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Page 1: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Research Highlights

2016

Page 2: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Biocatalysis and Biotechnology (BB)Investigator Department ExpertisePing Wang* BBE Enzymology and biocatalysis, bioconversion and

biosynthesis, biomaterials and functional coatings, bioelectrochemical processing, biosensors.

Mark Distefano Chem Organic and biochem., protein conjugates for therapeutic and biotechnology applications.

Mikael Elias Biochem Protein engineering and evolution, molecular modelling andrecognition, bioremediation and quorum quenching strategies.

Wei-Shou Hu CEMS Systems biotechnology, biochemical engineering, cell culture bioprocessing, stem cell technology

Romas Kazlauskas Biochem Biocatalytic synthesis of chemical intermediates and biofuels, enzyme modification for new reactions.

Lawrence Wackett Biochem Enzymes in biotechnology, immobilization technology, bioremediation, computer prediction tools for biocatalysis

Kechun Zhang CEMS Synthetic biology, metabolic engineering, protein engineering, biofuels, renewable chemicals.

*Program Leader (Email: [email protected]; Phone: 612-624-4792)

Chemical and fuel bioprocessing; Biocatalyst engineering; Biotransformation and Bioremediation; Enzyme evolution; Bio-based polymers and biocoatings; Pathway engineering; Synthetic biology; Systems biotechnology; Cell culture bioprocessing

Page 3: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Enzymatic Protein Labeling

Mark Distefano is exploring how proteinsaccelerate chemical reactions and howproteins recognize other molecules with highspecificity. This information is useful for drugdesign and biotechnology applications.

http://www.bti.umn.edu/faculty/biodistefano.html

Distefano Lab

Fluorescent labeling of CNTF

Protein prenylation is a ubiquitous post-translational modification

Page 4: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Systems Design and Cell Engineering

Hu Lab

Genome engineering for biomanufacturing, genome technology for CHO cells

Stem cell engineering for hepatic applications, biomanufacturing, for cell therapy

Biofilm and antibiotic resistance transmission, microbial invasion

Chinese hamster

Chinese hamster iPSC

Enterocuccus facaelis

Page 5: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Kazlauskas Lab

- engineers enzymes tobe more stable, to havehigher selectivity andeven to catalyze newreactions.

http://www.umn.edu/~rjk

Reconstructed ancestral esterases and hydroxynitrile lyases are more promiscuous than modern enzymes

Protein Engineering

Ancestral catalyze new reactions

Page 6: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Nano Biocatalysis and Biomaterials

Wang Lab

Conceiving and realizing nature-inspiredmultienzyme reaction pathways, ImmobilizedBiocatalysts, Bioproducts and Biopolymers,Bioenergy, Biosensors and Biomaterials.

http://www.bti.umn.edu/faculty/biowang.html

Page 7: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Bioproducts Innovations and Pathway Engineering

Our research program combinesprinciples of chemistry, biologyand engineering to achievebiosynthesis beyond nature

http://www.cems.umn.edu/about/people/faculty.id21395.html

Zhang Lab

Page 8: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Biomedical and Pharmaceutical Materials (BPM)

• Biomaterials for drug delivery, medical device coatings, and tissue engineering

• Drug/medical device combinations, characterization of drug/materials interactions

• Cell-based fabrication of bioartificial tissues

• Novel tissue mechanical testing and analysis methods

Investigator Department Expertise

Ron Siegel* Phm1/BME2 hydrogels, drug delivery systems, microfabrication

Effi Kokkoli CEMS3 bioadhesion and drug targeting

Jayanth Panyam Phm multifunctional nanodelivery vehicles

Wei Shen BME bioactive materials

Calvin Sun Phm drug crystal and particle engineering

Raj Suryanarayanan Phm solid state properties of drugs, stability of drug/biomaterial formulations

Bob Tranquillo BME/CEMS fabrication and characterization of bioartificial cardiovascular replacement tissues

Chun Wang BME bio-molecular materials, polymer-based DNA and drug delivery, protein-based tissue

scaffolds*Program Leader (Email:[email protected])Affiliated Investigators: Chris Macosko,3 Marc Hillmyer,4 Theresa Reineke,4 Tom Hoye.41Pharmaceutics; 2Biomedical Engineering; 3Chemical Engineering and Materials Science, 4Chemistry

Page 9: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Inert Biodegradable Surfaces with “Artificial Mucus”

Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science & Engineering, 2, 180-187 (2016)

Hydrophobic graft (PCL)Hydrophilic core (HA)

TCP PCL

PCL/(1% HA-g-PCL) PCL/(3% HA-g-PCL)

0

20

40

60

80

100

120

TCP PCL PCL/1%HA-g-PCL

PCL/3%HA-g-PCL

Cel

l cou

nt

1 week4 weeks

1 week

Medical device surface

Biodegradable matrix

Medical device surface

Active nanostructured

particles

Biocompatible surface coating

Medical device surface

Biodegradable matrix

Medical device surface

Active nanostructured

particles

Biocompatible surface coating

Medical device surface

Biodegradable matrix

Medical device surface

Active nanostructured

particles

Biocompatible surface coating

(PCL)

Page 10: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

(1) Addition of a cell mixture on thecapture substrate.

(2) Capture of target cells.(3) Washing of non-target cells.(4) Release of captured cells using the

molecular trigger B-PEG.

(4)(2) (3)

Targetcell

(1)

Non-targetcell

Cell surface antigen

Capture antibody Coiled-coil A

Coiled-coil B

PEG

Efficient Release of Affinity-Captured Cells Using Coiled-Coil-Based Molecular Triggers

Selective capture of endothelial cells

Efficient release of the captured endothelial cells by B-PEG

A label-free, affinity-based cell separation platformcomposed of a capture substrate and a cell-releasingmolecular trigger. The capture substrate is functionalizedwith a capture antibody and a coiled-coil A. The cell-releasing molecular trigger B-PEG, a conjugate of coiled-coil B and polyethylene glycol, can drive efficient andgentle release of the captured cells. No excessive shearstress or enzymes are involved, and the released cellshave neither external molecules attached nor endogenouscell-surface molecules cleaved, which might be critical forthe viability, phenotype, and function of sensitive cells.Wei Shen laboratory

Page 11: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Spacer between single stranded DNA (ssDNA) and hydrophobic tail affects self-assembly, secondary

structure and binding.

Depending on the spacer used ssDNA-amphiphiles self-assemble into spherical micelles and bilayer nanotapes. The nanotapes progress from twisted nanotapes to helical nanotapes to nanotubes.

We can control the diameter and length of the ssDNA nanotubes, and we are exploring both ssDNA micelles and nanotubes for the targeted delivery of oligonucleotides.

200 nmHelical

Tube

200 nm

Twisted

Helical

Tim Pearce1 and Efie Kokkoli21Department of Biomedical Engineering

2Department of Chemical Engineering and Materials Science

Page 12: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Modulating Tabletability by Coating

Lab webpage: http://www.pharmacy.umn.edu/faculty/sun_changquancalvin/index.htm

0

1

2

3

4

5

6

7

Tabl

et T

ensi

le S

tren

gth

(MPa

) B

C

D

E

F

A

A

B C

D E

Osei-Yeboah & Sun, J. Pharm. Sci. , 2015

PI: Changquan Calvin Sun

[email protected]

70 µm

Page 13: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Coating Process Fundamentals — CPF

Investigator Expertise

Lorraine F. Francis* Solidification, stress development, microstructure, printing

Satish Kumar* Transport processes, interfacial phenomena, microfluidics

Marcio S. Carvalho** Fluid mechanics, rheology, numerical methods

Alon V. McCormick Curing, thermodynamics & kinetics, NMR, stress development

C. Daniel Frisbie Printing processes, printed electronics

Chris W. Macosko Rheology, polymer processing

Xiang Cheng Colloids, polymers, rheology, visualization

Michael Tsapatsis Zeolite and particulate coatings, membranes, separations

Wieslaw Suszynski*** Coating process experiments, apparatus, flow visualization

*Program Co-Leaders

**Pontifica Universidade Catolica, Rio de Janeiro

***Research Engineer and Coating Process and Visualization Laboratory Manager

Page 14: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Trapping of liquid may be detrimental to coating quality

Model ProblemFlow of a liquid film on rotating cylinders

r

y

StentsAuto Bodies

Contact Lenses

Challenge: Non-uniform coating thickness due to surface curvature

3D Printed Parts Lens

Imposed Surface Topography & Complex Cross-section Shape

g

Reverse Flows

Increasing Film Thickness

Smooth coatings will likely require simultaneous rotation and drying

Film Rupture

Liquid Shedding

Incr

easin

g Ro

tatio

n Ra

te

Patterned Cylinders

Slender Cylinders

Coating of Rotating Discrete Objects with Complex Surface Geometry

Weihua Li (Kumar)

