EC-Twist - MEP Instruments

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EC-Twist - MEP Instruments

EC-Twist

Dynamic Mechanical Analyzer

::: Intelligence in Rheometry


A New Twist on DMTA

EC-Twist is a Dynamic Mechanical Analyzer

for DMTA analysis on solids as well as liquids.

The modular system performs measurements

in torsion and extension and is the first DMTA

solution that can also be used for shearrheological

experiments – at unprecedented

precision.

Easy adaptation

EC-Twist builds on your applications. Whatever your DMTA

requirements are and will be in the future – EC-Twist is

efficiently and comfortably adapted to meet your needs.

The flexible application software and patented features

such as Toolmaster TM , an automatic tool recognition and

configuration system, make sure of this. Changing a film

or solid bar fixture for a cone-plate measuring system is

just as easy as integrating a new temperature device or

connecting a CCD camera for sample visualization. You

can use EC-Twist to analyze solutions, melts, solid bars,

films, foils or reactive epoxy resins.

High precision

EC-Twist builds on technological innovation. The

decoupling of sample pretension (stepper motor) and

excitation (EC motor) considerably increases the system’s

precision for solid bar measurements.

EC-Twist’s peak performance is based on technological

highlights such as the air-bearing-supported, synchronous

EC motor, TruRate TM sample-adaptive motor control,

TruStrain TM real-time position control or the patented

normal force sensor integrated in the air bearing.

Wide range

Performed on highly diverse samples, DMTA analysis

calls for full flexibility – ensured by a wealth of different

measuring systems and temperature devices easily

connected to EC-Twist. The instrument also performs

DMTA tests in torsion or extension, as well as shear

viscosity determination and extensional rheological tests.


Ready to Meet Your Requirements

Convection temperature devices

Four convection temperature devices are available,

covering whichever temperature range you require.

While the commonly used CTD 620 is optimized to

cover almost 75 % of all applications, the patented

CTD 180 is the only convection oven based on Peltier

technology, enabling low-temperature measurements

without the use of liquid nitrogen. The specialized

CTD 600 and CTD 1000 temperature devices are

mainly used for non-polymer samples such as glassor

aluminum melts.

Tribology System: friction and wear analysis of high-performance plastics

CCD Camera Digital Eye

Use the Digital Eye to record and display images or

video sequences which are then optionally displayed

directly in the diagram, assigned to the measuring

points at which they were recorded.

Measurement of additional properties

Parallel-plate measuring system with thermo-melting polymer granules

Due to EC-Twist’s Toolmaster TM function (automatic

recognition and configuration of connected devices)

and its high-precision flange, the instrument is easily

and swiftly equipped with specialized devices like

the Tribology System, for tribological analysis of

high-performance plastics and lubricants, or optical

and dielectrical systems for structure analysis, such

as the SAXS or SALS system or the Dielectro-

Rheological Device.


Evaporation Unit

The Evaporation Unit (EVU) provides for constant

temperature setting from -150 °C without temperature

steps. Liquid nitrogen is continuously evaporated in

an isolated reservoir and transferred to the measuring

cell. This continuous evaporation without switch cycles

facilitates temperature control at a level of precision that

cannot be attained by means of valve control.

Safety

All outside surfaces of Anton Paar’s temperature devices are

touch-proof up to their maximum temperature. The exhausts

are designed with cooling mechanisms to ensure safe and

comfortable use anytime and at any temperature.

Shear

rheology

Extensional

rheology

DMTA

torsion

DMTA

extension

DMTA

reaction

Measuring system

Polymer solutions

Polymer melts

Solid polymers

Elastomers

Reactive systems (epoxy resins)

UV curing materials (Photo DMTA)

Parallel plate

Parallel plate, disposable

Cone-plate, TruGap TM

Solid rectangular fixture

Universal extensional fixture

Sentmanat extensional rheometer


DMTA in Torsion and Extension

Relaxation steps during the softening process of

a solid may become visible in the glass transition

region. Various evaluation methods enable the

quantification of a material’s transition from its solid

to its rubber-elastic state. The melting point T m

,

the glass transition temperature T g

, the secondary

β- and γ-relaxations, the shear modulus at a given

temperature – EC-Twist provides you with all these

values at the push of a button.

