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EC-Twist - MEP Instruments

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<strong>EC</strong>-<strong>Twist</strong><br />

Dynamic Mechanical Analyzer<br />

::: Intelligence in Rheometry


A New <strong>Twist</strong> on DMTA<br />

<strong>EC</strong>-<strong>Twist</strong> is a Dynamic Mechanical Analyzer<br />

for DMTA analysis on solids as well as liquids.<br />

The modular system performs measurements<br />

in torsion and extension and is the first DMTA<br />

solution that can also be used for shearrheological<br />

experiments – at unprecedented<br />

precision.<br />

Easy adaptation<br />

<strong>EC</strong>-<strong>Twist</strong> builds on your applications. Whatever your DMTA<br />

requirements are and will be in the future – <strong>EC</strong>-<strong>Twist</strong> is<br />

efficiently and comfortably adapted to meet your needs.<br />

The flexible application software and patented features<br />

such as Toolmaster TM , an automatic tool recognition and<br />

configuration system, make sure of this. Changing a film<br />

or solid bar fixture for a cone-plate measuring system is<br />

just as easy as integrating a new temperature device or<br />

connecting a CCD camera for sample visualization. You<br />

can use <strong>EC</strong>-<strong>Twist</strong> to analyze solutions, melts, solid bars,<br />

films, foils or reactive epoxy resins.<br />

High precision<br />

<strong>EC</strong>-<strong>Twist</strong> builds on technological innovation. The<br />

decoupling of sample pretension (stepper motor) and<br />

excitation (<strong>EC</strong> motor) considerably increases the system’s<br />

precision for solid bar measurements.<br />

<strong>EC</strong>-<strong>Twist</strong>’s peak performance is based on technological<br />

highlights such as the air-bearing-supported, synchronous<br />

<strong>EC</strong> motor, TruRate TM sample-adaptive motor control,<br />

TruStrain TM real-time position control or the patented<br />

normal force sensor integrated in the air bearing.<br />

Wide range<br />

Performed on highly diverse samples, DMTA analysis<br />

calls for full flexibility – ensured by a wealth of different<br />

measuring systems and temperature devices easily<br />

connected to <strong>EC</strong>-<strong>Twist</strong>. The instrument also performs<br />

DMTA tests in torsion or extension, as well as shear<br />

viscosity determination and extensional rheological tests.


Ready to Meet Your Requirements<br />

Convection temperature devices<br />

Four convection temperature devices are available,<br />

covering whichever temperature range you require.<br />

While the commonly used CTD 620 is optimized to<br />

cover almost 75 % of all applications, the patented<br />

CTD 180 is the only convection oven based on Peltier<br />

technology, enabling low-temperature measurements<br />

without the use of liquid nitrogen. The specialized<br />

CTD 600 and CTD 1000 temperature devices are<br />

mainly used for non-polymer samples such as glassor<br />

aluminum melts.<br />

Tribology System: friction and wear analysis of high-performance plastics<br />

CCD Camera Digital Eye<br />

Use the Digital Eye to record and display images or<br />

video sequences which are then optionally displayed<br />

directly in the diagram, assigned to the measuring<br />

points at which they were recorded.<br />

Measurement of additional properties<br />

Parallel-plate measuring system with thermo-melting polymer granules<br />

Due to <strong>EC</strong>-<strong>Twist</strong>’s Toolmaster TM function (automatic<br />

recognition and configuration of connected devices)<br />

and its high-precision flange, the instrument is easily<br />

and swiftly equipped with specialized devices like<br />

the Tribology System, for tribological analysis of<br />

high-performance plastics and lubricants, or optical<br />

and dielectrical systems for structure analysis, such<br />

as the SAXS or SALS system or the Dielectro-<br />

Rheological Device.