Page 15: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Self-Aligned Capillarity-Assisted Lithography for Electronics (SCALE)*

* Mahajan, A.; Hyun, W. J. et al.Adv. Electron. Mater. 1, 1500137 (2015)A. Mahajan, W. J. Hyun (Frisbie, Francis)

Fabrication of an organic thin-film transistor (OTFT) by the SCALE process

Features of SCALE-processed OTFTs Charge carrier mobility: 0.8 ± 0.4 cm2V-1s-1

On/off current ratio: 105.3 ± 0.3

Threshold voltage: -0.3 ± 0.0 V

Page 16: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Nanocrystal Coatings by Aerosol Jet Printing and Compaction

Objective

Develop continuous-amenable process for nanocrystal coatings

Results

Coating morphology depends on aerosol flow rate

Nanocrystal agglomerates form a continuous coating

Compaction increases density

Thermal annealing creates the desired microstructure

Increasing carrier gas flow rate

Williams et al. ACS Applied Materials & Interfaces 2015.Bryce Williams (Francis, Aydil)

Page 17: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Coating Patches: Analysis of Shutdown Process

D. Maza (Carvalho)

Goal: Study the effect of process conditions and die lip design on the trailing edgeof patches coated with slot die.

Method: Solve the transient Navier-Stokes equations for free surface flows using the finite element method.

Main Result:

Minimized trailing edge on patches coated withslot coating process.

Maza D. and Carvalho M.S., AIChE Journal, submitted for publication, 2016.

Page 18: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Slot Coating of Particle Suspensions

R. Reboucas and I. Siqueira (Carvalho)

Goal: Evaluate effect of particle concentration and size on process limits and particle distribution and orientation on the coated film.

Method: Solve the Navier-Stokes equations for free surface flows coupled with particle concentration and conformation transport equations using the finite element method

Reboucas, Siqueira, Souza Mendes and Carvalho, JNNFM, sub., 2016

Main Result:

Accurate prediction of process limits of particle suspension coating.

Effect of flow conditions on particle distribution and alignment on coated film.

Page 19: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Electronic Materials and Devices (EMD)

Investigator Department ExpertiseSteven Koester* ECE (program leader) Electronic devices, semiconductors

Chris Leighton CEMS Electronic/magnetic properties, film/layer growth

Paul Crowell Physics Magnetism, transport, ultra-fast spectroscopy

Steve Campbell ECE Thin-film photovoltaics, 2D materials

Bharat Jalan CEMS Complex oxides, molecular beam epitaxy

Renata Wentzcovitch CEMS Electronic structure theory

CollaboratorsAndre Mkhoyan (CEMS), Dan Frisbie (CEMS), Xiaodong Xu (U. Washington), Ludwig Bartels (UCR), Chris Palmstrøm (UCSB), Chris Kim (ECE)

Synthesis, structural and chemical characterization of materials relevant for a wide range of electronic, optical and magnetic devices. Particular emphasis is placed on the understanding of the fundamentals of electronic structure and transport in electronic and magnetic materials, in addition to the materials science, physics and chemistry of the interfaces and nanostructures that play a vital role in device operation.

Page 20: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

• Temperature and gate bias windows for effective gating carefully established.• Stark asymmetry in electrostatic vs. electrochemical gate response with bias polarity, with

important implications for electrolyte gating of n-type vs. p-type oxides.• Electrical control over transport, Curie temperature, etc., probed via anomalous Hall effect.

Walter, Wang, Luo, Frisbie and Leighton,Submitted, ACS Nano (2016).

• Electrolytes can be used as unconventional gate dielectrics in transistors, generating unprecedented surface charge densities, and controlling electronic and magnetic properties. This has been studied here in LSCO.

Leighton / Frisbieresearch.cems.umn.edu/leighton

Understanding Electrolyte Gating to Understand Complex Oxides: La0.5Sr0.5CoO3-δ (LSCO)

Page 21: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

• Spin injection from Co2MnSi and Co2FeSi into GaAs and detection at room temperature. Demonstration of spin pumping and large spin Hall magneto-resistance in heterostructures based on Co2FeAl/Pt.

