Broadband Turnkey System Concept 80

Novocontrol Technologies

Novocontrol Technologies GmbH & Co. KG

Top-class impedance analyzers with test interfaces for various applications Reliable sample environment for various temperature ranges and pressure variation Turnkey Dielectric and Impedance Spectrometers Software for instrument control, automation, and data analysis Sample cells for a large variety of applications

Impedance Measurement Requirements for Dielectric Measurements

• Broad frequency range • Wide impedance range • Small loss factors tan(  ) =  ’’ /  ’ = -Z s ’ / Z s ’’ Sample is in first order approximation a capacitor Capacitive impedance Z = j / (  C) Relaxation usually adds small changes in Z DC conductivity adds parallel resistance

Concept 80

(Table not included)

Alpha-A modular measurement system

Alpha-A Impedance analyzer system highlights

• Broad frequency range 3 µHz .. 40 MHz (> 13 decades) • Ultra wide impedance range 10 -4 from conductors to best isolators .. 10 14 Ω (18 decades) covers range in a single instrument set-up • Ultra wide capacity range 10 -15 .. 1 F allows broadband measurement of smallest capacities down to 1 fF.

• High phase accuracy (2 .

10 -3 ° ) and loss factor tan(δ) absolute accuracy (3 .

10 -5 ) for low loss dielectric materials and isolators broadband characterization. • Supports non-linear Dielectric, Conductivity and Impedance Spectroscopy or gain phase measurements in combination with all test interfaces.

Measurement examples Alpha total impedance range Typical results covering 18 orders of magnitude dynamics Short terminals Polyethylene 100 GOhm resistor 0.1 Ohm resistor 15 kOhm resistor 1 TOhm resistor Open terminals 100 Ohm resistor 15 10  10-3 10-2 10-1 100 101 102 103 Frequency [Hz] 104 105 -3 10  106 107 108

Alpha-A Impedance analyzer system highlights

• High speed measurements for online monitoring of time-dependent processes in the 5 ms range • Automatic self calibration and diagnosis by user compensates long term internal drift and verifies functionality. • Precision digital frequency response analyzer up to 40 MHz for two channel gain phase measurements with 0.001

° phase - and 10 -5 in amplitude resolution included. Operates like a broadband lock-in amplifier with two channels, extended accuracy and frequency range. • Optional control WinDETA software for turnkey calibration, operation, data evaluation, 2- and 3- dimensional graphical representation including non linear spectroscopy.

E4991A RF Material Analyzer

Frequency range: Impedance range: Accuracy: Capacity range : tan(  ) range: tan(  ) accuracy: Phase angle range: Accuracy: 1 MHz .. 3 GHz 100 m  .. 100 k  0.3% of measured value (best) 100 fF .. 100 nF 3 m .. 3 k 3 m (best) 0 .. 360 degrees Dc bias voltage range: Accuracy User calibrations Sample cells: 0.2 ° (best)  40 V; 46 mV Load, short, open, low loss capacitor sample cell short and open Two electrode RF reflection cell for temperatures from -160 .. 400 ° C

Concept 80 System Constituents:

• Two impedance analyzers with sample cells: a) Alpha-A (3 µHz to 20 MHz) with Alpha Active Sample Cell ZGS b) E4991A RF Materials Analyzer (1 MHz to 3 GHz) with RF Dielectric sample cell BDS 2200 (14 mm version) or BDS 2100 (7 mm version) • RF mounting stage • Quatro Cryosystem: -160 ° C to 400 ° C • Full software package WinDETA+WinPLOT+WinTEMP+WinFIT • Data Acquisition Unit (computer with GPIB interface, 22” LCD monitor, printer)

Alpha-A Active Sample cell ZGS (3 µHz .. 20 MHz; 40 MHz with Alpha-AT)

Sample cell with integrated test interface (current-to-voltage converter/amplifier) and optimized frequency performance. High-performance dielectric, conductivity or impedance measurements from 3 µHz up to 40 MHz (with Alpha-AT only).

Rigid air-line connection from electronics to electrodes suppresses performance limiting cable effects at high and low frequencies due to cable inductance and piezo-induced charges caused by mechanical noise.

Temperature range: -160 ° C .. 400 ° C

RF sample cell and extension line (1 MHz to 3 GHz)

BDS 2200 RF dielectric sample cell

RF extension line (1 MHz to 3 GHz)

High-temperature stable, low-loss precision line with two APC-7 connectors and Pt100 temperature sensor. Mounted between the impedance input of the RF Analyzer and the RF sample cell for thermal isolation. The combination of sample cell and extension line can be operated in the temperature range from -160 ° C to 400 ° C.

Quatro Cryosystem: High Precision Turnkey Temperature Control

4 Range: -160 ° C to 400 ° C Ramps: 0.01

° C/min to 20 ° C/min Stability: 0.01

° C Overshooting after set point step: typically < 0.2

° C Stabilization times typically < 8 minutes (for 0.1

° Cstability) low nitrogen consumption due to automatic pressure-temperature adaptation automatic adaptation of controller parameters vacuum-isolated cryostat and nitrogen lines

Quatro Cryosystem

A heating element builds up a specified pressure in the liquid nitrogen dewar in order to create a highly constant nitrogen gas flow. Pressure and temperature in the dewar are measured by two channels of the Quatro controller. Heated by a gas jet, the nitrogen gas flows directly through the sample cell which is mounted into the cryostat. The gas and sample temperatures are measured by the two remaining channels of the QUATRO controller. The four channel arrangement allows stable, fast and safe system operation in combination with low liquid nitrogen consumption (economical mode).

The cryostat is vacuum isolated by a two- stage rotary vane vacuum pump, providing thermal isolation by low vacuum (< 10 µbar). 4

Quatro Cryosystem

WinDETA Control and Data Visualisation Software

WinDETA Control and Data Visualisation Software

Control and evaluation software for dielectric and impedance spectroscopy Uniform user interface for several dielectric/ impedance analyzers and temperature controllers nearly independent of hardware Flexible experiment set-up: control of frequency, temperature (WinTEMP option), ac voltage, dc bias, and time in any multi dimensional arrangement Evaluates over 30 different electric quantities like e.g. permittivity, conductivity, inductance, etc. from measured impedance Graphical online display of measured data in two or three dimensional diagrams (WinPLOT option), temperature curve and system status Automatic calibration of hardware devices and sample cells Ex- and imports data in several flexible ASCII formats Curve fitting software WinFIT for equivalent circuit modelling, data transformations like WLF, Havriliak-Negami, and time domain conversion Supports Win2000, XP, Vista, Win7.

WinFIT Curve Fitting Software

Non linear curve fitting in the frequency domain Special relaxation fit functions like, e.g, Havriliak Negami, Cole Cole, Cole Davidson, Debye etc.

Automatical evaluation of a series of spectra taken at various temperatures Separation of relaxation and conductivity contributions Automatic creation of master plot representations Non linear curve fitting in the temperature domain including Vogel - Fulcher and Williams Landel Ferry (WLF) fit functions Relaxation time and maximum relaxation frequency determination Arrhenius activation plot related to activation energy and glass temperature Dielectric data conversion (Fourier Transform) from frequency to time domain Complete dielectric time domain representation including relaxation time distribution, relaxation function, step response function, peak answer function, time dependent dielectric constant and conductivity Shifts, deletes and inserts data points with a single mouse click Connects data curves being measured in different frequency ranges with different analyzers