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7o WORKSHOP INTERNACIONAL SENAI
                               “MATERIAIS”
          30 de ogosto 2012; Criciúma – SC – Brasil

"Tendências de Pesquisa, Desenvolvimento e Inovação
      dos Materiais para Aplicações Industriais"

   „Pesquisas em materiais poliméricos:
        tendências internacionais
          para o setor industrial”
          Erich Meusel; Rüdiger Strubl; Wolfgang Müller; Ralf-Peter Gottlöber;
                        Nicole Klose; Frances Stöckner; Anne Böhm; Klaus Heinemann
          Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.
          07407 Rudolstadt - Schwarza; GERMANY
          http://www.titk.de;                             E-Mail: heinemann@titk.de
          Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Prof. Dr. Klaus Heinemann
Disposition
                      „Polymer materials research:
       International highly topical trends for the industry sector”
                         TITK – industrial polymeric materials research institute,
                                in the Free State "Thuringia"; Germany

                         Material design using native polymers, esp. Cellulose

the TITK
                         Fibre reinforced materials for the lightweight construction

ALCERU® high tech
                         Nano-composites – polymer materials with uncommon properties
                         Specialized additives aiming at "macromolecular engineering"
Fibre reinforcement
                           Reactive "lcp’s":                             Basic concept for „lc- PEIA”
Nano- composites
                                                                         Selected results
                           Functionalized
                           Nano- layered silicates:                      PEIA- modified „nanoclays”
Specialized additives
                                                                         antibacterial „nanoclays”
- reactive lcp’s
                          Additives enriched
- PEIA-nanoclays          at filament surface:                           Conception – basic idea
- antibac- nanoclays                                                     Design and synthesis of the novel additives
-   additives enriched
                                                                         Filament properties – first results
        at the surface                                                   Résumé and outlook

POLYTRONIC               Functional polymer systems and "POLYTRONIC"
    Fig. 02               Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.    Prof. Dr. Klaus Heinemann
The TITK – 58 Years Industrial Research


Thüringisches Institut
für Textil- und
Kunststoff- Forschung e.V.


       Chemical
       Research



       Plastics
       Research


        Textile and
        Material
        Research


       Functional
       Polymer
                              Innovation            Competence                 Quality
       Systems and             for a progressive productive small and medium-sized industry
       physical
       Research

   Dr.-Ing. Ralf-Uwe Bauer
   Managing Director
   of the TITK reg. assoc.
TITK – the Research Institute
               for
        Polymer Materials

 Innovation   Competence    Quality
ThuringianThuringian Institute and Plastics Research Rudolstadt/ Germany
                           Institute for Textile for Plastics Research (TITK) Rudolstadt / Germany
                                     Department of Functional Polymers Systems

        “Technology triangle” Jena – Rudolstadt – Ilmenau

                                                                                     Friedrich-Schiller
                                                                                     University of Jena
                           Erfurt     Weimar             Jena

                                                                     A4
                                                   B88
                                           B85
                     A71
                                                                A9
Ilmenau                             B88
                                                 Rudolstadt
University of
Technology              Ilmenau           Saalfeld / ICE


                                                                                         Thuringia




Center for Micro- and
Nanotechnology
                                                    Rudolstadt
TITK - Network


                        TITK                                       OMPG
          Thuringian Institute for Textile and      East Thuringian Material Testing Comp.
          Plastics Research reg. assoc.             for Textiles and Plastics
          Employee:     133                         Employee:   44
          Member:        89
          Budget:        10 million EURO            Turnover:     5 million EURO
          Research & Development                    (100% subsidiary of TITK)
          regarding  Materials,                     Materials Testing and
          Processing and Technologies               Characterization Services



           25,1 %           28 %                 33 %           50 %                34 %

Shanghai Lyocell      AP®FIBRE       Technologiegesell-   Rubitherm
 Chemical Fibre         GmbH          schaft Thüringen    Compound
  Engineering         Rudolstadt       mbG & Co. KG         GmbH
Development Co.,
      Ltd.
Fig. 06               Thüringisches Institut für Textil- und Kunststoff-Forschung
Thüringisches Institut für
                Textil- und Kunststoff- Forschung e.V.

 Ostthüringische Materialprüfgesellschaft m. b. H.
          Accredited Testing of Plastics
                                SERVICE
                         Advisory Centre regarding Material Applications
                         Analyses of Recycling Materials
                         Investigations

TESTINGS                                               ANALYSES
 Thermical testings                                       Identification of plastics
 Mechanical testings
 Optical testings
 Flammability testings
 Electrical testings
                                OM                        Chemical Analyses
                                                          Damage analyses
                                                          Particle and
                                                          Surface analyses
 Rheological testings
                                PG
  „Co- Benefactor” of the endowed professorship „Plastics technology”
                             at the "University of Technology Ilmenau"          Fig. 07
TITK - Network
             Research & Development regarding
             Materials, Processing and Technologies




             East Thuringian Material Testing Company
             for Textiles and Plastics
             (100% subsidiary of TITK)
             Materials Testing and
             Characterization Services


   including: Production of
   applicators for the
   Cosmetic Industry
   by electrostatic coating
   using flock fibres

Fig. 08         Thüringisches Institut für Textil- und Kunststoff-Forschung
Thüringisches Institut für Textil- und Kunststoff-Forschung

 Strategic Research Orientation: Industrial Utilization
  Native Polymers and                                                Textile and
  Chemical Research                                               Material Research

                     Functional Polymers – Composite Materials
                      Structural Polymers – Plastics Processing

                                                                  Functional Polymer
  Plastics Research
                                                                   Systems Research
 Research Services, providing the Expertise and Potentials of the TITK
 to the small and medium-sized companies for their own developments

 Portfolio
  • Research and Development Services: Processes and Materials
  • Materials Testing and Characterization Services
  • Selling of Products and Materials resulting from previous Research and
    Development Activities and produced in small scale production
  • Selling of own Patents respectively Licences
Department:   “Native Polymers and Chemical Research”
                                    Dr. Frank Meister – Head of the department



          Field of Research: Structural and functional materials
                             based on “Native Polymers”

          Competences:

          - Characterization of polymers and polymer solutions

          - Shaping of native polymers
            into monofilaments, multifilaments, fibres, films and beads
            by means of “dry -wet” or “wet” techniques

          - Chemical modification of polysaccharides and proteins
            as well as their shaping for technical applications

          - Technologies for production of ceramic fibres and foils


Fig. 10           Thüringisches Institut für Textil- und Kunststoff-Forschung
1. “Native Polymers and Chemical Research”
                             ALCERU® - products – an Overview
                                                                                                                                                       ALCERU® duotherm
                                                                                                                                                                              ALCERU® piezo

Thüringisches Institut
für Textil- und                                     ALCERU® beads
Kunststoff- Forschung e.V.                                         0.45

