Polymere Materialien (Institut für Technische Chemie und Polymerchemie)

Ausstattung / Equipment Prof. Wilhelm with short descriptions

Here you find a list of the equipment of Prof. Wilhelm including pictures and description. A short tabular overview you can find here.

These methods are available for service measurement of industry or other institutes for a limited extend. Please contact directly one of the professors (see "polymer chemistry - contact") or the specific contact person of the method of interest.

 

 

Synthesis of polymers

 

 

Anionic synthesis

Anionic Synthesis
Contact Person: Matthias Heck, Miriam Cziep

Two vaccum lines for anionic synthesis allows the chemical synthesis of model polymers, especially for complex morphologies like block copolymers, star polymers or com polymers.

 

 

Polymer processing

 

 

Polymer Extrusion (Laboratory scale)

Labstation, Brabender
Contact Person: Ingo Naue

Brabender extruder (Single screw, properties: D=19mm, L=250mm, Tmax=400°C)
used for examination of melt instabilities during extrusion.

Polymer Extrusion (model samples)

Haake Minilab, Thermo Scientific
Contact Person: Ingo Naue

Haake Minilab: Mini Extruder for sample amount as small as 5 g. Equipped with double screws for better mixing, used for model compound or composite materials

injection moulding (Spritzguss)

Haake MiniJet Pro, Thermo Scientific
Contact Person: Ingo Naue

Haake Minijet Pro: injection molding machine for lab scale, starting from sample amounts as low as 2 ml.  In combination with the Haake MiniLab, an extruder in lab scale (see left side of picture), we can produce also composites or blends.

polymer foaming, batch reaktor

custom built SFT-High Pressure Reactor, Supercritical Fluid Technologies
Contact Person: Faust, Lorenz

SFT-High Pressure Reactor: High pressure 100 ml stainless steel vessel with supercritical fluid pump and temperature control unit for batch foaming experiments operating with scCO2 up to 10,000 psi (690 bar) and a max. temperature of 200 °C. Nucleation can be induced either in a one-step foaming process by sudden depressurization or in a two-step foaming process by rapidly heating the saturated sample outside of the reactor in a hot oil bath.

 

 

 Mechanical characterisation of polymers

 

 

Rheometer for low/high viscosity samples

ARES-G2, TA-Instruments
Contact Person: Daniel Zimmermann

ARES rheometer of the latest generation with broad sensitivity range starting from Low viscosity (Water bath) up to polymer melts. The group is owning two devices of this instrument. Including Oven for temperature range from -70 °C to 400 °C). Linear and non-linear regime (FT-Rheology) of material behaviour, FT-Rheology included in standard software.

 

High Senistivity Rheometer

DHR3, TA Instruments
Contact Person: Christopher Klein

Equipped with magnetic bearing, double optical encoder for the deformation and a force rebalance transducer, the DHR3 offers a minimum detectable torque resolution of about 0.05nNm and a displacement of 2nrad. The available Peltier element offers a range of temperatures from 40°C to 200°C.

Rheometer for high viscosity samples
Rheometer DHR1

DHR1, TA-Instruments /> Contact Person: Daniel Zimmermann

Rheometer DHR1 for liquids and polymer melts, stress-controlled. Mainly used in the practical course or for measurements of liquids.

Rubber Rheometer

SISV100, Scarabaeus
Contact person: Shouliang Nie

Rubber tester from Scarabaeus:
allows rheological measurements under pressure
 

Extension rheology

Caber, HAAKE (Thermo Scientific)
Contact Person: Dr. Christopher Klein

Haake Capillary Breakup Extensional Rheometer (CABER)
Allows the determination of the extension characteristics of non-newtonian fluids. Modified by our group for additional force detection. Now its is possibible to measure elongation and force simultaneously.

