang (PhD 2012)  Ashley Nelson (PhD Candidate)

 Olga Ivanova (Postdoc 2014)  Blake Perez (MS 2014)  Phillip Lambert (MS 2014)  Alison Schultz (PhD Candidate)  Justin Sirrine (PhD Candidate)

 Faculty:  Thomas Campbell (VT, ICTAS)  Vicki Long (VT, Chemistry)







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How has ACS Webinars benefited you?

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“ACS Webinars benefits me because the topics are timely, I can attend during workday, and the information can be put to immediate use. Our Institute is limiting travel to meetings so webinars ARE the way I continue my career development.”

Trudy Holyst, M.S. Senior Lab Technologist, Protein Chemistry Core Lab, Blood Research Institute

Be a featured fan on an upcoming webinar! Write to us @ [email protected]

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@acswebinars youtube.com/acswebinars

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Benefits of ACS Membership Chemical & Engineering News (C&EN) The preeminent weekly news source.

NEW! Free Access to ACS Presentations on Demand® ACS Member only access to over 1,000 presentation recordings from recent ACS meetings and select events.

NEW! ACS Career Navigator Your source for leadership development, professional education, career services, and much more.

www.acs.org/2joinACS

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3D Printing: From Molecules to Manufacturing

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