The following contains brief descriptions of the most

essential EC-Twist test types for your consideration.

DMTA in torsion

One of EC-Twist’s main applications is the dynamic mechanical

thermal analysis of thermoplastics, thermosets or elastomers in

torsion. The measurement is performed in the destruction-free

linear viscoelastic range using the Solid Rectangular Fixture

SRF. The SRF enables determination of the shear moduli G’

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

4 Oscillatory signal measured by the EC motor, without

superposition of a pretension force

4 Separate pretension and compensation of thermal

expansion by the stepper motor

4 Optimal measuring signal, especially in borderline

areas – the extremely low temperatures below the glass

temperature and the high temperatures close to the melting

point

4 Typical specimen dimensions (in mm): 40 x 10 x 1

DMTA in extension

The UXF Universal Extensional Fixture enables the

measurement of the storage and loss modulus E’ and E’’

as well as the damping factor tan (δ) of thin film sheets and

fibers in the glass transition region. The system can be used

to characterize multi-layer laminates as well as coating films.

4 Modular design with various drums and QuickSnap fixture

4 Measurement of E’, E’’ and tan (δ)

4 Strain- or stress-controlled tests

4 Typical specimen dimensions (in mm): 19 x 5 x 0.05

4 For extensional melt rheology (in mm): 19 x 10 x 1

Shrinkage and expansion measurement

By applying a constant tensile stress or strain to a film or

fiber, its shrinkage or expansion is measured depending on

time and temperature. This method enables the practical

evaluation of shrink films as well as investigations on film

shrinkage by accidental heating (e.g. by solar radiation).

Temperature sweep in torsion with glass transition

Temperature sweep in extension with glass transition

Film shrinkage and thermal expansion


DMTA on Reaction Kinetics

The kinetics of reactive materials is investigated

isothermally or by presetting a temperature ramp

and a defined heating rate. The measurement is

performed with disposable parallel-plate measuring

systems (15 mm or smaller). A special evaluation

macro in the application software evaluates the

degree of cross-linkage based on the storage

modulus and analyzes the sol-gel transition.

One of the key features for precisely following

reaction kinetics is the fast data acquisition based

on EC-Twist’s TruStrain TM functionality. Typical

sampling rates are 1 Hz as a quasi-standard or

10 Hz for rapid curing processes.

DMTA on reaction kinetics

In the case of thermal cross-linkage, the liquid or

two-component sample (resin and hardener) is heated and

undergoes a viscosity reduction down to the softening point.

From this point onwards, the cross-linkage reaction starts.

Until its pot life the sample is still soft, but subsequently, i.e.

at the sol-gel point, transforms into a gel-like state. Then it

reaches its curing point and arrives at its final rigidity.

a sample pressed into tablet shape. In a test like this, the

sample passes through three phases. At first it is solid

and unlinked. After the material’s fusion and melting at the

melting point, its cross-linking starts, which leads to the

material’s near-complete curing after it passes its curing

point.

Photo DMTA (UV curing)

During the past few years, there has been rapidly growing

interest in UV light curing of materials, a photochemical

polymerization process. This technology has considerable

practical and economic benefits. To measure materials’

curing behavior, a powerful ultraviolet (UV) light source is

connected to the measuring cell via a flexible light guide

and controlled by the software.

4 Optionally available with a built-in radiometer for

calibration purposes

4 Light source can be synchronized with rheological

measuring profile using the application software

Apart from “liquid-to-solid” curing procedures, EC-Twist also

measures the cross-linkage reaction of an epoxy powder or

Measuring modes offered by EC-Twist

Shear, continuous Shear, oscillatory Torsion, oscillatory

Extension, continuous

Extension, oscillatory

Reaction kinetics of a curing resin

Curing reaction of an epoxy resin with high

concentration of filler

UV cure and rate of cross-linkage


Melt Rheology

EC-Twist’s range of measuring possibilities is

not limited to solid samples. With cone-plate,

TruGap TM or parallel-plate measuring systems

with automatic gap control, polymers can also

be measured as melts. Constant TruGap TM

monitoring and control enables the use of

cone-plate measuring systems to determine

Mastercurves (Time-Temperature Superposition

TTS) and measure temperature ramps – so

when measuring polymer melts, you benefit

from a constant shear rate in the measuring

gap. Gap errors due to thermal expansion are

no longer an issue.