• Heusler alloys have important applications in memory and logic applications as well as high-sensitivity magnetic sensors.

Heusler Alloy-Based Spintronic Devices

• Developing spintronic devices based on highly-polarized Heusler alloy ferromagnets integrated with semiconductors as well as high-Z metals (e.g. Pt):

Spin pumping devicesMicrowave detection of spin accumulation

C. Liu et al., Nature Communications 7, 10296 (2016).

Crowell

Page 22: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

2D Materials• Developed black phosphorus growth

• Developing growth system for transition metal dichalcogenides (TMDs):

SulfidesSelenidesHeterojunctions

Photovoltaics• Developed wide gap, low trap

density CuInAlGaSe process

• Developed technique to control in-situ MoSe2 orientation to prevent delamination

• Developed method for measuring interface trap density in materials with bulk traps

Energy from Valence Band (eV)

Inte

rfac

e Tr

ap D

ensi

ty (c

m-2

/eV)

Wide gap layerCu-deficient layer

Narrow gap layer

Novel Semiconductors

Campbell

• Applications in flexible electronics and thin-film solar cells.

S. A. Campbell, MRS, 2015.

Page 23: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

SnS Nanosheets – Another “2D” Semiconductor?

• SnS is a 2D semiconductor with similar crystal structure to black phosphorus:

• Synthesized large (up to 10 µm wide and as thin as 3.5 nm) nanoplates. Raman / XRD consistent with orthorhombic SnS. applications in optoelectronics and printed electronics.

research.cems.umn.edu/aydil

5 µm

300

322

340

In

tens

ity (A

rb. U

nits

)

20 30 40 50 60 70

SnS SnS2

2θ (degrees)

Aydil

Page 24: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

bare Cu Gr, short pre-anneal Gr, long pre-anneal0.00

0.05

0.10

0.15

0.20

Cor

rosi

on R

ate

(mm

/yr)

Material

~ 10x

Graphene Coatings for Corrosion Protection

• Developed growth process for graphene directly on copper wires:

• Used Tafel analysis to quantify corrosion rate in PBS electrolyte solution.

• Demonstrated 10x reduction in corrosion rate compared to bare Cu.

• Applications for medical electronics.

www.ece.umn.edu/users/skoester

Schematic diagram showing graphene-coated copper wire

-0.4 -0.3 -0.2 -0.1

10-7

10-6

10-5

10-4

Cur

rent

den

sity

(A/c

m2 )

Pentential vs. reference (V)

Bare Cu Gr/Cu - short pre-anneal Gr/Cu - long pre-anneal

Q. Su and S. Koester, to be published.

Koester

Page 25: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Faculty Member Department ExpertiseRussell J. Holmes CEMS Thin films, LEDs, solar cells

David Blank CHEM Ultrafast spectroscopy

Chris Douglas CHEM Molecular synthesis

C. Daniel Frisbie CEMS TFTs and printed electronics

P. Paul Ruden ECE Device modeling, transport theory

*Program Leader

Flexible Electronics and Photovoltaics (FEP)

Interested in the design of materials, device architectures, and processes for the realization of flexible electronics and optoelectronics based on organic

and hybrid organic-inorganic materials

Page 26: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

NPD588.7 g/mol

Pvap~0.7-7 Pa forT=260°C-290°C

Purification of specialty electronic materials

0 10 20 30 40 50 60 700

2

4

6

8

10

12

14

16

18

Inve

rse

Sub

limat

ion

Rat

e (h

r/g)

Distance to Collection Zone (cm)

NPD

Transport

Deposition

• Thermal gradient sublimation is used in industry to purify high value, small molecule organic semiconductors

• Identified rate limited steps as transport down the tube to the deposition zone and a resistance to physical vapor deposition

• Developed model has been used to optimize separation efficiency for multicomponent feeds and predict conditions for scale-up

Morgan, N. et al. AIChE Journal, 60, 1347 (2014) and Morgan, N. et al. Org. Electron., 24, 212 (2015)

PI: Cussler, Holmes and Dow Chemical Co.