Evaporation Unit<br />

The Evaporation Unit (EVU) provides for constant<br />

temperature setting from -150 °C without temperature<br />

steps. Liquid nitrogen is continuously evaporated in<br />

an isolated reservoir and transferred to the measuring<br />

cell. This continuous evaporation without switch cycles<br />

facilitates temperature control at a level of precision that<br />

cannot be attained by means of valve control.<br />

Safety<br />

All outside surfaces of Anton Paar’s temperature devices are<br />

touch-proof up to their maximum temperature. The exhausts<br />

are designed with cooling mechanisms to ensure safe and<br />

comfortable use anytime and at any temperature.<br />

Shear<br />

rheology<br />

Extensional<br />

rheology<br />

DMTA<br />

torsion<br />

DMTA<br />

extension<br />

DMTA<br />

reaction<br />

Measuring system<br />

Polymer solutions<br />

Polymer melts<br />

Solid polymers<br />

Elastomers<br />

Reactive systems (epoxy resins)<br />

UV curing materials (Photo DMTA)<br />

Parallel plate<br />

Parallel plate, disposable<br />

Cone-plate, TruGap TM<br />

Solid rectangular fixture<br />

Universal extensional fixture<br />

Sentmanat extensional rheometer


DMTA in Torsion and Extension<br />

Relaxation steps during the softening process of<br />

a solid may become visible in the glass transition<br />

region. Various evaluation methods enable the<br />

quantification of a material’s transition from its solid<br />

to its rubber-elastic state. The melting point T m<br />

,<br />

the glass transition temperature T g<br />

, the secondary<br />

β- and γ-relaxations, the shear modulus at a given<br />

temperature – <strong>EC</strong>-<strong>Twist</strong> provides you with all these<br />

values at the push of a button.<br />

The following contains brief descriptions of the most<br />

essential <strong>EC</strong>-<strong>Twist</strong> test types for your consideration.<br />

DMTA in torsion<br />

One of <strong>EC</strong>-<strong>Twist</strong>’s main applications is the dynamic mechanical<br />

thermal analysis of thermoplastics, thermosets or elastomers in<br />

torsion. The measurement is performed in the destruction-free<br />

linear viscoelastic range using the Solid Rectangular Fixture<br />

SRF. The SRF enables determination of the shear moduli G’<br />

and G’’ and the loss or damping factor tan (δ) of solid bars.<br />

4 Oscillatory signal measured by the <strong>EC</strong> motor, without<br />

superposition of a pretension force<br />

4 Separate pretension and compensation of thermal<br />

expansion by the stepper motor<br />

4 Optimal measuring signal, especially in borderline<br />

areas – the extremely low temperatures below the glass<br />

temperature and the high temperatures close to the melting<br />

point<br />

4 Typical specimen dimensions (in mm): 40 x 10 x 1<br />

DMTA in extension<br />

The UXF Universal Extensional Fixture enables the<br />

measurement of the storage and loss modulus E’ and E’’<br />

as well as the damping factor tan (δ) of thin film sheets and<br />

fibers in the glass transition region. The system can be used<br />

to characterize multi-layer laminates as well as coating films.<br />

4 Modular design with various drums and QuickSnap fixture<br />

4 Measurement of E’, E’’ and tan (δ)<br />

4 Strain- or stress-controlled tests<br />

4 Typical specimen dimensions (in mm): 19 x 5 x 0.05<br />

4 For extensional melt rheology (in mm): 19 x 10 x 1<br />

Shrinkage and expansion measurement<br />

By applying a constant tensile stress or strain to a film or<br />

fiber, its shrinkage or expansion is measured depending on<br />

time and temperature. This method enables the practical<br />

evaluation of shrink films as well as investigations on film<br />

shrinkage by accidental heating (e.g. by solar radiation).<br />

Temperature sweep in torsion with glass transition<br />

Temperature sweep in extension with glass transition<br />

Film shrinkage and thermal expansion


DMTA on Reaction Kinetics<br />

The kinetics of reactive materials is investigated<br />

isothermally or by presetting a temperature ramp<br />

and a defined heating rate. The measurement is<br />

performed with disposable parallel-plate measuring<br />

systems (15 mm or smaller). A special evaluation<br />

macro in the application software evaluates the<br />

degree of cross-linkage based on the storage<br />

modulus and analyzes the sol-gel transition.<br />

One of the key features for precisely following<br />

reaction kinetics is the fast data acquisition based<br />

on <strong>EC</strong>-<strong>Twist</strong>’s TruStrain TM functionality. Typical<br />