                                                                    0.4          Polymer/Solvent-System : Polystyrene/THF
                                                                                                                                      34± 5 nm
                                                                                 Pore surface/pore volume : 59 ± 10 m3/cm3
                                                                   0.35          Water retention behaviour: 16 cm3/g



       Chemical                                                     0.3




                                                    PSD (volume)
                                                                   0.25

       Research                                                     0.2

                                                                   0.15

                                                                    0.1

                                                                   0.05




                                                                                                                                                                                     ALCERU® ceramic
                                                                     0
                                                                          0        5       10        15       20        25       30   35    40    45
                                           Information: PSS GmbH Mainz                                Transverse pore diameter [nm]

       Plastics
       Research
                             ALCERU® supersorb
                                          900



                                          800

                                                                          Destw asser

                                          700                             0.9% NaCl-Lösung


        Textile and                       600
                                                                          künstl. Blut




        Material
                                   R %
                                  WV[ ]




                                          500



                                          400


        Research                          300
                                                                                                                                                                             ALCERU®
                                          200



                                          100                                                                                                                               conductive
                                                                                                                                                   ALCERU® exchange
                                            0
                                                0                    10             20          30          40          50
                                                                                                     SAP-Gehalt [%]


       Functional
       Polymer
       Systems and
       physical
       Research               REM micrograph of ALCERU®-supersorb fibres                                                  + Ag+                                       2µm


   Dr.-Ing. Ralf-Uwe Bauer
   Managing Director
   of the TITK reg. assoc.                                                                                                                       ALCERU® antibacterial
"Cell SolutionTM clima"
– a high potential PCM micro-composite material –
Composition: • a new textile micro-composite material with thermo regulating properties
                • PCM (Phase Change Material) is directly and permanently embedded
                                 in the fibre cross-section via dry-jet-wet spinning process
                • highest heat storage capacity (up to 40 Joules per gram of fibre)

                                        Yarn composition / Fibre characteristics
                                        -   cellulose > 47 %
                                        -   PCM component 30 - 40 % (absolute)
                                        -   minerals about 7 %
                                        -   humidity < 12 %
                                        -   finishing agent < 2 %
                                        -   fibre fineness 2.2 - 6.7 dtex (according to customers demands)
                                        -   staple length 38 - 60 mm (according to customers demands)
                                        -   tenacity > 16 cN/tex
                                        -   fibre elongation > 10 %
                                        -   typical phase change temperature* 28 - 35 C

Effectivity: • proved washing permanence up to 50 washing cycles at 60 C
             • excellent textile processability and dyeable in all colour gradations
             • at least 10 % of Cell SolutionTM clima fibres in blended yarn
               (cotton, lyocell, viscose, wool, polyamide, polyester, ...) or fabric are recommended
             • outstanding wearing comfort and micro climate because of
               excellent skin temperature regulation in bed textiles & heat or cold protection clothes


Dr. Frank Meister, Head of Department                                                  Fig. 12
Permethrin - based Nanocomposite ALCERU®-Fiber
                      Requirements:
                      → increasing of blocking effect
                         regarding blood-sucking insects
                      → lower insecticide contamination
                         of clothes wearer




                                                                      T- shirt made of yarns
                                                                  containing 7 % functional fibres
Evaluation                                                         "Cell SolutionTM protection"
of fibres and fabrics made
from insect blocking fibres
demonstrate
the functionality
even after 50 washing cycles                                       3-Phenoxybenzyl(1RS)-cis,trans-3-(2,2-dichlorovinyl)-
and their safety                                                          2,2-dimethylcyclopropanecarboxylate

at typical usage                                                              Permethrin
Fig. 13                Thüringisches Institut für Textil- und Kunststoff-Forschung
Flame- resistant melamine melt- blown fibre mats

            Scheme of modified meltblown process (mini plant at TITK):
            MER melamine resin granulate                                           Constructional
                                               Catalyst                              Industry
                                                                    Crosslinking
                                                          Hot air
                                                                      >180°C
                                                                           °
             Meltblown                                                                    Tempering,
              fibre jet                    +                                              Finishing
                                                                                          Consolidation
                                                                                          (if needed)


                                      Conveying screen


                    • typical value ranges: 10 µm ~1µm, 35 - 350 g/m²,
                                          30 cm width (pilot plant)
                    • inherent flame resistance: LOI = 32
                    • don‘t shrink, melt or drip when exposed to a flame
                    • excellent heat dimensional stability
                    • high thermal & acoustic insulation properties
                    • textile processability
                    • self- bonded web
                    • high filtration efficiency
                    • Excellent chemical resistance especiallyagainst
                      alkali and organics; fair acid - resistant
Fig. 14   Thüringisches Institut für Textil- und Kunststoff-Forschung
2. “Textile and Material Research”

        Research Fields
         ► Fibre Reinforced Composites –
           materials and their production
           technologies

         ► Technical Textiles – textile composites,
           sandwich - structures (light- weight materials)
           and recycling as well as reutilization processes

         ► High Performance Fibres and Textile Fabrics
           – Usage as reinforcing materials
             and other technical applications –

         ► Materials Testing /Characterization




Dr. Renate Lützkendorf, Head of Department                    Fig. 15
2. “Textile and Material Research”
              Fiber reinforced composites – New developments:

                          Composites – reinforced with CARBON fibres
                          Composites – reinforced with ARAMIDE fibres


              "Long fibres reinforced granulates" developments



                                        and                           result in


               ARAMIDE - Recycling fibres      Thermoplastic Matrix fibres             Long fibres
                                                                                       reinforced
                                                                                       granulates
              Matrix materials:       PP; PA 6; PA 6.6

              ARAMIDE - content: up to 70%

              Applications:           - Compounding;
                                      - Injection moulding

              Industry:               - Automobiles
                                      - Tyres

Dr. Renate Lützkendorf, Head of Department                                        Fig. 16
3. “Plastics Research”
                               Dr. Stefan Reinemann
                               head of the department

                             Focus of Research Activities
Thüringisches Institut                                         Compounding          Injection
für Textil- und              ► Development of Formulations,                         Moulding
Kunststoff- Forschung e.V.
                               Processing technologies and
                               Processing methods
       Plastics
       Research              ► Characterization of the Material Behaviour of
                               thermoplastic polymers with the main topics:
       Chemical                - Nanocomposites: Carbon Nano Tubes (CNT)
       Research                                         expanded graphite
                                                                                  Films and Sheets
                                                        layered silicates
       Textile and             - Compounds using el. conductive additives – EM- Shielding
       Material                - Synthetic / Natural / Glass Fibre reinforced Compounds
       Research
                               - Fire - retardant modification and testing
                               - in-situ-Modification of Polyesters / Polyamides
       Functional              - Catalysis of Polyesters / Polyamides
       Polymer                 - “Nanocapsules” with core - shell architectures
       Systems and
       physical                               by means of DENDRITIC POLYMERS
       Research
                             ► Material specific Plastics Recycling –
   Dr.-Ing. Ralf-Uwe Bauer
                               Conceptions, Processes, Products
   Managing Director         ► Transfer Centre for Technologies
   of the TITK reg. assoc.     of material specific Plastics Recycling           Extrusion
3. Department: “Plastics Research”



