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JUBILEE SCIENTIFIC CONFERENCE
“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
New Polymeric Materials - Challenges and Perspectives
Krzysztof Pielichowski
Cracow University of Technology Department of Chemistry and Technology of Polymers

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
INTRODUCTION
MATERIALS:
CERAMICS METALS POLYMERS: 1950 – 1,5 mln t → 2014 – 260 mln t High growth potential, e.g. BRIC countries Novel polymeric materials: copolymers, blends, (nano)composites, hybrids, …

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
INTRODUCTION
• POLYMER – a compound of high molecular weight consisting of repeating units called „mers” („macromolecule” – Hermann Staudinger, (1920). "Über
Polymerisation". Ber. Deut. Chem. Ges. 53 (6): 1073.)
• PLASTICS – polymer + additives (eg. fillers, stabilizers) => composites, blends
e.g. poly(vinyl chloride)

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
POLYMERS CLASSIFICATION
POLYMERS
Natural Synthetic Elastomers • proteins, eg. fibroin (silk), colagen • polysaccharides, eg. cellulose, starch • natural resins (Gutta- percha, amber) • natural rubber, • polyurethanes ---------------------------- • amorphous • (semi)crystalline • thermoplastics– PE, PS • thermosets: thermoset (e.g. phenol- formaldehyde resins), chemically cured resins (e.g. epoxies)

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
THERMOPLASTICS THERMOSETS
CAN be reshaped – weak interactions bonds between linear chains CAN’T be reshaped - crosslinked processable (e.g. extrusion, injection molding) curing (heat, pressure, catalyst) e.g. food containers, lighting panels, pipes, garden hoses, plastic bags, … e.g. glues, varnishes, in electronic components such as circuit boards, … easy to recycle hard to recycle

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
HISTORICAL BACKGROUND
1868 – nitrocellulose, Alfred Nobel • 1850-1875 – first plastic on industrial scale – celluloid (USA) • 1909 – phenol-formaldehyde resin, Baekeland, USA • 1915 – synthetic rubber, Germany • 1920-30: H. Staudinger, macromolecule definition (1953 Noble prize, discoveries in the field of macromolecular chemistry)1927 – poly(vinyl chloride) • 1933-35: PE (Imperiacl Chemical Industries), PS (UK) • 1936 – Nylon® (PA) W.T. Carothers, • 1936 – poly(methyl methacrylate) • 1939-50: patents for other polymers (1950 – Badische Anilin & Soda-Fabrik PS; 1950-56: Ziegler-Natta catalysts 1st class.; 1963 – O. Wichterle, patent for hydrogel HEMA, contact lenses; • 1991 – first polymer nanocomposite in industrial scale (PA6/MMT, Toyota) • 1995 – ATRP (K. Matyjaszewski, M. Sawamoto) • 1998 – RAFT (CSIRO, Australia) • 2000 – H. Heeger, A. McDiarmid, H. Shirakawa, Nobel prize for the discovery and development of conductive polymers • … (bio, nano, …)
[http://www.polymerexpert.fr/en/presentation/histoire-des-polymeres/]

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
BIOCOMPOSITES / BIOPOLYMERS
Fig. Trends in the development of biocomposites/biopolymers [Product overview and
market projection of emerging bio-based plastics PRO-BIP 2009, Final report]

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
OUR RESEARCH DIRECTIONS
• Phase change materials • Hydrogels • Organic-inorganic hybrid materials

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Phase change materials (PCM)
http://www.textileworld.com/Issues/2004/March/Features/Phase_Change_Materials, http://www.rgees.com/technology.php

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Phase change materials (PCM)
Progress in Materials Science 65 (2014) 67–123 Fig. The number of articles dedicated to PCMs for thermal energy storage for the period of 1994–2013. Source: Science Direct, ‘‘phase change materials’’ and ‘‘thermal energy storage’’.

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
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PEO Degree of crystallinity [%] PEO 400 59,4 PEO 1000 77,4 PEO 3400 84,7 PEO 10000 90,3 PEO 20000 81,4 PEO 35000 84,8
Table. Degree of crystallinity vs average molar mass of PEO Fig. DSC curves for melting and crystallization process of PEO
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PEG-based PCMs disadvantages - solid-liquid phase transition and in consequence leakage, poor thermal conductivity Shape stabilization with cellulose and polysaccharides Incorporation of carbon nanomaterials (fullerenes, carbon nanotubes, graphene)

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
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Tab . Temperatures and heat of phase transition for melting and crystallization process for PEO/cellulose and PEO/cellulose derivatives
PEO/cellulose and its derivative systems

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
PEO/starch PCMs
Hydrogen interactions in PEO/starch blends: (a) EO/amylopectine, (b) PEO/amylose.

