Broadband Dielectric Spectroscopy (BDS) was carried out in the frequency range from 1 Â 10 À2 Hz to 1 Â 10 7 Hz with a Novocontrol Alpha-N High Resolution Dielectric Analyzer, where temperature was controlled utilizing a Novocontrol Quatro cryosystem. The custom made sample cell consisted of two polished stainless steel electrodes spaced by a quartz glass ring, providing a sample thickness of approximately 400 mm.
Quatro cryosystem
Manufactured by Novocontrol
Sourced in Germany
The Quatro cryosystem is a laboratory equipment designed for cryogenic temperature control. It provides precise temperature regulation for various applications that require low-temperature environments.
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Lab products found in correlation
Broadband dielectric spectrometer, by Novocontrol (2 mentions)
Bds 1200 cell, by Novocontrol (2 mentions)
Alpha frequency response analyzer, by Novocontrol (1 mentions)
Alpha an, by Novocontrol (1 mentions)
Concept 80, by Novocontrol (1 mentions)
Thermomixer comfort, by Eppendorf (1 mentions)
Alpha analyzer, by Novocontrol (1 mentions)
Em scd050, by Leica (1 mentions)
Zgs interface, by Novocontrol (1 mentions)
Windeta software, by Novocontrol (1 mentions)
Alpha a, by Novocontrol (1 mentions)
Concept 80 system, by Novocontrol (1 mentions)
Alpha n analyzer, by Novocontrol (1 mentions)
High resolution alpha analyzer, by Novocontrol (1 mentions)
14 protocols using quatro cryosystem
1
Broadband Dielectric Spectroscopy of Polymer Samples
2
Dielectric Characterization of Samples
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Molecular dynamic characterization of the samples was determined by means of a Novocontrol Broadband Dielectric Spectrometer (Hundsagen, Germany) which involved an Alpha analyzer. The temperature varied from 163 to 313 K in steps of 5 K using the temperature control system Novocontrol Quatro cryosystem, with a precision of ±0.1 K during each sweep in frequency. At each temperature, a frequency sweep from 5 × 10−2 to 3 × 106 Hz was measured. The samples were dried at 313 K before each measurement, in a vacuum oven until a constant weight was reached to avoid interference of water in the dielectric response. In order to avoid moisture uptake, during all the DRS experiments the samples were under a steady flow of inert N2 atmosphere. This temperature range was chosen because it covers the glass transition temperature and avoids other transitions that can experience the matrix with increasing temperature. Molded disc-shaped samples of approximately 10 mm diameter and 0.12 mm thickness were mounted in the dielectric cell between two parallel cylindrical gold-plated electrodes. Accurate measure of sample thickness was determined with a micrometer screw. The dielectric permittivity and the dielectric loss have been recorded for each sample in dependence on temperature and frequency. The experimental uncertainty was less than 5% in all cases.
3
Dielectric Properties of Ionic Liquids
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Dielectric properties were determined using the impedance analyzer (Novocontrol Alpha frequency response analyzer) (Novocontrol Technologies GmbH & Co. KG, Montabaur, Germany) at a frequency range from 0.1 to 10 MHz at an applied voltage of 3 V. A Quatro Cryosystem from the same manufacturer was used to control the temperature within a cryostat with an accuracy better than of ±0.1 K. For dielectric measurements a temperature figure was applied form initial RT (25 °C) down to −85 °C followed by a stepwise increase with 10 K increments to 95°. The chosen temperature was held constant for 5 min for all studied samples before frequency scan. All IL films were equipped with circular frames of 20 mm diameter. The so-defined freestanding area was covered with gold powder and finally covered with the metal discs to ensure a proper electric contact to the measurement system.
4
Broadband Dielectric Spectroscopy of Materials
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The dielectric properties (ε′, ε″, and σ′) were measured using a broadband dielectric spectrometer (Novocontrol GmbH) with an active sample cell based on a high-resolution impedance analyzer (Novocontrol Alpha) at frequencies between 10−1 and 106 Hz. The sample was placed in a stainless-steel liquid cell (diameter: 20.00 mm and electrode spacing: 1.560 mm) to realize a parallel plate geometry. For the upper-frequency range from 106 to 109 Hz, a Hewlett Packard HP 4291B network analyzer, in combination with a calibrated coaxial line and a Novocontrol RF cell (parallel plates of 5 mm diameter with 100 μm electrode separation), was used. The sample temperature was controlled using a Novocontrol Quatro cryosystem, allowing for temperature control with ±0.01 K accuracy via dry N2 gas flow derived from liquid nitrogen. To ensure complete filling of the cell, a fresh sample was first heated from room temperature to 393 K, followed by stabilization at this temperature for 15 min to eliminate any possible thermal history. The sample was then cooled to 193.15 K at a 10 K min−1 cooling rate. Thereafter, the sample was heated to 393 K and cooled to 193 K with 2 K temperature intervals (heating/cooling rate: 10 K min−1) for the dielectric spectroscopy measurements. More details can be found in references.39 (link),40 (link),41 (link)
5
Broadband Dielectric Characterization of Sintered Pellets
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Sintered pellets with sputtered or evaporated Au electrodes were used to measure complex conductivities at various temperatures and from 0.1 Hz up to the GHz range with a Novocontrol Concept 80 setup. The setup consists of a broadband analyser (Alpha-AN, Novocontrol), which is connected to a BDS 1200 cell in combination with an active ZGS cell interface (Novocontrol) allowing 2-electrode dielectric measurements. The temperature is automatically controlled by means of a QUATRO cryo-system (Novocontrol) making use of a heating element which builds up a specified pressure in a liquid nitrogen Dewar vessel to create a highly constant N2 gas flow. After being heated by a gas jet, the evaporated N2 flows directly through the sample cell that is mounted in a cryostat. With this setup, temperatures can be set with an accuracy of ±0.01 °C. To reach up to 3 GHz we used an Agilent E4991 A high-frequency analyser connected to a high frequency cell designed by Novocontrol.