Capillary Rheometer + Rheotens extension

Rheotester 2000, Goettfert
Contact Person: Wolfgang Arbogast

Capillary rheometer (Goettfert) for extremely high shear rates, equipped with pressure sensors to detect conditions for "shark-skin" and related effects.
Rheotens-extension for the application of elongation shear stress on the polymer sample

Capillary Rheometer

Rheograph 50, Goettfert
Contact Person: Wolfgang Arbogast

Capillary rheometer (Goettfert) for extremely high shear rates (up to 6 Mill 1/s) and high sensitivity
Equipped for PVT-Measurements
Temperature from -40 °C to 400 °C, also food rheology possible

Dielectric spectroscopie

Dielectric Analyzer, Novocontrol
Contact person: Dr. Christopher Klein

Dielectric spectrometer: Detection of molecular motion under shear
Combination with Rheology (ARES for polymer melts) possible.

 

Dynamic mechanical thermoanalyzer (DMTA)

Eplexor 150N, Gabo
Contact Person: Daniel Zimmermann

Gabo Explexor: Dynamic mechanical material testing with high forces and high frequencies:
Linear and non-linear (FT-Rheology) regime of material answer
Elongation or pressure possible

 

 

Combined Methods

 

 

Rheo-NMR

Self-construction,
1H-Relaxationspectroscopy combined with Rheology
Contact Person: Jonas Keller

Rheo-NMR: Correlated information about molecular mobility and mechanical properties. Application examples: Curing of Rubber, Shear induced crystallisation

Rheo-Dielectric

Self-construction:
Fully advanced Rheometer & Dielectric Spectroscopy
Contact Person: Dr. Christopher Klein

Correlated information about local mobility (size scale nm-range) and mechanical properties. Also conductive materials can be analyzed with this method.

SEC-NMR GPC-NMR

Self-construction,
Size exclusion spectroscopy combined with chemical information via NMR-spectroscopy
Contact Person: Carlo Botha

With this new combination we want to achieve chemical information combined with simultaneously recovered size information and separation. The result is a 2D-diagram chemical shift against elution volume.

This characterization method allows to analyze blends or copolymers not only for their average composition. It delivers the full composition as a function of the size of the molecule. For further information please see the page in the research areas "Low-field-NMR and SEC"

One part of the self-developed 3-dimensional spectroscopy: dim1:Size via SEC, dim2: chemical composition via SEC-FTIR or SEC-NMR, dim3: topology, endgroups via SEC-IR-QCL

SEC-FTIR, GPC-FTIR

Self-construction,
Size exclusion spectroscopy combined with chemical information via IR-spectroscopy
Contact Person: Dr. Micheal Pollard

Correlated information about molecular size and chemical composition.
Application example: Chemical composition of blockcopolymers as a function of molecular weight.

One part of the self-developed 3-dimensional spectroscopy: dim1:Size via SEC, dim2: chemical composition via SEC-FTIR or SEC-NMR, dim3: topology, endgroups via SEC-IR-QCL

SEC-IR-QCL

Self-construction,
Size exclusion spectroscopy combined with chemical information via IR-spectroscopy
Contact Person: Dr. Micheal Pollard

Correlated information about molecular size and special chemical groups.
Application example: Amount of rare functional groups (at the moment: 1 Carbonyl group in a polymer of 500.000 g/mol), in future also planned for determination of endgroups and bracnhing units.

One part of the self-developed 3-dimensional spectroscopy: dim1:Size via SEC, dim2: chemical composition via SEC-FTIR or SEC-NMR, dim3: topology, endgroups via SEC-IR-QCL

 

 

Classical polymer characterisation

 

 

Size exclusion chromatography (SEC, GPC)

Agilent 1200 series, Polymer standard service (PSS)
Contact Person: Wolfgang Arbogast

Size exclusion chromatography (german: Gelpermeationschromatographie, GPC)
Calibration versus PS-Standards, solvent normally THF.

Triple Detection: Standard concentration detector either UV or RI-Detector, plus viscosity detector and MALLS-detector (multi-angle-laser-light-scattering) for measurement of unkonwn samples or samples with no available calibration curve.

Infrared spectroscopy (IR)

Vertex 70, Bruker
Contact person: Pollard, Micheal Dr.