   Fibre reinforced Polypropylene – using “Synthetic fibres”, e.g. PET or PAN

                       Results using PAN – fibres:
                                    - increase of the STRENGTH:                       up to 30%
                                    - enhancement of the STIFFNESS:                   up to 50%
                                    - improvement of the IMPACT TOUGTNESS:            up to 500%


    "Falling-ball impact test" (- 30°C)




        0% PAN            10% PAN              20% PAN            30% PAN



Dr. Stefan Reinemann, Head of Department                                    Fig. 18
2. Department: “Plastics Research”

          Effect of
          "PA 6 / PP - OMMT - Nanocomposite" – Blends




Fig. 19   Thüringisches Institut für Textil- und Kunststoff-Forschung e.V.
3. Department: “Plastics Research”
          Heat accumulating and Heat storing polymer granulates




              „accumulating“ process     loaded           „pull - out“ process   unloaded

           • PCM – containing Polymer Granulate Material:
           • Melting temperatures of the PCMs used
             are determining the accumulating and the
             “pull - out” temperatures of the heat storage granul es,
              [e.g. (6 / 42 / 52 / 58 und 82) °C]

           Applications as buffer store for:
           - Thermal Solar Collectors
           - Heat Pumps (cold and/or warm site)                                       REM Foto: Einlagerung des Wärmespeicher-Paraffins
                                                                                              in der Polymermatrix

           - Solid - phase burning oven / oil or gas burner / air-conditioning systems, engine heat

Fig. 20   Thüringisches Institut für Textil- und Kunststoff-Forschung e.V.
Heat accumulating and Heat storing polymer granulates

          Reference and Demonstration apparatus at TITK

  Station III :      Floor heating zone            •   Heated area – office floor:    ca. 60 m²
                                                   •   Collector area:                ca. 52 m2
                                                   •   20 Sunlight Collectors:
                                                       (BUDERUS® SKB4.0-w)
                                                   •   Installed Solar power:        26 – 31 KW

                                                   •   Phase Change Temperature:        42 °C
                                                   •   PCM - Granulate Mass:         1000 kg
                                                       height of the granulate bed:      4 cm
                                                   •   Heat power Output:           ca. 40 kW
                                                   •   Floor surface temperature: ca. 30 °C

     Fig. 1: Schematic Plan
             of the Solar – Thermal
             Floor Heating




                                      Fig. 2: Schematic Layout
                                              of the Floor
                                                                                                  21
Fig. 21
TITK- department:       “Plastics Research”
                       “Autoclave Technology”
►   Syntheses of POLYESTERS (PET, PTT, PBT and PEN)
►   Modification of polyesters using Co-monomers
►   "in-situ"- modification of polyesters using various additives
►   Evaluation of catalyzer systems for polyester syntheses
►   Equipment:
      2L- Autoclave                     10L- Autoclave
      - overpressure up to 15 bar         - overpressure up to 20 bar
      - polymer yield up to 1 kg          - polymer yield up to 6 kg

►   Syntheses of POLYAMIDES (PA 6, PA 6.6)
►   Modification of polyamides using Co-monomers
►   "in-situ"- modification of polyamides using additives
►   Equipment:                                                          10L-Autoclave for (trans)esterification
                                                                               and polycondensation
      5L- Autoclave                     10L- Autoclave (t < 320 °C)
      - overpressure up to 20 bar         - overpressure up to 25 bar
      - polymer yield up to 3 kg          - polymer yield up to 5 kg

► New equipment for "up-scaling" of polymer syntheses,
  including “Finisher” to increase the melt viscosity (mbatch ~ 30 kg)

Dr. Stefan Reinemann; head of the department                        Fig. 22
Department: „Functional Polymer Systems
                       and Physical Research”
         Head of the department: Prof. Dr. Klaus Heinemann

        consists of two Research Teams:
Synthetic Functional Polymer Materials and – composites

Organic Nano - Layers and – layer systems            as well as

Micro Structuring and – materials patterning technologies

for POLYMER ELECTRONIC – (IC&M – Technologies),
MICROSYSTEM–, MEDICINE– and TRANSPORT Applic.

Chemical and physico - chemical modification of
technical „High- Performance”- and „High- Tech” – polymers
using functional, migrating or reactive additives to the
generation of specific surface or interface properties
and/or special material functionalities,
including their processing to films and filaments
for the FIBRE– and POLYMER PROCESSING INDUSTRIE
N N
                  C       C        „Synthesis Chemistry”
                      O
  _                            n
            LCP – modified polyamide and polyester resins and fibres
  _         Flame - retardant polyamide and polyester resins and fibres
  _         Surface - modified polymer films and fibres
  _         “reactive polymer blending” and fibres thereof
  _         Polymer modification by “reactive compounding” using
            "chain extender" or "reactive modifier" and fibres thereof
  _         Permanent hydrophobic modification of polyamides & polyesters
  _         Permanent hydrophilic modification of polyamides & polyesters
  _         Fluorescent polyamide and polyester fibres
  _         Functional polymer systems for smart fibres and smart textiles
  _         Bi- component – High temperature – melt spinning technology
            with velocities up to 6.000 m/min (LOY, POY,HOY, FOY)

Fig. 24   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
O                                                                                       O
         C                                                                                       C
     O                                                                                               O
         C                                                                                       C
         O                     OC       CO                    OC        CO       n               O
                                    O                              O


                 ϑ = 250 °C
                 m = 6,5 kg / h
                 DZ = 200 / min
                                                  +   (2n + 2)     H2N               PA 6        COOH
                 t   = 2 min
                 ZSK 25
                 Fa. Werner&Pfleiderer                - ( 2 n + 2 ) H2O

             O                                                                              O
             C                                                                              C
HOOC PA N                                                                                       N PA COOH
             C                                                                              C
             O                    OC         CO              OC         CO   n              O
                                        N                          N
                                        PA                         PA
                                        CO OH                      COOH


         Reaction of lc – poly (esterimide anhydrides) with PA 6
                                                                                                 Fig. 25
         in molten state to form graft - block - copolyesterimides
Mode of action in polyamide fibres