Page 27: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Acce

ptor

= Host Donor (SubPc)= Guest Donor (SubNc)

Broad absorbing, cascade organic solar cells

NB

N

N N

N

N

Cl

N

BN

N N

N

N

Cl

SubPc, Guest

10 nm 25 wt. % SubNc in SubPc

ITO10 nm MoOX

3 nm SubNc42 nm C60

10 nm Blocking layerAl

-0.2 0.0 0.2 0.4 0.6 0.8 1.0-10

-8

-6

-4

-2

0

2

Cur

rent

Den

sity

(mA

/cm

2 )

Voltage (V)

Neat SubNc / C60

Dilute SubNc:UGH2 / C60

Dilute SubNc:SubPc / C60

Dilute SubNc:SubPc / C70

Performance at an intensity of 100 mW/cm2 under AM 1.5G solar simulated illumination

Host Acceptor ηP [%]

None C60 2.0 ± 0.1

None C70 2.2 ± 0.1

UGH2(Non-absorbing) C60 2.8 ± 0.1

SubPc C60 3.2 ± 0.1

SubPc C70 4.3 ± 0.2

SubNc, Host

• SubPc and SubNc have complementary optical absorption

• Excitons are generated on both materials with transport occurring on SubNc – Energy cascade between SubPc and SubNc

• Diffusion on SubNc can be engineered via dilution

Performance of host-guest cascade cell exceeds that of conventional devices that do not use a composite donor layer as well as those with a non-absorbing host

Menke, S.M. and Holmes, R.J., ACS Appl. Mater. Interfaces, 7, 2912 (2015)

PI: Holmes

Page 28: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

2 µm 1 µm

SEM cross-sections showing Ag seed layer on the channel walls(left) anda channel completely filled with Cu metal (right)

Ag seed layer Electroless Plated Cu Line width and spacing down

to 2 µm Conductivity 60 % of bulk

metal Additive Roll-to-roll compatible

Major Process Attributes

New Approach for High-Resolution Printed Electronics

Inkjet-printed Ag ink is wicked into microimprinted channels on a plastic substrate, followed by a Cu electroless plating step. Ag metal inside the channel acts as a seed layer for selective deposition of Cu .

Mahajan, A. et al. ACS Appl. Mater. Interfaces 7, 1841-1847 (2015)

PI: Frisbie and Francis (CPF)

Page 29: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Unwind Coating Imprint Metrology Rewind

• Manufactured by Carpe Diem Technology

• Line Speed: 4-800 inches per minute

• Web Width: 4-6 inches

R2R Nanoimprint at Minnesota

Page 30: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Second R2R Line: Multimaterials, Slot, Gravure, Aerosol Jet

•Forward – reverse operation, multiple web paths

•Fully enclosed, HEPA filtered air

Unwind

Aerosol jet and drop on demandprinter

Gravure printing

Photonic sintering unit

Rewind

Slot coating

4 ft

IR heater

Corona

Page 31: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Microstructured Polymers (MP)

Investigator Department ExpertiseFrank S. Bates CEMS Thermodynamics, scattering, synthesis

Marc A. Hillmyer* CHEM Polymer synthesis and characterization(Director: Polymer Synthesis Facility)

Timothy P. Lodge CHEM/CEMS Polymer dynamics, solutions, scattering

Chris Macosko CEMS Rheology, processing

Mahesh Mahanthappa CEMS Synthesis, morphology, self-assembly

David C. Morse CEMS Theory and modeling

Theresa Reineke CHEM Biomedicine, Diagnostics, Targeted Delivery

Collaborators include:Lorraine Francis (CEMS), Dan Frisbie (CEMS), Tom Hoye (CHEM), Chris Leighton (CEMS), Ron Siegel (PHRM), Bill Tolman (CHEM)

*Program Leader

Synthesis, characterization, dynamics, processing, properties, and theory

Page 32: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Toughening Poly(lactide) with Block Copolymer Micelles

Tuoqi Li, Jiuyang Zhang, Deborah K. Schneiderman, Lorraine Francis and Frank S. Bates (ACS Macro Letters 2016)

1 µm

5 wt% EB-1

• Low molecular weight poly(ethylene oxide)-b-poly(butylene oxide) (EB) diblock copolymer forms micelles in poly(L-lactide) (PLLA)

EB diblock copolymer

PLLA

Izod impact strength Tensile strength

• Dispersion of micelles in PLLA is due to a negative χ parameter between poly(ethylene oxide) and PLLA.

