The surface functional groups of the microspheres were investigated by FTIR using a Nicolet 6700 spectrometer (Thermo Electron Co., USA). TGA was carried out using a STA 6000 (PerkinElmer, USA) under a nitrogen atmosphere at a flow rate of 50 mL min−1 and a heating rate of 20 °C min−1 from 40 °C to 800 °C. The morphology and elemental analysis of the microspheres were carried out by scanning electron microscopy (SEM) using a ZEISS EV0 MA15 SEM from Carl Zeiss Micro Image Co., Ltd. The non-isothermal DSC curing reaction of the Ba and Ba/PZPT mixture was monitored using a Q20 equipment (TA instruments) from 40 °C to 350 °C at different heating rates of 5, 10, 15, and 20 °C min−1. In situ FTIR spectroscopy was conducted using a frontier PerkinElmer FTIR spectrometer, and spectra were recorded every 18 s from 100 to 250 °C at a heating rate of 2.5 °C min−1. DMA was carried out using a Q800 analyzer (TA Instruments) from 40 to 300 °C at a heating rate of 5 °C per step and a frequency of 1 Hz in the air. In the three-point bending mode, samples with 40 × 10 × 3.2 mm3 dimension were used.
Q800 analyzer
Manufactured by TA Instruments
Sourced in United States
The Q800 analyzer is a thermal analysis instrument designed to measure the physical and chemical properties of materials. It is capable of performing dynamic mechanical analysis (DMA) and thermogravimetric analysis (TGA) measurements.
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6 protocols using q800 analyzer
1
Characterization of Barium Microspheres
2
Tensile and Dynamic Mechanical Analysis of Cellulose Nanofiber Composites
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The dried CNF films, neat epoxy films and composites were tested according to ASTM D 638-Type V specifications. Tensile tests were performed using an Instron machine (Model 3367, Instron, Norwood, MA, USA) equipped with a 2 kN load cell, in which a gauge length of 2.5 cm and a cross head speed of 10 mm min−1 were used. Dynamic mechanical analysis (DMA) were carried out using a TA Instruments Q800 analyzer (TA Instruments, New Castle, DE, USA) in tension mode. Rectangular test specimens were 6–7 mm wide and the span was 15 mm. The frequency and amplitude of oscillation were set at 1 Hz and 15 μm, respectively. The temperature varied from room temperature to 180 °C at a heating rate of 3 °C/min.
3
Tensile and Fracture Properties of Epoxy/MWNT Composites
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The tensile test of Epoxy/MWNT composites was conducted on a universal testing machine (CMT4104, SANS, Shanghai, China) at a tensile rate of 5 mm min−1. The single edge notched bend (SENB) test was performed to measure the fracture resistance of epoxy/bc@fMWNT composites in mode I tension. The specimens were prepared according to the specifications, ASTM D5045-99, whose dimensions are 10 mm wide × 4 mm thick × 70 mm length. The SENB specimens were loaded in three-point bending at a crosshead speed of 10 mm/min and a span of 40 mm. For all mechanical tests, at least five samples of each blend were tested, from which the mean values and standard deviations were calculated. DMA properties were studied with a dynamic temperature ramp from 40 to 200 °C (ramping rate = 2 °C min−1) using a Q 800 analyzer (TA Instruments, New Castle, DE, USA), at 1 Hz with a constant strain of 20 mm by single cantilever mode.
4
Comprehensive Characterization of Polymer-Based Materials
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SEMs and EDS were
performed on ZEISS EV0 MA15 transmission electron microscope (Carl
Zeiss Micro Image Co. Ltd). TGA was performed on SDTA85e thermo-analyzer
instrument (Mettler Toledo, Switzerland) under a nitrogen atmosphere
at a heating rate of 20 °C/min from 40 to 800 °C. TG/IR
was conducted on a PerkinElmer STA6000 thermogravimetric analyzer,
which was connected to a PerkinElmer FTIR spectrophotometer through
a stainless steel transfer pipe. The fire performances of PBa and
its composites were evaluated by CONE tests (Fire Testing Technology,
UK), according to ASTM E1354/ISO 5660 standard. Each specimen was
exposed horizontally under a heat flux of 35 kW/m2. The
storage moduli and tangent loss angles of materials were investigated
by dynamic thermomechanical analysis using a Q800 analyzer (TA instruments)
in three-point bending mode with sample dimensions of 40 × 10
× 3 mm3 from 40 to 300 °C at a heating rate of
5 °C/step and frequency of 1 Hz.