        UV- or light                                                 PA 6 – incompatible component
     stabilizer molecule                                              (migration causing element)
reactive lcp’s
PEIA &                                                                                                in reality:
Nanoclays
“Antibac –                                                                                          FORMATION
Nanoclays”
                                                                                                      OF A
Additives                                                                                         CONCENTRATION
enriched                                                                                            GRADIENT !
at the surface
conception                                                                                         may be expected
basic idea
objectives
                 component with PA 6 – affinity
syntheses           (anchoring segment)                                                       PA 6 – fibre surface
processing
results
                 Spontaneous migration of the stabilizer additives during the fibre forming process
analyses
                 ➄ Enrichment of the stabilizer molecules nearby the boundary layer of PA fibre
résumé
outlook          Immobilization of the complex additives molecule in the accomplished fibre

the TITK         Improved light protection efficiency by accessibility of stabilizer molecules in the surface region

Fig. 26                Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.        Prof. Dr. Klaus Heinemann
„Reactive Complex- forming agent s – Biocides”

                          Application of a novel Silver Salt – Complex in PA 6.6
          Reference                250 ppm                 750 ppm                  1500 ppm    5000 ppm




Fig. 27               Thüringisches InstitutInstitut fürfür Textil- und Kunststoff-Forschung
                           Thüringisches für Textil- und Kunststoff-Forschung
                              Thüringisches Institut Textil- und Kunststoff-Forschung          Steffi Sensfussund Team
                                                                                                  Dr. R. Strubl
“Modular multifunctional apparatus for additive syntheses”




Fig. 28   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
“Modular multifunctional apparatus for additive syntheses”

                    Chemical syntheses in liquid media,
                                               also under explosion- protected conditions
                    ► Batch- Volumes:                            10 Litre (stainless steel) and 16 Litre (titanium)
                    ► Reaction temperatures: up to 200 °C                                                        up to 300 °C
                    ► Reaction pressures:                        up to 0,5 bar
                    ► Reaction media:                            homogeneous and heterogeneous phases
                    ► Isolation of products:        vacuum distillation; evaporation;
                                                     phase separation; Extraction;
                    for:     • alkylations; acylations
                             • halogenations; nitrations; sulphonations; epoxidations
                             • esterifications; transesterifications; amidations; saponification
                    ► Online-IR-Spectroscopy for reaction analysis und -optimization (                                  7 bar)
                    ► Calorimetry of reactions, also in case of increased pressure                                   (100 bar)
                    Compound separations by vacuum distillation up to 15 kg/h (offer of service)

                    Chemical syntheses at „Kilogram – scale“ (customer order)


Fig. 29   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
Department of FUNCTIONAL POLYMER SYSTEMS




                       „Processing Equipment”




Fig. 30   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
Micro – twin- screw – melt compounder & spinning device
             Technical Parameters:                  - Polymer melt temperatures:        ϑ ≤ 350 °C;
                                                    - Melt volume – Polymer mass: v = 5,5 cm3; m ~ 8 g !!!;
                                                    - Screw speed:                      n = (1 … 360) min-1




                                                          HAAKE „MiniLab”
                                                       Thermo ELECTRON GmbH
                                                            76227 Karlsruhe

Fig. 31   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
Micro – melt spinning apparatus

              Micro – extrusion system „Minitruder” (Fa. Randcastle Inc.; USA)
              - Polymer melt temperatures: ϑmax ≤ 430 °C
              - throughputs:                                                  10 - 120 g/h          or      80 - 980 g/h




Fig. 32   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
Bicomponent – High temperature – melt spinning device
                       with winding speeds up to 6.000 m/min

                                     Bicomponent nozzle
                                        outer          inner
                                            annular gap
                                       (sheath)       (core)




                                                  Quelle: EMPA & Fa. Fourné


Fig. 33   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
„POLYTRONIC”
      Focus: Generation of polymer-based electronic system components
             Functional Polymer Systems: „from Material – to System”

      Technology developments in the direction of „upscaling“ of
      explored microtechnologies of "polymer engineering" in favour of the
      scientific and technical prearrangement of the serial manufacturing of:
      –   Polymer- based field effect transistors and integrated circuits,
      –   Sensors,
      –   Actuators,
      –   Photovoltaic Cells und Modules as well as
      –   Modules by using substances with „switchable“
          electrochromic, photochromic and thermochromic properties;
      for applications regarding
      information-, communication- and media technology, microelectronics,
      microsystems-, medical- and traffic technology, including
      "Reel-to-Reel"- Technologies       for - coating
                                         and - micro structuring
Fig. 34   Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.   Dr. Rüdiger Strubl & Team
Department: “Functional Polymer Systems”

     I. Topic: Polymer Electronic Applications
                                      Schematic View of a PFET (Polymer-Field-Effect-Transistor)
                                                                   on a flexible polymer film
2 mm                                                                                                          metal or
                                 d: 100 - 3.000 nm                      Gate electrode
                                                                                                              conducting
                                                                                                              polymer
                                   Insulator (d: 400 nm – 1.000 nm                                            (PANI,
                                                                                                              PEDOT:PSS)
                                                Semi conductor
                                                                                                              Poly(3-alkyl-
                                               (d: 5 nm – 50 nm)
                                                                                                              thiophenes)
                                                                                                              metal, ITO or
                                                                                             drain            conducting
                                                                                                              polymer
                                                                                   source                     (PANI,
                           0,5 - 3 mm                                                                         PEDOT:PSS)
                                                                                                    PET; PI; ABS; glass
                 flexible polymer substrate – d: 100 - 200 µm

Fig. 35 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Mario Schrödner & Team
Department: “Functional Polymer Systems”

   II. Topic: Flexible Polymer Photovoltaic
   Possible Applications:

                              • Solar cells on tents
                                  (esp. for aid organisations)


                              • Solar cells on textiles
                                  [esp. for military and sport textiles (GPS)]


                              • Solar cells on credit cards
                                (credit cards – real „smart cards”)




Fig. 36 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Mario Schrödner & Team
II. Topic: Flexible Polymer Photovoltaic
 P                                        Possible Applications:
                                                                                      Portable PV-
      Consumer
                                                                                             Modules
      electronics




                                         intelligent                       electronic
                                         packaging                         textiles
        Modules on
      curved surfaces
                                                    Building Integration                              Smart cards
                                                                                                                     80
                                                                                                                 1   .9
                                                                                                                     23
                                                                                                                 4   56
                                                                                                                 7    0
                                                                                                                     89
                                                                                                                 *   0#



                                                               (BIPV)
Fig. 37 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.Frau Dr. Steffi Sensfuß & Team
department: „Functional Polymer Systems” – "POLYTRONIC"
          I. Topic:         II. Topic: Polymer Solar Cell
                                          Applications:
  Polymer-Field-Effect-Transistors
           Schematic Drawing PFET




                                    III. Topic:

          Micro- and Nanometre-thin Functional Layers
                 by „Reel - to - Reel” – Technology
                   Coating Equipment "LBA 200"
Fig. 38                                                   Dr. Schrödner & Team
Reel – to – Reel coating equipment „LBA 200”