• Micelles impart outstanding impact and tensile toughness at relatively low loadings without compromising modulus, Tg or optical clarity

Page 33: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

33

0.2 μm

2000 3000 4000 5000

Cou

nts

Energy (eV)

SnLα

SnLβ

interface

inclusion

PLA

HDPE

Thurber Lodge, Macosko, ACS Macro Letters, 2015, 1, 30-33

60 / 30 / 10 / 0.4 HDPE / HO-PE-OH / PLA / SnOct2

1 μm

d = 0.26 ± 0.04 μm

1 μm

90 / 10 HDPE / PLA

d = 0.77 ± 0.20 μm

1 μm

TEM +EDS

Catalyst Localized at Interface in Polymer Blends

Page 34: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Versatile ion gels for plastic electronics

Choi, Gu, Hong, Xie, Frisbie, and Lodge, ACS Appl. Mater. Int., 6, 19275-19281 (2014)Moon, Lodge, and Frisbie, Chem. Mater., 26, 5358-5364 (2014)Moon, Lodge, and Frisbie, Chem. Mater. 27, 1420-1425 (2015) Ueki, Nakamura, Usui, Kitazawa, So, Lodge, and Watanabe, Angew. Intl. Ed., 54, 3018-3022 (2015)Choi, Xie, Gu, Frisbie, and Lodge, ACS Appl. Mater. Interfaces, ASAP (2015)

ABA triblock copolymers swollen with ionic liquids are excellent candidates for organictransistor gate dielectrics, polymer gel electrolytes, and luminescent devices, among others.This versatility stems from a combination of attributes, including tunable mechanical strength,high throughput printability, high ionic conductivity, high capacitance, and thermal stability.

Electrochromic ion gel operating at only 1 V. Methyl viologen is the chromophore, in an ion gel containing PS-PMMA-PS and [EMI][TFSI]

(H. C. Moon)

Photoreversible ion gel consisting of P(NIPAm-ran-AzoMA)-PMMA-P(NIPAm-ran-AzoMA) in [EMI][PF6], operating under alternating UV and visible irradiation (T. Ueki)

Page 35: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

PCHE–PEO Block Polymer for Metal Oxide Templating

Schulze, Sinturel, & HillmyerACS Macro Lett., 4, 1027, 2015

2. Selectively Deposit Inorganic Precursors within PEO domain

3. Oxidize Inorganic and Remove BP Template

UV/Ozone

Spincoat Inorganic Precursor Solution

1. Solvent anneal PCHE–PEO Film

PS–PEO

On O

Hm

PCHE–PEO

On O

Hm

Approach• Anionic polymerization and hydrogenation for the

synthesis of new block polymer PCHE-PEO

• PEO selectively imbibes sol-gel reactants/metal ions

Outcome• Large χ enabled self-assembly at low N

• Formation of ultra-small particles (6 ± 1 nm)

• Versatile templating of silica, iron oxide, titania

100 nm

TiO2 Particles

Highlighted in MRS Bulletin, 11, 900, 2015.

Page 36: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Elastomers and PSAs from Isosorbide-Based Block Polymers

J. J. Gallagher, M. A. Hillmyer, T. M. Reineke, ACS Sustainable Chem. Eng. 2015, 2016 University of Minnesota, Department of Chemistry

OO

BTCBA, AIBN

AAI, AIBN OOO

OO

O O

OH

H

Z

O O O

OO

OO

OH

H

ZR

OO

Z

O O

ZR

OHO

O

O

O

OS S

S

SS

S 1010

BTCBA

70 °C, 2 h

DMF, 70 °C, 2h

PolymerMn, th. Mn, SEC Mn, NMR Đ wt% PAAI

(kg/mol) (kg/mol) (kg/mol) (NMR)PAAI-PnBA-PAAI

(53k, 12%) 51.7 53.3 49.8 1.09 12

PAAI-PnBA-PAAI (60k, 17%) 56.1 60.2 65.6 1.12 17

PAAI-PnBA-PAAI(70k, 21%) 59.5 69.2 67.5 1.15 21

PSA Peel Test

Page 37: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Nanostructural Materials and Processes (NMP)

Investigator Department ExpertiseAlon McCormick CEMS Materials and Emulsions Synthesis; Spectroscopy and

CryoMicroscopyC. Daniel Frisbie CEMS Molecular Materials and Interfaces; Molecular

ElectronicsWayne Gladfelter CHEM Materials Chemistry; Inorganic Chemistry; Scanning

