FDSC measurements were performed using a Mettler-Toledo Flash DSC 2+ operated with UFS 1 sensors, described in [7 (link)]. The sample support temperature in the calorimeter was set to 29°C and the sensor was purged with high-purity N2 at a flow rate of 30 ml min−1. To improve the thermal contact between sample and sensor the active zone of the sample side of the sensor was wetted with a very small amount of silicon oil (AK 500.000 Wacker). To create a thin silicon oil film, the sensor was heated five times at 2000 K s−1 to 250°C without sample. The sample was placed on the active zone of the sensor using a hair with a fine tip. Unless otherwise noted, the hydrous ACMC was dried in an external furnace at 250°C for 2 h. Before the heating measurement the sample was additionally dried at 250°C for 60 s or 600 s on the FDSC sensor. The sample mass was between 60 and 130 ng. The sample mass was estimated from the crystallization enthalpy of Δhc = 156.6 J g−1 measured with conventional DSC. This method is described in [8 (link)]. Samples were measured between 30°C and 520°C with heating rates between 2000 and 6000 K s−1.
Flash dsc 2
Manufactured by Mettler Toledo
Sourced in United States, Switzerland
The Flash DSC 2+ is a differential scanning calorimetry (DSC) instrument designed for thermal analysis of materials. It provides fast and precise measurements of thermal transitions, such as melting, crystallization, and glass transitions, in a wide range of sample types.
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5 protocols using flash dsc 2
1
High-Speed Calorimetry of Hydrous ACMC
2
Flash DSC Measurements of Melt-Spun Ribbons
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FDSC measurements were performed using a prototype of a Mettler-Toledo Flash DSC 2+. This instrument is an advanced version based upon Flash DSC technology, with a sealed measurement cell for reduced oxygen content. The Flash DSC 2+ can be operated with a UFS 1 sensor70 or a new UFH 1 sensor (see insert to Supplementary Fig. 4 ), which can be operated to about 1000 °C. The active area of the latter sensor is reduced by 1/3 and the membrane thickness is reduced compared to the UFS 1 sensor. The diameter of the active zone is approximately 100 μm, which increases the applicable cooling rate to approximately 40,000 K s−1.
The sample support temperature of the FDSC was set to −30 °C using a Huber intracooler TC45, and the furnace was purged with nitrogen at a flow rate of 60 ml min−1. The melt-spun ribbons were cut under a stereomicroscope into small pieces with a surface of approximately 104 μm2. Their mass was estimated using the melting enthalpy of ΔHm = 40.4 J g−1 (ref. 14 (link)) to be on the order of 1 μg, for which no size-dependent nucleation and crystallization effects are expected45 (link). Details regarding temperature calibration, thermal lag (Supplementary Fig.4 ), and enthalpy resolution (Supplementary Fig. 5 ) are given in the Supplementary Methods section.
The sample support temperature of the FDSC was set to −30 °C using a Huber intracooler TC45, and the furnace was purged with nitrogen at a flow rate of 60 ml min−1. The melt-spun ribbons were cut under a stereomicroscope into small pieces with a surface of approximately 104 μm2. Their mass was estimated using the melting enthalpy of ΔHm = 40.4 J g−1 (ref. 14 (link)) to be on the order of 1 μg, for which no size-dependent nucleation and crystallization effects are expected45 (link). Details regarding temperature calibration, thermal lag (Supplementary Fig.
3
High-Cooling-Rate Crystallization of PP
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A semi-crystalline polypropylene (Talc filled PP, SABIC, Riyadh, Saudi Arabia) was used in the experiments. The melt flow rate (MFR) of the PP at 230 °C and 2.16 kg was 18 g/10 min, and the density was 1239 kg/m3 at room temperature. The material was used as received and no purification was conducted.
The Flash DSC 2+ by Mettler-Toledo, Columbus, OH, USA was employed. This instrument could reach ultra-high cooling rates of up to 40,000 K/s, which achieved the exploration of high cooling rate’s effect on crystallization behavior.
A high-pressure capillary rheometer (Rheograph 25, GÖTTFERT Werkstoff-Prüfmaschinen GmbH, Buchen, Germany) was used to measure the PVT diagrams of the PP. This instrument could realize isothermal or isobaric PVT measurements according to ISO 17744. The long diameter ratio of capillary tube was 25:2 and the sample mass weight of PVT diagram test was 3 kg.
The Flash DSC 2+ by Mettler-Toledo, Columbus, OH, USA was employed. This instrument could reach ultra-high cooling rates of up to 40,000 K/s, which achieved the exploration of high cooling rate’s effect on crystallization behavior.
A high-pressure capillary rheometer (Rheograph 25, GÖTTFERT Werkstoff-Prüfmaschinen GmbH, Buchen, Germany) was used to measure the PVT diagrams of the PP. This instrument could realize isothermal or isobaric PVT measurements according to ISO 17744. The long diameter ratio of capillary tube was 25:2 and the sample mass weight of PVT diagram test was 3 kg.
4
Calorimetry Analysis of Metallic Glasses
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The present calorimetry was performed using a combination of Flash DSC (Mettler Toledo Flash DSC 2+) and conventional DSC (Mettler Toledo DSC 3). The heat flow curves of MGs at a relatively low heating rate (0.083–1.33 K/s) is obtained by continuous heating on a conventional DSC using a refrigerated cooling system with a N2-gas DSC cell purge under a 50 ml/min nitrogen gas flow. The sample masses were 8–15 mg. In order to ensure the reliability of the measurement, each crystallized sample was heated again to obtain a baseline. The conventional DSC was calibrated by using pure In and Zn standard. The heat flow curves of MGs at higher heating rates were obtained by continuous heating on a Flash DSC under 80 ml/min argon gas flow. The twin-type chip sensor based on MEMS technology is made of a sample and a reference. The FSC chip sensors were preconditioned and calibrated following the manufacturer recommendation. The FSC samples were prepared by cutting the melt-spun ribbons into small pieces under a stereomicroscope and then transferred using an electrostatic manipulator hair onto a temperature-corrected MultiSTAR UFS1 sensor or UFH sensor. Samples were placed on the sensitive area of a MEMS chip sensor for a range of heating rates from 3 to 20 000 K/s.
5
Characterizing Polymer Crystallization Kinetics
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A chip-calorimeter instrument, Flash DSC 2+ (made by Mettler-Toledo, Zurich, Switzerland) equipped with a Huber TC-100 intracooler was employed. The maximum heating rate and the maximum cooling rate can reach 50,000 K/s and 40,000 K/s, respectively. FSC has been widely used due to its advantages such as ultra-fast heating and cooling scanning rate, outstanding temperature control ability and accurate time resolution. It can inhibit the crystallization nucleation of the polymer sample during the process of heating and cooling, and avoid the influence on the subsequent crystallization kinetics test. The results enable us to obtain the initial information about the structure of the aggregated states inside the polymer crystals, to produce a new understanding of the annealing and melting behavior of polymer crystals, and to deepen understanding of the nucleation mechanism of polymer crystals. Schick, C. et al. [22 (link),23 (link),24 (link)] have suggested that heterogeneous nucleation can be effectively bypassed and homogeneous nucleation can be observed in the bulk at low temperatures, using the fast cooling rate provided by FSC. Based on the proposal of Schick, C. et al., this study assumes that this hypothesis is valid; therefore, the crystallization kinetics of diblock copolymer can be deduced.
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