6
Dielectric Characterization of Materials
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Dielectric measurements were carried out on an Alpha-S impedance analyzer in the range from 0.1 Hz to 1 MHz. Samples around 0.1 mm thick were dried under vacuum and placed in a 10 mm diameter parallel plate capacitor mounted on a temperature-controlled cryostat (BDS 1100) and exposed to a heated gas stream evaporated from a liquid nitrogen Dewar. The temperature control was assured by Quatro Cryosystem from Novocontrol GmbH (Montabaur, Germany). Isothermal scans were performed from 0 to 180 °C (thermal stability: 0.5 °C) in 5 °C steps. The complex permittivity ε* = ε′ + iε″ and complex conductivity σ* = σ′ + i σ″ were determined as a function of frequency.
7
Broadband Dielectric Characterization
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The complex permittivity ε* = ε′ − iε′′ and the real part of the conductivity σ′ at frequencies 1 Hz ≤ ν ≤ 1 MHz were determined using a frequency-response analyzer (Novocontrol alpha-Analyzer) and at 1 MHz ≤ ν ≤ 3 GHz employing a coaxial reflection impedance analyzer (Agilent E4991A or Keysight E4991B). All samples were measured in steel-plate capacitors. For sample cooling between 170 and 370 K, a Novocontrol Quatro Cryosystem was utilized. For BPY BF4, the spectrum was additionally expanded to 40 GHz using a coaxial reflection measurement with an open-ended sensor (Agilent E8363B PNA Series Network Analyzer with 85070E Dielecric Probe Kit). Sample heating from 300 to 370 K was done by an Eppendorf Thermomixer Comfort with an additional external temperature sensor.
8
Ionic Conductivity of La-Ba-F Perovskite
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The ionic conductivity of the as-prepared La Ba F was checked by solid-state impedance spectroscopy. Hence, the powder samples were pressed to cylindrical pellets with a diameter of 5 mm and a thickness of ca. 1 mm; we used a press of P. O. Weber and applied a uniaxial force of 0.5 t. Ion blocking Pt electrodes with a thickness of 100 nm were applied on both sides of the pellet by sputtering (Leica sputter device (EM SCD050, Leica Microsystems, Wetzlar, DE)). Impedance data were recorded with a Novocontrol Concept 80 broadband spectrometer in combination with an active BDS 1200 cell [28 ] and a ZGS interface (Novocontrol). Impedance data were recorded over a frequency range from 10 Hz to 10 Hz at temperatures ranging from 20 to 200 C. A QUATRO cryo-system (Novocontrol, Montabaur, DE) controlled the temperature of all measurements, which were carried out under a constant flow of dry, freshly evaporated N gas.
9
Broadband Dielectric Spectroscopy of Felt Samples
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DRS measurements in a frequency range from 5·10−2 to 3·106 Hz were performed using a Novocontrol Broadband Dielectric Spectrometer (Hundsagen, Germany) consisting of an SR 830 lock-in amplifier with an Alpha dielectric interface. The measurements were performed in an N2 atmosphere from 20 °C to 160 °C and to 100 °C, in steps of 5 °C, for the pristine and coated felt samples, respectively. Temperature control was carried out by means of a Novocontrol Quatro cryosystem, with an accuracy of ±0.1 °C during each sweep in frequency. Disc-shaped samples, of about 0.1 mm thickness and a 20 mm diameter, were used. The experimental uncertainty was better than 5% in all cases.
10
Dielectric Impedance Spectroscopy of Materials
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Complex impedance spectra of the samples were measured in a frequency range between 100 Hz and 10 MHz by using a Novocontrol a-S high resolution dielectric analyzer equipped with a Quatro cryosystem and controlled by WINDETA software (Novocontrol, Montabaur, Germany). Samples were filled into a coin-shaped sample chamber and sandwiched between two stainless steel electrodes. The temperature was controlled by a preheated flow of dry nitrogen. Impedance measurements were performed at 295 K. The real part of the conductivity s 0 was plotted against the frequency and the conductivity for the direct current case s dc was extrapolated from the conductivity plateau value at low frequencies.
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