performed on ZEISS EV0 MA15 transmission electron microscope (Carl
Zeiss Micro Image Co. Ltd). TGA was performed on SDTA85e thermo-analyzer
instrument (Mettler Toledo, Switzerland) under a nitrogen atmosphere
at a heating rate of 20 °C/min from 40 to 800 °C. TG/IR
was conducted on a PerkinElmer STA6000 thermogravimetric analyzer,
which was connected to a PerkinElmer FTIR spectrophotometer through
a stainless steel transfer pipe. The fire performances of PBa and
its composites were evaluated by CONE tests (Fire Testing Technology,
UK), according to ASTM E1354/ISO 5660 standard. Each specimen was
exposed horizontally under a heat flux of 35 kW/m2. The
storage moduli and tangent loss angles of materials were investigated
by dynamic thermomechanical analysis using a Q800 analyzer (TA instruments)
in three-point bending mode with sample dimensions of 40 × 10
× 3 mm3 from 40 to 300 °C at a heating rate of
5 °C/step and frequency of 1 Hz.
5
Tensile and Dynamic Mechanical Analysis
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Uniaxial tensile tests were carried out with a Criterion 42 (MTS Systems, Eden Prairie, MN, United States) machine equipped with a low force (10 N) cell. Rectangular uniform pieces (5 mm × 15 mm) were cut and elongated at room conditions using a crosshead speed of 0.2 mm/min with a clamping distance of 7 mm. The Young’s modulus (E) was calculated from the maximum slope of the stress-strain curve (typically around 1–2% strain). Ten replicates per specimen were analyzed.
Storage moduli (E′) were obtained at room conditions by Dynamic Mechanical Analysis (DMA) measurements using a Q800 analyzer (TA Instruments, New Castle, DE, United States) in tension mode. In these tests, the sample is stressed with a low amplitude sinusoidal force and the strain response is simultaneously decomposed into an instantaneous in-phase (elastic) and a delayed out-of-phase (viscous) components. The storage modulus (E′) corresponds to the pure elastic response of the sample. Experiments were repeated with five samples at each daa stage. A more detailed description of the procedure is provided elsewhere (Benítez et al., 2021 (link)).
Storage moduli (E′) were obtained at room conditions by Dynamic Mechanical Analysis (DMA) measurements using a Q800 analyzer (TA Instruments, New Castle, DE, United States) in tension mode. In these tests, the sample is stressed with a low amplitude sinusoidal force and the strain response is simultaneously decomposed into an instantaneous in-phase (elastic) and a delayed out-of-phase (viscous) components. The storage modulus (E′) corresponds to the pure elastic response of the sample. Experiments were repeated with five samples at each daa stage. A more detailed description of the procedure is provided elsewhere (Benítez et al., 2021 (link)).
6
Thermal and Mechanical Analysis of PLA/CNC Composites
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Neat PLA and the PLA/CNC composites were analyzed using differential scanning calorimetry (DSC, 214, Netzsch, Germany). The samples were heated from 25 to 200 °C, held at 200 °C for 5 min to eliminate thermal history, cooled to 25 °C, and heated again to 200 °C under nitrogen purge. The heating rate was 10 °C/min, while the cooling rate 2 °C/min. Crystallization temperature (Tc) and crystallization enthalpy (△Hc) were determined from the cooling scan. The glass transition temperature (Tg), cold crystallization temperature (Tcc), melting temperature (Tm), cold crystallization enthalpy (△Hcc) and melting enthalpy (△Hm) were determined from the second heating scan.
The thermal decomposition of neat PLA and the PLA/CNC composites were evaluated by thermogravimetric analysis (TG, Netzsch 209F3, Germany). The samples were heated from 30 to 600 °C under nitrogen purge. The heating rate was 10 °C/min. Dynamic mechanical analysis (DMA) was performed in single cantilever mode using a TA Instruments Q800 analyzer (New Castle, DE). The dimensions of the test samples were 35 × 10 × 0.5 mm (length × width × thickness). The measurements were done at constant frequency (1 Hz) and amplitude (15 μm) in the temperature range from 30 to 120 °C with the heating rate of 3 °C/min.
The thermal decomposition of neat PLA and the PLA/CNC composites were evaluated by thermogravimetric analysis (TG, Netzsch 209F3, Germany). The samples were heated from 30 to 600 °C under nitrogen purge. The heating rate was 10 °C/min. Dynamic mechanical analysis (DMA) was performed in single cantilever mode using a TA Instruments Q800 analyzer (New Castle, DE). The dimensions of the test samples were 35 × 10 × 0.5 mm (length × width × thickness). The measurements were done at constant frequency (1 Hz) and amplitude (15 μm) in the temperature range from 30 to 120 °C with the heating rate of 3 °C/min.
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