                                                                                         Antrag                               Lösungsmittel
                                                                                                       IR-Feld
                                                                           Beschich-
                                                                           tungsmittel                                    T
                                                                                                     Trocknung-/
                                                                                                     Erstarrungsstrecke
                                                                                            Corona

                                                                                                      Abwicklung                        Aufwicklung




                                                                           Steuerung
                                                                              PC             Rolle - zu - Rolle

                Parameters:
                Width of the substrate tape: ≤ 20 cm
                Speed of the tape:           ≤ 10 m/min
                Corona Activation:            2.5 kW
                Infrared – dryer:             3.4 kW
                Hot air – dryer:        80 – 120 ° C

       Continuous wet coating using
  diluted polymer- solutions/ -dispersions
 by means of „Reel- to- Reel– Technology”
Fig. 39          Thüringisches Institut für Textil- und Kunststoff-Forschung   Frau DP K. Schultheis; Dr. L. Blankenburg
Roll-to-Roll (R2R) Coating Technology
                             processing flexible Polymer Solar Cells
                       Spin coating          Doctor blading               continuous coating R2R



          Processing parameters R2R
          Materials
          - Substrate: PET/ITO (175 µm)
          - Baytron PH (~100 nm)
          - P3HT/PCBM (1:1) 1.2% in Chlorobenzene (~60 - 150 nm)
          Technology parameters
          - Corona – pre- treatment: 200 W
          - Velocity of the band: 1 - 2 m/min                                                     20
          - Width of the slot: 3 - 5 cm                                                                                  dark
                                                                                                                         illuminated
          - Dosing rate: 1 - 5 ml/min                                                             15

          - Circulating air drying: 80 °C (Baytron)                                                            ISC:      6.13 mA/cm2
                                                                                                  10           VOC:    618 mV




                                                                              current [mA/cm ]
                                                                             2
                                                                                                               FF:     0.46
          Completing of the Cells - discontinuous                                                              ηAM1.5: 1.74 %
                                                                                                      5
          - Vapour deposition of the Al- electrode
          - Annealing: 5 min at 100°C                                                                 0
                                                                                           -0,5            0                     0,5   1
          Measuring conditions – Cell characterisation                                                -5
          - AM 1.5
          - Cell dimension: 5x5 mm²                                                               -10
                                                                                                                      bias [V]
          - environmental conditions
                                        Efficiencies: „Spincoating” = 5,4 %                       →        „R2R” = 1,7 % →             4,5 %
Fig. 40               Thüringisches Institut für Textil- und Kunststoff-Forschung Frau DP K. Schultheis; Dr. L. Blankenburg

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Pesquisas em materiais poliméricos: tendências internacionais para o setor industrial