Bruker Vertex 70 for FT-IR spectroscopy
equipped with serveral detectors for MIR- and NIR-spectroscopy
with high spectral resolution
and possibility for time resolved spectroscopy.

Small angle X-ray scattering (SAXS)

S3-Micro, Hecus X-ray systems
Contact Person: Dr. Nico Dingenouts

Due to start up money from the Barner-Kowollik group and in a joint effort we are happy to have access to Small-angle X-ray scattering (SAXS) for determination of structure and interaction in solution and ordering in melt and solids, point focus and 2D-Dectection

Differential scanning calorimetry (DSC)

TA Q-200, TA Instruments
Contact Person: Begüm, Ozen

Differential scanning calorimetry (TA-Instruments Q200) for  temperature depending behaviour of polymer and other materials,
temperature range from liquid nitrogen to 400°C

Low-Field NMR-Spectroscopy

Spinsolve 60, Magritek
Contact person: Carlo Botha

The Magritek Spinsolve 60 NMR spectrometer sets a new standard for 60MHz benchtop NMR instruments. The Spinsolve 60 spectrometer provides high quality 1H NMR spectra in seconds and is based on permanent magnets, therefore no liquid nitrogen or helium is needed for the operation.
The main idea for this spectrometer is the usage in combination with GPC as the Magritec is also able to measure samples in flow. With this combination, we plan to build up a two dimensional charaterisation GPC-NMR, with size resolution due to the GPC and chemical information due to the NMR.

Low-Field NMR-Spectroscopy

MQ20 (2x), Bruker
Contact person: Jonas Keller

Bruker Minspec mq20 in two different implementations
a) Standard MQ20 with temperature control for relaxation times measurement to view the dynamics in polymer solutions and melts on a molecular scale
b) Optimized MQ20 with fully digital electronics, special lock system and possibility of shimming, used in a project testing NMR-spectroscopy of polymers with low-field equipment

Dn/dc measurement

DnDc2010, Particle Standard Service (PSS)
Contact Person: Dr. Nico Dingenouts

Measurement of optical contrast, e.g. dn/dc for solutions of polymers allowing a high number of different solvents.
Absolute requirement for static light scattering (SLS), also necessary for GPC/MALLS combination measurements.

Static Light Scattering (SLS) And Dynamic Light Scattering (DLS)

ALV/CGS-3 Goniometer System, ALV, Germany
Contact Person: Dr. Nico Dingenouts

Static Light scattering for determination of molecular weight, radius of gyration and second virial coefficient
High temperature range (up to 90 °C), free selection of angle (Goniometer) and solvent (Quartz cuvettes)
DLS for determination of hydrodynamic radii or aggregation behavior. Small sample amount, also possible in depolarized scattering mode.

Dynamic Light Scattering (DLS) and Zeta-Potential

Nicomp 380 DLS, Particle Sizing Systems (PSS)
Contact Person: Dr. Nico Dingenouts

Dynamic Light Scattering Spectrometer Nicomp 380 DLS from Particle Sizing Systems
with high sensitive detector and strong laser for small particles R>1nm
including
a) multi-angle-option for the necessary extrapolation of hydrodynamic radii of polymers
b) back scattering option for measurement of turbid samples
c) Zeta-Potential measurement for charged samples, e.g. latices charged

Microscopy (Polarisation, Extension)

Zeiss Axiophot, Zeiss
Contact Person: Dr. Christopher Klein

Optical Zeiss Microscope with digital video camera
and two specific sample holders for:
- extension table for polymers under shear
- polarisation microscope, typically used for nematic phases in liquid crystals

Microscopy (Surface, incidient light)

Keyence VHX 900F
Contact Person: Dr. Christopher Klein

Digital microscope for surfaces (incident light microscope) with µm-resolution and an impressiv depth of field due to features as automatic focus stacking. Enlargement rand reaching from 1:1 up to 2000:1. It's the perfect complement to our Zeiss transmission microscope.