Probe MicroscopyGreg Haugstad CHARFAC AFM Scanning Probe Microscopy

(Director, Characterization Facility)R. Lee Penn CHEM Environmental Solid State ChemistryIlja Siepmann CHEM Predictive Modeling of Phase and Sorption EquilibriaAndreas Stein CHEM Solid State Chemistry of Porous MaterialsMichael Tsapatsis CEMS Materials Synthesis, Structure Elucidation Joe Zasadzinski CEMS Microscopy of Complex Fluids

Associated Investigators: Frank Bates, Lorraine Francis, Christy Haynes, Eric Kaler, Chris Macosko, Wei Zhang

synthesis, phase behavior, structure, and performance of surfactants and self-assembled molecular and colloid systems

Page 38: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Contact-mode height image… (steric, “frictionless” contact)

In situ colloid probe AFM: “Hyperspectral” force mapping methods (here on crosslinked, oriented fibrin gel) Haugstad (Anne Ellis, Bob Tranquillo)

blue green

yellow

redorange

Elasticity histogram

Young’s modulus (MPa)

Hertzian modelR = 3.3 um probek = 0.08 N/m cantilever

Topography

Young’s Modulus

interlaced with force spectroscopy

Hysteresis: modulus correlation“Force spectroscopy”: Normal force vs. Z

Soft location Stiff location

84-nm shear-modulation, 100 Hz

Shear force

6.6 um

Mechanical hysteresis loops

Goal: Quantify mechanical anisotropyNeed: hyperspectral dataset analysis (large)

Simultaneously: shear response

Guido and Tranquillo, “A methodology for the systematic and quantitative study of cell contact guidance in oriented collagen gels…”, J Cell Sci, 1993

Morin and Tranquillo, “Guided sprouting from endothelial spheroids in fibrin gels aligned by magnetic fields and cell-induced gel compaction”, Biomaterials, 2011

32x32 = 1024 sites over 20x20 μm image

Page 39: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

2.Surfactant mixtures for dispersionExample: Span 80 effect on crude oil dispersion

Dispersion processes (McCormick group with collaborators)

1. Cryo-EM Monitoring

Multi-lamellar

Lee, H.; Morrison, E.; Frethem, C.; Zasadzinski, J.; and McCormick, A. Cryogenic electron microscopy study of nanoemulsion formation from microemulsions, Langmuir, 2014, 30 (36), 10826-10833. doi: 10.1021/la502207f

Example of nanoemulsion with non-ionic surfactant

Lee, H.; Arunagirinathan, M.; Vagias, A.; Lee, S.; Bellare, J.; Davis, H.; Kaler, E.; McCormick, A.; and Bates, F. Almost Fooled Again: New Insights into Cesium Dodecyl Sulfate Micelle Structures, Langmuir, 2014, 30 (43). 12743-12747. doi:10.1021/la502809y

Riehm, D.; McCormick, A. The role of dispersants’ dynamic interfacial tension in effective crude oil spill dispersion. Mar. Pollut. Bull., 2014, 84, 155-163. doi:10.1016/j.marpolbul.2014.05.018

0102030405060708090

0.0001

0.001

0.01

0.1

1

0 10 20 30 40 50 60

Effe

ctiv

enes

s (%

)

Initi

al

wt% Span 80

OPT

IMU

M

Inte

rfac

ial T

ensi

on (m

N/m

)

10wt% 50wt% 60wt%

Dyna

mic

cree

p ov

er m

inut

es

Sphere (ellipsoids) to cylinder transition

Page 40: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Characterizing the dynamics of aggregation in reactive systems (PENN)

pH 3.5

pH 5.5

CRYO-TEM images of nanoparticles in liquid media.

WATER

WATER: after aging.

TetrahydrofuranIsopropanol

Burrows, Talmon, Penn; 2013

Yuwono, Burrows, Soltis, Penn (JACS, 2010)

Yuwono, Burrows, Soltis, Penn(Faraday Trans 2012)

U60 clustersin waterSoltis et al., JACS, 2016

Page 41: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Predictive Modeling of Separation Processes and Nanostructured Materials– Siepmann

Funding from NSF (CBET, CHE, SI2), DOE (MGI, SciDAC, EFRC, EERE), Industry & IPRIMEDiscovery of Zeolites for Sweetening of Sour Natural Gas•Hierarchical screening of all known zeolites for binary H2S/CH4 and H2S/C2H6 mixtures and of 16 top--performing zeolites for four-- and five--component mixtures•Simula'ons yield direct informa'on on selec'vity, capacity & number of adsorp'on stagesShah, Tsapatsis & Siepmann, Angew. Chem. Intl. Ed. 55, 5938 (2016)