sampling rates are 1 Hz as a quasi-standard or<br />

10 Hz for rapid curing processes.<br />

DMTA on reaction kinetics<br />

In the case of thermal cross-linkage, the liquid or<br />

two-component sample (resin and hardener) is heated and<br />

undergoes a viscosity reduction down to the softening point.<br />

From this point onwards, the cross-linkage reaction starts.<br />

Until its pot life the sample is still soft, but subsequently, i.e.<br />

at the sol-gel point, transforms into a gel-like state. Then it<br />

reaches its curing point and arrives at its final rigidity.<br />

a sample pressed into tablet shape. In a test like this, the<br />

sample passes through three phases. At first it is solid<br />

and unlinked. After the material’s fusion and melting at the<br />

melting point, its cross-linking starts, which leads to the<br />

material’s near-complete curing after it passes its curing<br />

point.<br />

Photo DMTA (UV curing)<br />

During the past few years, there has been rapidly growing<br />

interest in UV light curing of materials, a photochemical<br />

polymerization process. This technology has considerable<br />

practical and economic benefits. To measure materials’<br />

curing behavior, a powerful ultraviolet (UV) light source is<br />

connected to the measuring cell via a flexible light guide<br />

and controlled by the software.<br />

4 Optionally available with a built-in radiometer for<br />

calibration purposes<br />

4 Light source can be synchronized with rheological<br />

measuring profile using the application software<br />

Apart from “liquid-to-solid” curing procedures, <strong>EC</strong>-<strong>Twist</strong> also<br />

measures the cross-linkage reaction of an epoxy powder or<br />

Measuring modes offered by <strong>EC</strong>-<strong>Twist</strong><br />

Shear, continuous Shear, oscillatory Torsion, oscillatory<br />

Extension, continuous<br />

Extension, oscillatory<br />

Reaction kinetics of a curing resin<br />

Curing reaction of an epoxy resin with high<br />

concentration of filler<br />

UV cure and rate of cross-linkage


Melt Rheology<br />

<strong>EC</strong>-<strong>Twist</strong>’s range of measuring possibilities is<br />

not limited to solid samples. With cone-plate,<br />

TruGap TM or parallel-plate measuring systems<br />

with automatic gap control, polymers can also<br />

be measured as melts. Constant TruGap TM<br />

monitoring and control enables the use of<br />

cone-plate measuring systems to determine<br />

Mastercurves (Time-Temperature Superposition<br />

TTS) and measure temperature ramps – so<br />

when measuring polymer melts, you benefit<br />

from a constant shear rate in the measuring<br />

gap. Gap errors due to thermal expansion are<br />

no longer an issue.<br />

Shear rheology of melts<br />

A flow curve over a wide range of shear rates can also<br />

be generated from a Mastercurve using the Cox-Merz<br />

transformation. Regression models such as Carreau-<br />

Yasuda allow the calculation of important material<br />

parameters such as the relaxation time and power law<br />

index. The polymer's zero-shear viscosity is directly<br />

proportional to the molar mass.<br />

Transient time effects<br />

Stress relaxation tests provide information on<br />

time-dependent relaxation behavior after a defined<br />

deflection; creep tests on the other hand enable “longterm<br />

flow” measurements of melts, bars, films and fibers<br />

under a constant stress load.<br />

Time-Temperature Superposition<br />

The Time-Temperature Superposition enables<br />

the determination of Mastercurves at a<br />

given reference temperature. In this way, the<br />

frequency response and relaxation behavior<br />

can be determined over a range of more than<br />

10 decades.<br />

Extensional viscosity<br />

Extensional rheology is an excellent method<br />

for morphologically investigating elastomers<br />

or polymers. By measuring extensional<br />

viscosity under a preset constant strain rate,<br />

a distinction between linear and branched<br />

polymers is easily made.<br />

Further testing options<br />

In addition to the applications presented here,<br />

various further tests are available. <strong>EC</strong>-<strong>Twist</strong>’s<br />

application software offers diverse presets such<br />

as strain and amplitude, torsion, extension,<br />

compression (normal force), temperature<br />

and many more which can be combined in<br />

real time, enabling the exact simulation of<br />

application conditions.<br />

Flow curve converted from frequency<br />

sweep using Cox-Merz<br />

Mastercurve (Time-Temperature Superposition)<br />

Extensional viscosity of branched and<br />

linear polymer melts vs. time


Specifications<br />

Unit <strong>EC</strong>-<strong>Twist</strong> 302 <strong>EC</strong>-<strong>Twist</strong> 502<br />