Shear rheology of melts

A flow curve over a wide range of shear rates can also

be generated from a Mastercurve using the Cox-Merz

transformation. Regression models such as Carreau-

Yasuda allow the calculation of important material

parameters such as the relaxation time and power law

index. The polymer's zero-shear viscosity is directly

proportional to the molar mass.

Transient time effects

Stress relaxation tests provide information on

time-dependent relaxation behavior after a defined

deflection; creep tests on the other hand enable “longterm

flow” measurements of melts, bars, films and fibers

under a constant stress load.

Time-Temperature Superposition

The Time-Temperature Superposition enables

the determination of Mastercurves at a

given reference temperature. In this way, the

frequency response and relaxation behavior

can be determined over a range of more than

10 decades.

Extensional viscosity

Extensional rheology is an excellent method

for morphologically investigating elastomers

or polymers. By measuring extensional

viscosity under a preset constant strain rate,

a distinction between linear and branched

polymers is easily made.

Further testing options

In addition to the applications presented here,

various further tests are available. EC-Twist’s

application software offers diverse presets such

as strain and amplitude, torsion, extension,

compression (normal force), temperature

and many more which can be combined in

real time, enabling the exact simulation of

application conditions.

Flow curve converted from frequency

sweep using Cox-Merz

Mastercurve (Time-Temperature Superposition)

Extensional viscosity of branched and

linear polymer melts vs. time


Specifications

Unit EC-Twist 302 EC-Twist 502

Bearing - Air Air

EC motor (brushless DC) with high-resolution optical encoder -

Permanent torque (60 min), no signal drift -

EC mode (controlled shear rate and shear stress)

Maximum torque mNm 200 230

Minimum torque, rotation nNm 10 10

Minimum torque, oscillation nNm 2 2

Torque resolution nNm 0.1 0.1

Angular deflection, set value µrad 0.1 to ∞ 0.1 to ∞

Angular deflection, resolution nrad 10 10

Step rate, time constant ms 5 5

Step strain, time constant ms 10 10

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

Minimum angular velocity (1 rad/s 10 -9 10 -9

Maximum angular velocity rad/s 314 314

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

Maximum angular frequency rad/s 628 628

Normal force range N 0.005 to 50 0.005 to 50

Normal force resolution mN 0.5 0.5

Dimensions mm 678 x 444 x 586 753 x 444 x 586

Weight kg 42 47

Toolmaster TM , measuring system -

Toolmaster TM , measuring cell -

QuickConnect for measuring systems, screwless -

Electronic trimlock for the measuring system -

Digital Eye, Software video option and camera -

Virtually gradient-free (horizontal, vertical) temperature control -

CoolPeltier TM , Peltier system with built-in cooling option requiring

no additional accessories for counter-cooling

°C -5 to 200 -5 to 200

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

Actively Peltier-controlled hood, Peltier technology °C -40 to 200 -40 to 200

Concentric-cylinder Peltier temperature control °C -30 to 200 -30 to 200

Convection Temperature Devices (CTD) °C -150 to 1000 -150 to 1000

Automatic gap control/setting, AGC/AGS -

TruGap TM for in-place measurement and control of the gap -

T-Ready TM -

Direct strain, amplitude controller -

Direct stress, amplitude controller -

TruRate TM -

TruStrain TM -

Normal force and velocity profiles, tack, squeeze -

Raw data (LAOS, waveform, ...) -

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

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

duration > 1 day

3) Theoretical value (duration per cycle = 2 years)

Legend:

optional


Photos: Croce & Wir

Anton Paar ® GmbH

Anton-Paar-Str. 20

A-8054 Graz

Austria - Europe

Tel: +43 (0)316 257-0

Fax: +43 (0)316 257-257

E-mail: info@anton-paar.com

Web: www.anton-paar.com

Instruments for:

Density & concentration

measurement

Rheometry

Viscometry

Sample preparation

Microwave synthesis

Colloid science

X-ray structure analysis

Refractometry

Polarimetry

High-precision temperature

measurement

Specifications

subject to change

without notice

02/13 C92IP008EN-F

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