  • 1. 7o WORKSHOP INTERNACIONAL SENAI “MATERIAIS” 30 de ogosto 2012; Criciúma – SC – Brasil "Tendências de Pesquisa, Desenvolvimento e Inovação dos Materiais para Aplicações Industriais" „Pesquisas em materiais poliméricos: tendências internacionais para o setor industrial” Erich Meusel; Rüdiger Strubl; Wolfgang Müller; Ralf-Peter Gottlöber; Nicole Klose; Frances Stöckner; Anne Böhm; Klaus Heinemann Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. 07407 Rudolstadt - Schwarza; GERMANY http://www.titk.de; E-Mail: heinemann@titk.de Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Prof. Dr. Klaus Heinemann
  • 2. Disposition „Polymer materials research: International highly topical trends for the industry sector” TITK – industrial polymeric materials research institute, in the Free State "Thuringia"; Germany Material design using native polymers, esp. Cellulose the TITK Fibre reinforced materials for the lightweight construction ALCERU® high tech Nano-composites – polymer materials with uncommon properties Specialized additives aiming at "macromolecular engineering" Fibre reinforcement Reactive "lcp’s": Basic concept for „lc- PEIA” Nano- composites Selected results Functionalized Nano- layered silicates: PEIA- modified „nanoclays” Specialized additives antibacterial „nanoclays” - reactive lcp’s Additives enriched - PEIA-nanoclays at filament surface: Conception – basic idea - antibac- nanoclays Design and synthesis of the novel additives - additives enriched Filament properties – first results at the surface Résumé and outlook POLYTRONIC Functional polymer systems and "POLYTRONIC" Fig. 02 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Prof. Dr. Klaus Heinemann
  • 3. The TITK – 58 Years Industrial Research Thüringisches Institut für Textil- und Kunststoff- Forschung e.V. Chemical Research Plastics Research Textile and Material Research Functional Polymer Innovation Competence Quality Systems and for a progressive productive small and medium-sized industry physical Research Dr.-Ing. Ralf-Uwe Bauer Managing Director of the TITK reg. assoc.
  • 4. TITK – the Research Institute for Polymer Materials Innovation Competence Quality
  • 5. ThuringianThuringian Institute and Plastics Research Rudolstadt/ Germany Institute for Textile for Plastics Research (TITK) Rudolstadt / Germany Department of Functional Polymers Systems “Technology triangle” Jena – Rudolstadt – Ilmenau Friedrich-Schiller University of Jena Erfurt Weimar Jena A4 B88 B85 A71 A9 Ilmenau B88 Rudolstadt University of Technology Ilmenau Saalfeld / ICE Thuringia Center for Micro- and Nanotechnology Rudolstadt
  • 6. TITK - Network TITK OMPG Thuringian Institute for Textile and East Thuringian Material Testing Comp. Plastics Research reg. assoc. for Textiles and Plastics Employee: 133 Employee: 44 Member: 89 Budget: 10 million EURO Turnover: 5 million EURO Research & Development (100% subsidiary of TITK) regarding Materials, Materials Testing and Processing and Technologies Characterization Services 25,1 % 28 % 33 % 50 % 34 % Shanghai Lyocell AP®FIBRE Technologiegesell- Rubitherm Chemical Fibre GmbH schaft Thüringen Compound Engineering Rudolstadt mbG & Co. KG GmbH Development Co., Ltd. Fig. 06 Thüringisches Institut für Textil- und Kunststoff-Forschung
  • 7. Thüringisches Institut für Textil- und Kunststoff- Forschung e.V. Ostthüringische Materialprüfgesellschaft m. b. H. Accredited Testing of Plastics SERVICE Advisory Centre regarding Material Applications Analyses of Recycling Materials Investigations TESTINGS ANALYSES Thermical testings Identification of plastics Mechanical testings Optical testings Flammability testings Electrical testings OM Chemical Analyses Damage analyses Particle and Surface analyses Rheological testings PG „Co- Benefactor” of the endowed professorship „Plastics technology” at the "University of Technology Ilmenau" Fig. 07
  • 8. TITK - Network Research & Development regarding Materials, Processing and Technologies East Thuringian Material Testing Company for Textiles and Plastics (100% subsidiary of TITK) Materials Testing and Characterization Services including: Production of applicators for the Cosmetic Industry by electrostatic coating using flock fibres Fig. 08 Thüringisches Institut für Textil- und Kunststoff-Forschung
  • 9. Thüringisches Institut für Textil- und Kunststoff-Forschung Strategic Research Orientation: Industrial Utilization Native Polymers and Textile and Chemical Research Material Research Functional Polymers – Composite Materials Structural Polymers – Plastics Processing Functional Polymer Plastics Research Systems Research Research Services, providing the Expertise and Potentials of the TITK to the small and medium-sized companies for their own developments Portfolio • Research and Development Services: Processes and Materials • Materials Testing and Characterization Services • Selling of Products and Materials resulting from previous Research and Development Activities and produced in small scale production • Selling of own Patents respectively Licences
  • 10. Department: “Native Polymers and Chemical Research” Dr. Frank Meister – Head of the department Field of Research: Structural and functional materials based on “Native Polymers” Competences: - Characterization of polymers and polymer solutions - Shaping of native polymers into monofilaments, multifilaments, fibres, films and beads by means of “dry -wet” or “wet” techniques - Chemical modification of polysaccharides and proteins as well as their shaping for technical applications - Technologies for production of ceramic fibres and foils Fig. 10 Thüringisches Institut für Textil- und Kunststoff-Forschung
  • 11. 1. “Native Polymers and Chemical Research” ALCERU® - products – an Overview ALCERU® duotherm ALCERU® piezo Thüringisches Institut für Textil- und ALCERU® beads Kunststoff- Forschung e.V. 0.45 0.4 Polymer/Solvent-System : Polystyrene/THF 34± 5 nm Pore surface/pore volume : 59 ± 10 m3/cm3 0.35 Water retention behaviour: 16 cm3/g Chemical 0.3 PSD (volume) 0.25 Research 0.2 0.15 0.1 0.05 ALCERU® ceramic 0 0 5 10 15 20 25 30 35 40 45 Information: PSS GmbH Mainz Transverse pore diameter [nm] Plastics Research ALCERU® supersorb 900 800 Destw asser 700 0.9% NaCl-Lösung Textile and 600 künstl. Blut Material R % WV[ ] 500 400 Research 300 ALCERU® 200 100 conductive ALCERU® exchange 0 0 10 20 30 40 50 SAP-Gehalt [%] Functional Polymer Systems and physical Research REM micrograph of ALCERU®-supersorb fibres + Ag+ 2µm Dr.-Ing. Ralf-Uwe Bauer Managing Director of the TITK reg. assoc. ALCERU® antibacterial
  • 12. "Cell SolutionTM clima" – a high potential PCM micro-composite material – Composition: • a new textile micro-composite material with thermo regulating properties • PCM (Phase Change Material) is directly and permanently embedded in the fibre cross-section via dry-jet-wet spinning process • highest heat storage capacity (up to 40 Joules per gram of fibre) Yarn composition / Fibre characteristics - cellulose > 47 % - PCM component 30 - 40 % (absolute) - minerals about 7 % - humidity < 12 % - finishing agent < 2 % - fibre fineness 2.2 - 6.7 dtex (according to customers demands) - staple length 38 - 60 mm (according to customers demands) - tenacity > 16 cN/tex - fibre elongation > 10 % - typical phase change temperature* 28 - 35 C Effectivity: • proved washing permanence up to 50 washing cycles at 60 C • excellent textile processability and dyeable in all colour gradations • at least 10 % of Cell SolutionTM clima fibres in blended yarn (cotton, lyocell, viscose, wool, polyamide, polyester, ...) or fabric are recommended • outstanding wearing comfort and micro climate because of excellent skin temperature regulation in bed textiles & heat or cold protection clothes Dr. Frank Meister, Head of Department Fig. 12