Bearing - Air Air<br />

<strong>EC</strong> motor (brushless DC) with high-resolution optical encoder -<br />

Permanent torque (60 min), no signal drift -<br />

<strong>EC</strong> mode (controlled shear rate and shear stress)<br />

Maximum torque mNm 200 230<br />

Minimum torque, rotation nNm 10 10<br />

Minimum torque, oscillation nNm 2 2<br />

Torque resolution nNm 0.1 0.1<br />

Angular deflection, set value µrad 0.1 to ∞ 0.1 to ∞<br />

Angular deflection, resolution nrad 10 10<br />

Step rate, time constant ms 5 5<br />

Step strain, time constant ms 10 10<br />

Step time (rate, strain), 99 % of set value (all samples) ms 30 30<br />

Minimum angular velocity (1 rad/s 10 -9 10 -9<br />

Maximum angular velocity rad/s 314 314<br />

Minimum angular frequency (2 rad/s 10 -7 (3 10 -7 (3<br />

Maximum angular frequency rad/s 628 628<br />

Normal force range N 0.005 to 50 0.005 to 50<br />

Normal force resolution mN 0.5 0.5<br />

Dimensions mm 678 x 444 x 586 753 x 444 x 586<br />

Weight kg 42 47<br />

Toolmaster TM , measuring system -<br />

Toolmaster TM , measuring cell -<br />

QuickConnect for measuring systems, screwless -<br />

Electronic trimlock for the measuring system -<br />

Digital Eye, Software video option and camera -<br />

Virtually gradient-free (horizontal, vertical) temperature control -<br />

CoolPeltier TM , Peltier system with built-in cooling option requiring<br />

no additional accessories for counter-cooling<br />

°C -5 to 200 -5 to 200<br />

Peltier-based convection oven, does not require LN 2 for cooling °C -20 to 180 -20 to 180<br />

Actively Peltier-controlled hood, Peltier technology °C -40 to 200 -40 to 200<br />

Concentric-cylinder Peltier temperature control °C -30 to 200 -30 to 200<br />

Convection Temperature Devices (CTD) °C -150 to 1000 -150 to 1000<br />

Automatic gap control/setting, AGC/AGS -<br />

TruGap TM for in-place measurement and control of the gap -<br />

T-Ready TM -<br />

Direct strain, amplitude controller -<br />

Direct stress, amplitude controller -<br />

TruRate TM -<br />

TruStrain TM -<br />

Normal force and velocity profiles, tack, squeeze -<br />

Raw data (LAOS, waveform, ...) -<br />

1) Depending on measuring point duration and sampling time, practically any value is achieved<br />

2) Set frequencies below 10 -4 rad/s are of no practical relevance due to the measuring point<br />

duration > 1 day<br />

3) Theoretical value (duration per cycle = 2 years)<br />

Legend:<br />

optional


Photos: Croce & Wir<br />

Anton Paar ® GmbH<br />

Anton-Paar-Str. 20<br />

A-8054 Graz<br />

Austria - Europe<br />

Tel: +43 (0)316 257-0<br />

Fax: +43 (0)316 257-257<br />

E-mail: info@anton-paar.com<br />

Web: www.anton-paar.com<br />

<strong>Instruments</strong> for:<br />

Density & concentration<br />

measurement<br />

Rheometry<br />

Viscometry<br />

Sample preparation<br />

Microwave synthesis<br />

Colloid science<br />

X-ray structure analysis<br />

Refractometry<br />

Polarimetry<br />

High-precision temperature<br />

measurement<br />

Specifications<br />

subject to change<br />

without notice<br />

02/13 C92IP008EN-F

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