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
HYDROGELS - OVERVIEW

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
HYDROGELS – TISSUE ENGINEERING

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
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• PEG hydrogels – appl. in biotechnology, tissue engineering, drug delivery systems – hydrophilic character, porous structure, biocompatibility, however low mechanical stability • nanoparticles – reinforcement of hydrogel matrix (silicates, e.g. Laponite) • hydrogels PEG/Laponite – gel when low concentration of Laponite, high concentration of Laponite – crosslinked materials
Fig. Nanoparticles addition lead to decrease of pores size; hydrogels are characterized by highly porous structure. Fig. Nanoparticles are physically and covalently bonded to PEG – formation of mechanically strong and flexible material
HYDROGEL PEG/LAPONITE
[K. Shikinaka, K. Aizawa, Y. Murakami, Y. Osada, M. Tokita, J. Watanabe, K. Shigehara, J. Coll. Interf. Sci. 369 (2012) 470–476.]

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
HYDROGELS – DYNAMIC HYBRIDS
Fig. Schematics and optical microscope images of pH- responsive actuation using electrochemically-generated pH gradients [L.D. Zarzar, PhD
dissertation, Dynamic Hybrid Materials: Hydrogel Actuators and Catalytic Microsystems, HARVARD Univ. 2013].

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Fig. SEM microphotographs of swollen acrylic matrix
Przemysł Chemiczny, 2011, 90/7, 1000-1003

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Fig. The dependence of swelling ratio upon the concentration of fertilizers in dried hydrogels Fig. The dependence of ammonium ions release ratio upon the time Fig. Synthesis of PAA hydrogel and synthesis of PAA/fertilizer hydrogels. Polish J. of Environ. Stud. 2009, 18, 475-479

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
HYBRID MATERIALS
goal : create materials with specific combinations of properties by combining different molecular building blocks in various ratios and by controlling their mutual arrangement Fig. Inorganic-Organic Hybrid Materials

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
HYBRID MATERIALS
Inorganic Building Blocks Mechanical, optical, electrical, magnetical properties Connecting Blocks Reduction of the crosslinking density, coupling sites between inorganic / organic components Organic Building Blocks Functional groups, crosslinking, A polymerizability Flexibility, elasticity, processability polyhedral cages
[S.-T. Zheng, T. Wu, C. Chou, A. Fuhr, P. Feng, X. Bu, J. Am. Chem. Soc., 134, 4517-4520, 2012].

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
A few examples of today’s applications of hybrid materials, arising from the game of invention . Starting with the ancient creative imaginings of a hybrid being (part unicorn, part fish; inspired by art on the ceiling of the Church of St. Martin of Zillis) and ending with speculation about the future. Intermediate examples of hybrid materials include: (1) a fresco containing Maya blue, (2) hearing aids, (3) solar modules, (4) tennis balls, (5) flexible waveguide, (6) portable O2 sensor, (7) super gas barrier nylon, (8) dental fillings, (9) antistatic coating, (10) rubbery monoliths, (11) tires, (12) herbicides, (13) colored glass coatings, (14) electro-optical multichip module, (15) biocatalyst lipase on silica, (16) persistent luminescent nanoparticles for small animal imaging [G.L. Drisko, C. Sanchez, Eur. J. Inorg. Chem. 2012, 5097–5105].