  • 13. Permethrin - based Nanocomposite ALCERU®-Fiber Requirements: → increasing of blocking effect regarding blood-sucking insects → lower insecticide contamination of clothes wearer T- shirt made of yarns containing 7 % functional fibres Evaluation "Cell SolutionTM protection" of fibres and fabrics made from insect blocking fibres demonstrate the functionality even after 50 washing cycles 3-Phenoxybenzyl(1RS)-cis,trans-3-(2,2-dichlorovinyl)- and their safety 2,2-dimethylcyclopropanecarboxylate at typical usage Permethrin Fig. 13 Thüringisches Institut für Textil- und Kunststoff-Forschung
  • 14. Flame- resistant melamine melt- blown fibre mats Scheme of modified meltblown process (mini plant at TITK): MER melamine resin granulate Constructional Catalyst Industry Crosslinking Hot air >180°C ° Meltblown Tempering, fibre jet + Finishing Consolidation (if needed) Conveying screen • typical value ranges: 10 µm ~1µm, 35 - 350 g/m², 30 cm width (pilot plant) • inherent flame resistance: LOI = 32 • don‘t shrink, melt or drip when exposed to a flame • excellent heat dimensional stability • high thermal & acoustic insulation properties • textile processability • self- bonded web • high filtration efficiency • Excellent chemical resistance especiallyagainst alkali and organics; fair acid - resistant Fig. 14 Thüringisches Institut für Textil- und Kunststoff-Forschung
  • 15. 2. “Textile and Material Research” Research Fields ► Fibre Reinforced Composites – materials and their production technologies ► Technical Textiles – textile composites, sandwich - structures (light- weight materials) and recycling as well as reutilization processes ► High Performance Fibres and Textile Fabrics – Usage as reinforcing materials and other technical applications – ► Materials Testing /Characterization Dr. Renate Lützkendorf, Head of Department Fig. 15
  • 16. 2. “Textile and Material Research” Fiber reinforced composites – New developments: Composites – reinforced with CARBON fibres Composites – reinforced with ARAMIDE fibres "Long fibres reinforced granulates" developments and result in ARAMIDE - Recycling fibres Thermoplastic Matrix fibres Long fibres reinforced granulates Matrix materials: PP; PA 6; PA 6.6 ARAMIDE - content: up to 70% Applications: - Compounding; - Injection moulding Industry: - Automobiles - Tyres Dr. Renate Lützkendorf, Head of Department Fig. 16
  • 17. 3. “Plastics Research” Dr. Stefan Reinemann head of the department Focus of Research Activities Thüringisches Institut Compounding Injection für Textil- und ► Development of Formulations, Moulding Kunststoff- Forschung e.V. Processing technologies and Processing methods Plastics Research ► Characterization of the Material Behaviour of thermoplastic polymers with the main topics: Chemical - Nanocomposites: Carbon Nano Tubes (CNT) Research expanded graphite Films and Sheets layered silicates Textile and - Compounds using el. conductive additives – EM- Shielding Material - Synthetic / Natural / Glass Fibre reinforced Compounds Research - Fire - retardant modification and testing - in-situ-Modification of Polyesters / Polyamides Functional - Catalysis of Polyesters / Polyamides Polymer - “Nanocapsules” with core - shell architectures Systems and physical by means of DENDRITIC POLYMERS Research ► Material specific Plastics Recycling – Dr.-Ing. Ralf-Uwe Bauer Conceptions, Processes, Products Managing Director ► Transfer Centre for Technologies of the TITK reg. assoc. of material specific Plastics Recycling Extrusion
  • 18. 3. Department: “Plastics Research” Fibre reinforced Polypropylene – using “Synthetic fibres”, e.g. PET or PAN Results using PAN – fibres: - increase of the STRENGTH: up to 30% - enhancement of the STIFFNESS: up to 50% - improvement of the IMPACT TOUGTNESS: up to 500% "Falling-ball impact test" (- 30°C) 0% PAN 10% PAN 20% PAN 30% PAN Dr. Stefan Reinemann, Head of Department Fig. 18
  • 19. 2. Department: “Plastics Research” Effect of "PA 6 / PP - OMMT - Nanocomposite" – Blends Fig. 19 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V.
  • 20. 3. Department: “Plastics Research” Heat accumulating and Heat storing polymer granulates „accumulating“ process loaded „pull - out“ process unloaded • PCM – containing Polymer Granulate Material: • Melting temperatures of the PCMs used are determining the accumulating and the “pull - out” temperatures of the heat storage granul es, [e.g. (6 / 42 / 52 / 58 und 82) °C] Applications as buffer store for: - Thermal Solar Collectors - Heat Pumps (cold and/or warm site) REM Foto: Einlagerung des Wärmespeicher-Paraffins in der Polymermatrix - Solid - phase burning oven / oil or gas burner / air-conditioning systems, engine heat Fig. 20 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V.
  • 21. Heat accumulating and Heat storing polymer granulates Reference and Demonstration apparatus at TITK Station III : Floor heating zone • Heated area – office floor: ca. 60 m² • Collector area: ca. 52 m2 • 20 Sunlight Collectors: (BUDERUS® SKB4.0-w) • Installed Solar power: 26 – 31 KW • Phase Change Temperature: 42 °C • PCM - Granulate Mass: 1000 kg height of the granulate bed: 4 cm • Heat power Output: ca. 40 kW • Floor surface temperature: ca. 30 °C Fig. 1: Schematic Plan of the Solar – Thermal Floor Heating Fig. 2: Schematic Layout of the Floor 21 Fig. 21
  • 22. TITK- department: “Plastics Research” “Autoclave Technology” ► Syntheses of POLYESTERS (PET, PTT, PBT and PEN) ► Modification of polyesters using Co-monomers ► "in-situ"- modification of polyesters using various additives ► Evaluation of catalyzer systems for polyester syntheses ► Equipment: 2L- Autoclave 10L- Autoclave - overpressure up to 15 bar - overpressure up to 20 bar - polymer yield up to 1 kg - polymer yield up to 6 kg ► Syntheses of POLYAMIDES (PA 6, PA 6.6) ► Modification of polyamides using Co-monomers ► "in-situ"- modification of polyamides using additives ► Equipment: 10L-Autoclave for (trans)esterification and polycondensation 5L- Autoclave 10L- Autoclave (t < 320 °C) - overpressure up to 20 bar - overpressure up to 25 bar - polymer yield up to 3 kg - polymer yield up to 5 kg ► New equipment for "up-scaling" of polymer syntheses, including “Finisher” to increase the melt viscosity (mbatch ~ 30 kg) Dr. Stefan Reinemann; head of the department Fig. 22
  • 23. Department: „Functional Polymer Systems and Physical Research” Head of the department: Prof. Dr. Klaus Heinemann consists of two Research Teams: Synthetic Functional Polymer Materials and – composites Organic Nano - Layers and – layer systems as well as Micro Structuring and – materials patterning technologies for POLYMER ELECTRONIC – (IC&M – Technologies), MICROSYSTEM–, MEDICINE– and TRANSPORT Applic. Chemical and physico - chemical modification of technical „High- Performance”- and „High- Tech” – polymers using functional, migrating or reactive additives to the generation of specific surface or interface properties and/or special material functionalities, including their processing to films and filaments for the FIBRE– and POLYMER PROCESSING INDUSTRIE
  • 24. N N C C „Synthesis Chemistry” O _ n LCP – modified polyamide and polyester resins and fibres _ Flame - retardant polyamide and polyester resins and fibres _ Surface - modified polymer films and fibres _ “reactive polymer blending” and fibres thereof _ Polymer modification by “reactive compounding” using "chain extender" or "reactive modifier" and fibres thereof _ Permanent hydrophobic modification of polyamides & polyesters _ Permanent hydrophilic modification of polyamides & polyesters _ Fluorescent polyamide and polyester fibres _ Functional polymer systems for smart fibres and smart textiles _ Bi- component – High temperature – melt spinning technology with velocities up to 6.000 m/min (LOY, POY,HOY, FOY) Fig. 24 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 25. O O C C O O C C O OC CO OC CO n O O O ϑ = 250 °C m = 6,5 kg / h DZ = 200 / min + (2n + 2) H2N PA 6 COOH t = 2 min ZSK 25 Fa. Werner&Pfleiderer - ( 2 n + 2 ) H2O O O C C HOOC PA N N PA COOH C C O OC CO OC CO n O N N PA PA CO OH COOH Reaction of lc – poly (esterimide anhydrides) with PA 6 Fig. 25 in molten state to form graft - block - copolyesterimides