AngewandteChemie

5938

International Edition: DOI: 10.1002/anie.201600612 H2S Capture

Identifying Optimal Zeolitic Sorbents for Sweetening of Highly Sour Natural GasMansi S. Shah, Michael Tsapatsis, and J. Ilja Siepmann*

AngewandteChemieCommunications

⌫ 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

Angew. Chem. Int. Ed. 2016, 55, 5938 –5942

Understanding Transport in Hierarchical Zeolites• MD elucidate the complex diffusion of sorbates in house--of--cards

nanosheets where the large free energy penalty for transfer frommicropores to mesopores leads to a tortuous diffusion pathway

Bai, …, Tsapatsis & Siepmann, ACS Nano, submi9ed

Sensitivity of Nucleation FreeEnergies to Force Fields•This work demonstrates that the sensi'vity of predicted nuclea'on rates to details of the molecular models can be dramatically reduced by comparing nucleation at the same relative state pointKeasler & Siepmann, J. Chem. Phys. 143, 164516 (2015)

Page 42: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science
Page 43: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Industrial Fellows

2016

Page 44: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime Industrial Fellows (8)

Company Employee Research Topic Faculty

Asahi Kasei Ryo Katayama Effect of Drying Conditions on Particle Distribution Lorraine Francis/ Satish Kumar

Boston Scientific Bruce Forsyth High sensitivity alpha-particle detectors Steve Koester

Dai Nippon Printing Koichi Nakano Coating flow of non-Newtonian liquid in tensioned-web-over-

slot die coatingLorraine Francis/

Satish Kumar

Ecolab Stephan Hubig Evaluation of Nano Coatings for Surface Modification: Development of a tool kit for performance testing Alon McCormick

Evonik Industries Alex Todd Synthesis and self-assembly of model semi-crystalline blockpolymers Marc Hillmyer

Medtronic Carl Schu Ion Sensor applications to new products Andreas Stein

Toray Yu Abe An Analysis of the Drying State in Multi-layer Coating Xiang Cheng/Lorraine Francis

Valspar Tessie Panthani Film Formation and Stress Development Lorraine Francis

Page 45: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

Industrial Fellow

Ryo KatayamaAsahi Kasei

IPrime ProgramCoating Process Fundamentals

Faculty Sponsors Satish Kumar & Lorraine Francis

Effect of drying conditions on particle distribution

Page 46: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime ProgramElectronic Materials and Devices

Faculty SponsorSteve Koester

Research ProjectHigh sensitivity alpha-particle detectors

Industrial Fellow

Bruce ForsythBoston Scientific

PhotoPending

Page 47: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime ProgramCoating Process Fundamentals

Faculty SponsorSatish Kumar &Lorraine Francis

Research ProjectCoating flow of non-Newtonian liquid in tensioned-web-over-slot die coating

Industrial Fellow

Koichi NakanoDai Nippon Printing

Page 48: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime ProgramNanostructural Materials and Processes

Faculty SponsorsAlon McCormick

Research ProjectEvaluation of nano coatings for surface modification: development of a tool kit for performance testing

Industrial Fellow

Stephan HubigEcolab

Page 49: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime ProgramMicrostructured Polymers

Faculty SponsorMarc Hillmyer

Research ProjectSynthesis and self-assembly of model semi-crystalline block polymers

Industrial Fellow

Alex ToddEvonik Industries

Page 50: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime ProgramNanostructural Materials Processes

Faculty SponsorAndreas Stein

Research ProjectIon Sensor applications to new products

Industrial Fellow

Carl SchuMedtronic

Page 51: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime ProgramCoating Process Fundamentals

Faculty SponsorXiang Cheng & Lorraine Francis

Research ProjectAn analysis of the drying state in multi-layer coating

Industrial Fellow

Yu AbeToray

Page 52: Research Highlights 2016 - University of Minnesota...Inert Biodegradable Surfaces with “ Artificial Mucus ” Wenshou Wang, Ronald A. Siegel, and Chun Wang, ACS Biomaterials Science

IPrime ProgramCoating Process Fundamentals

Faculty SponsorLorraine Francis

Research ProjectFilm formation and stress development

Industrial Fellow

Tessie PanthaniValspar

PhotoPending