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
POLYMERIC NANOHYBRIDS
Hybrid materials – mixtures of two or more materials with new properties created by new electron orbitals formed between each material, such as covalent bond between polymer and silanol molecules in inorganic/organic hybrids.
Hybrid composite Hybrid polymer
The composite material in which two or more high- performance reinforcements are combined. Understood as the polymer where an organic part is combined, on the molecular level, with an inorganic part. Fig. Schematic representation of different materials dimensions

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
HYBRID MATERIALS - POSS
Network Modifiers (non-reactive organic groups) Precursors with Functional Organic Groups 3-dimensional structure
One or more reactive groups (grafting, polymerization)
Thermally and chemically robust hybrid (organic- inorganic) framework
Nanoscale Si-Si distance = 0.5 nm R-R distance = 1.5 nm
Unreactive organic ( R ) groups (solubilization and compatibilization)
[G. Kickelbick, Prog. Polym. Sci., 28, 83-114, 2003]

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
NANOHYBRIDS POLYMER-POSS
Organic-inorganic nanohybrids materials – incorporation of inorganic groups into polymer macrochains, eg. polyhedral oligomeric silsesquioxanePOSS
PROPERTIES: ▪ increase the temperature range, ▪ increase of oxygen stability, ▪ increase of UV stability, ▪ improvement of surface , ▪ improved mechanical properties, ▪ reduced flammability, ▪ reduced heat released during combustion, ▪ higher density Fig. POSS-polymer system
Adv. Polym. Sci. 2006, 201, 225-296

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
POSS can be incorporated into a polymer chain as (i) a side branching of the main macrochain, (ii) a network node or (iii) as a part of the polymer backbone chain. POSS-polymer hybrids are an interesting class of materials, but microphase separation effects may decrease possible advantages of nanoscale incorporation. Chemical ways of POSS incorporation into the polymer structure:
a. side branching, b. network node, c. part of backbone chain.
A physical way of POSS incorporation into the polymer matrix:
Through melt processing of polymers, e.g. by extrusion ❖ POSS as a nanofiller

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Synthesis of PU/POSS
POSS as a side branching
I STEP: Synthesis of PU prepolymer:
• diphenylmethane-4,4’-diisocyanate (MDI) • poly(tetramethylene glycol) (Terathane 1400) (PTMG) • 1,2-propanediol-heptaisobutyl-POSS (PHIPOSS) • Temperature: 80°C • Atmosphere: N2
II STEP: Synthesis of PU elastomer:
• 1,4-butanediol

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Morphology PU/POSS
POSS as a side branching
Lateral force AFM images for PU/POSS
V.N. Bliznyuk et al. Polymer, 49, 2008, 2298
For the sample with the smaller filler content, the POSS molecules aggregate to nanometer size longitudinal crystallites (about 60–70 nm in length), which form spherulites of several microns average sizes. At higher filler content (PU10), POSS forms more regular crystallites of about 120 nm sizes. These observations indicate that PHIPOSS shows strong tendency to form crystallites in PU matrix, however of different types, i.e. extended structures for PU04 and more regular, smaller structures for the higher POSS content (PU10).
Polymer, 2010, 51 (3), 709-718

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
POSS impact on the thermal properties of polymers:
✓ increased melting temperature, ✓ shift the Tonset towards higher temperatures, ✓ reduced heat emission → increased thermal stability of hybrids.
Thermal stability

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Py-GC/MS studies
Py-GC/MS thermograms for the non-oxidative thermal degradation of the 0-10% DSIPOSS/PU hybrid elastomers. Note that in the unmodified elastomer a primary de-polymerization event (a) with an onset of ~250°C that is followed by a second high temperature process (b) e attributed to the degradation of the monomer units. It is evident from these data that the inclusion of DSIPOSS both shifts (a) & (b) to higher temperatures and decreases the overall yield of volatile degradation products. Polymer Degradation and Stability, 2010, 95, 1099-1105

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
Research team/collaboration:
- Dr. Bartłomiej Janowski (CUT) - Małgorzata Jancia (CUT) - Prof. Polycarpos Pissis (NTU Athens) - Dr. Konstantinos Raftopoulos (NTU Athens, CUT, TU Muenchen) - Dr. Bożena Tyliszczak (CUT) - Dr. Katarzyna Bialik-Wąs (CUT) - Dr. Kinga Pielichowska (AGH-UST) - Dr. James Lewicki (LLNL, Livermore) - Dr. Joanna Pagacz (CUT) - Dr. Edyta Hebda (CUT) - Jan Ozimek (CUT)

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“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
THANK YOU FOR YOUR ATTENTION

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JUBILEE SCIENTIFIC CONFERENCE
“PRACTICAL APPLICATIONS OF INNOVATIVE SOLUTIONS RESULTING FROM SCIENTIFIC RESEARCH”
New Polymeric Materials - Challenges and Perspectives
Krzysztof Pielichowski
Cracow University of Technology Department of Chemistry and Technology of Polymers
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