  • 26. Mode of action in polyamide fibres UV- or light PA 6 – incompatible component stabilizer molecule (migration causing element) reactive lcp’s PEIA & in reality: Nanoclays “Antibac – FORMATION Nanoclays” OF A Additives CONCENTRATION enriched GRADIENT ! at the surface conception may be expected basic idea objectives component with PA 6 – affinity syntheses (anchoring segment) PA 6 – fibre surface processing results Spontaneous migration of the stabilizer additives during the fibre forming process analyses ➄ Enrichment of the stabilizer molecules nearby the boundary layer of PA fibre résumé outlook Immobilization of the complex additives molecule in the accomplished fibre the TITK Improved light protection efficiency by accessibility of stabilizer molecules in the surface region Fig. 26 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Prof. Dr. Klaus Heinemann
  • 27. „Reactive Complex- forming agent s – Biocides” Application of a novel Silver Salt – Complex in PA 6.6 Reference 250 ppm 750 ppm 1500 ppm 5000 ppm Fig. 27 Thüringisches InstitutInstitut fürfür Textil- und Kunststoff-Forschung Thüringisches für Textil- und Kunststoff-Forschung Thüringisches Institut Textil- und Kunststoff-Forschung Steffi Sensfussund Team Dr. R. Strubl
  • 28. “Modular multifunctional apparatus for additive syntheses” Fig. 28 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 29. “Modular multifunctional apparatus for additive syntheses” Chemical syntheses in liquid media, also under explosion- protected conditions ► Batch- Volumes: 10 Litre (stainless steel) and 16 Litre (titanium) ► Reaction temperatures: up to 200 °C up to 300 °C ► Reaction pressures: up to 0,5 bar ► Reaction media: homogeneous and heterogeneous phases ► Isolation of products: vacuum distillation; evaporation; phase separation; Extraction; for: • alkylations; acylations • halogenations; nitrations; sulphonations; epoxidations • esterifications; transesterifications; amidations; saponification ► Online-IR-Spectroscopy for reaction analysis und -optimization ( 7 bar) ► Calorimetry of reactions, also in case of increased pressure (100 bar) Compound separations by vacuum distillation up to 15 kg/h (offer of service) Chemical syntheses at „Kilogram – scale“ (customer order) Fig. 29 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 30. Department of FUNCTIONAL POLYMER SYSTEMS „Processing Equipment” Fig. 30 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 31. Micro – twin- screw – melt compounder & spinning device Technical Parameters: - Polymer melt temperatures: ϑ ≤ 350 °C; - Melt volume – Polymer mass: v = 5,5 cm3; m ~ 8 g !!!; - Screw speed: n = (1 … 360) min-1 HAAKE „MiniLab” Thermo ELECTRON GmbH 76227 Karlsruhe Fig. 31 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 32. Micro – melt spinning apparatus Micro – extrusion system „Minitruder” (Fa. Randcastle Inc.; USA) - Polymer melt temperatures: ϑmax ≤ 430 °C - throughputs: 10 - 120 g/h or 80 - 980 g/h Fig. 32 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 33. Bicomponent – High temperature – melt spinning device with winding speeds up to 6.000 m/min Bicomponent nozzle outer inner annular gap (sheath) (core) Quelle: EMPA & Fa. Fourné Fig. 33 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 34. „POLYTRONIC” Focus: Generation of polymer-based electronic system components Functional Polymer Systems: „from Material – to System” Technology developments in the direction of „upscaling“ of explored microtechnologies of "polymer engineering" in favour of the scientific and technical prearrangement of the serial manufacturing of: – Polymer- based field effect transistors and integrated circuits, – Sensors, – Actuators, – Photovoltaic Cells und Modules as well as – Modules by using substances with „switchable“ electrochromic, photochromic and thermochromic properties; for applications regarding information-, communication- and media technology, microelectronics, microsystems-, medical- and traffic technology, including "Reel-to-Reel"- Technologies for - coating and - micro structuring Fig. 34 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rüdiger Strubl & Team
  • 35. Department: “Functional Polymer Systems” I. Topic: Polymer Electronic Applications Schematic View of a PFET (Polymer-Field-Effect-Transistor) on a flexible polymer film 2 mm metal or d: 100 - 3.000 nm Gate electrode conducting polymer Insulator (d: 400 nm – 1.000 nm (PANI, PEDOT:PSS) Semi conductor Poly(3-alkyl- (d: 5 nm – 50 nm) thiophenes) metal, ITO or drain conducting polymer source (PANI, 0,5 - 3 mm PEDOT:PSS) PET; PI; ABS; glass flexible polymer substrate – d: 100 - 200 µm Fig. 35 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Mario Schrödner & Team
  • 36. Department: “Functional Polymer Systems” II. Topic: Flexible Polymer Photovoltaic Possible Applications: • Solar cells on tents (esp. for aid organisations) • Solar cells on textiles [esp. for military and sport textiles (GPS)] • Solar cells on credit cards (credit cards – real „smart cards”) Fig. 36 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Mario Schrödner & Team
  • 37. II. Topic: Flexible Polymer Photovoltaic P Possible Applications: Portable PV- Consumer Modules electronics intelligent electronic packaging textiles Modules on curved surfaces Building Integration Smart cards 80 1 .9 23 4 56 7 0 89 * 0# (BIPV) Fig. 37 Thüringisches Institut für Textil- und Kunststoff-Forschung (TITK) e. V.Frau Dr. Steffi Sensfuß & Team
  • 38. department: „Functional Polymer Systems” – "POLYTRONIC" I. Topic: II. Topic: Polymer Solar Cell Applications: Polymer-Field-Effect-Transistors Schematic Drawing PFET III. Topic: Micro- and Nanometre-thin Functional Layers by „Reel - to - Reel” – Technology Coating Equipment "LBA 200" Fig. 38 Dr. Schrödner & Team
  • 39. Reel – to – Reel coating equipment „LBA 200” Antrag Lösungsmittel IR-Feld Beschich- tungsmittel T Trocknung-/ Erstarrungsstrecke Corona Abwicklung Aufwicklung Steuerung PC Rolle - zu - Rolle Parameters: Width of the substrate tape: ≤ 20 cm Speed of the tape: ≤ 10 m/min Corona Activation: 2.5 kW Infrared – dryer: 3.4 kW Hot air – dryer: 80 – 120 ° C Continuous wet coating using diluted polymer- solutions/ -dispersions by means of „Reel- to- Reel– Technology” Fig. 39 Thüringisches Institut für Textil- und Kunststoff-Forschung Frau DP K. Schultheis; Dr. L. Blankenburg
  • 40. Roll-to-Roll (R2R) Coating Technology processing flexible Polymer Solar Cells Spin coating Doctor blading continuous coating R2R Processing parameters R2R Materials - Substrate: PET/ITO (175 µm) - Baytron PH (~100 nm) - P3HT/PCBM (1:1) 1.2% in Chlorobenzene (~60 - 150 nm) Technology parameters - Corona – pre- treatment: 200 W - Velocity of the band: 1 - 2 m/min 20 - Width of the slot: 3 - 5 cm dark illuminated - Dosing rate: 1 - 5 ml/min 15 - Circulating air drying: 80 °C (Baytron) ISC: 6.13 mA/cm2 10 VOC: 618 mV current [mA/cm ] 2 FF: 0.46 Completing of the Cells - discontinuous ηAM1.5: 1.74 % 5 - Vapour deposition of the Al- electrode - Annealing: 5 min at 100°C 0 -0,5 0 0,5 1 Measuring conditions – Cell characterisation -5 - AM 1.5 - Cell dimension: 5x5 mm² -10 bias [V] - environmental conditions Efficiencies: „Spincoating” = 5,4 % → „R2R” = 1,7 % → 4,5 % Fig. 40 Thüringisches Institut für Textil- und Kunststoff-Forschung Frau DP K. Schultheis; Dr. L. Blankenburg