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398 protocols using dma q800

1

Thermal and Mechanical Analysis of PTK-UR and PEUR Scaffolds

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Thermal transitions were measured by a TA Instruments (New Castle, DE) Q200 DSC and Q800 DMA. For DSC analysis, samples ranging in mass from 10–15 mg were heated from −80° C to 200° C at a rate of 10° C min−1, cooled to −80° C at a rate of −20° C min−1, and heated a second time to 200° C at a rate of 10° C min−1. All transitions were obtained from the second heating run. For dynamic mechanical analysis (DMA, Q800 DMA, TA Instruments, New Castle, DE), cylindrical samples (6 × 6 mm) were analyzed from −80° to 55° C at a ramp rate of 1° C min−1. Scaffolds were compressed at a frequency of 1 Hz with 1% strain during the thermal treatment. Glass transitions were obtained at the peak of tan δ.
The mechanical properties of the different PTK-UR and PEUR scaffold formulations were measured in compression at 37°C in a submersion compression clamp using the Q800 DMA. Cylindrical 6 × 6 mm scaffold samples were tested after incubation in phosphate buffered saline (PBS) for 7 days at 37°C. Using a preload force of 0.1 N, samples were compressed along the longitudinal axis at a strain rate of 10% per min until 60% compressive strain was achieved. The Young’s modulus for each sample was calculated from the slope of the initial linear region of each respective stress-strain curve after toe-in.
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2

Dynamic Mechanical and Tensile Properties

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Compression molded samples with dimensions of 14.0 mm × 8.0 mm × 0.3 were analyzed in a Q800 DMA (TA Instruments, New Castle, DE, USA) using a film clamp at 1 Hz under multi frequency-strain mode from −50 to 310 °C and at a heating rate of 3 °C min−1 [72 (link)]. A total of two measurements were taken for each sample. The results were presented as loss factor (tan δ) and given by the ratio between the loss modulus (E″) and the storage modulus (E′) as a function of temperature.
Tensile tests were carried out at 21 °C in a Q-800 DMA equipment (TA Instruments) according to the ISO 527-3 method and with rectangular compression-molded films 14.0 mm × 8.0 mm × 0.3 mm that had previously been conditioned at 21 °C and 50% relative humidity for a period of at least 48 h. The samples were placed between a fixed and a moveable film clamp, and the experiments were performed in triplicate in tensile mode. The tensile strength (σ), Young’s modulus (E) and elongation at break (ε) were determined [73 (link)].
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3

Comprehensive Material Characterization

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The rheological measurements were performed on a Haake MARSIII rheometer equipped with a geometry of 25 mm parallel plates at 25°C. The electrical tests were performed by a CHI 660E electrochemical workstation (CH Instruments, Chenhua Co., Shanghai, China). The tensile and compression tests were performed on a CMT-1104 universal testing machine (CMT-1104, SUST Electrical Equipment Co., Zhuhai, China). The dynamic mechanical analysis was performed on a DMAQ800 analyzer (DMAQ800, TA, America). The samples were frozen in liquid nitrogen for 10 min before lyophilizing with a freeze drier (FD-1C-50, Beijing Boyikang) at −35°C for about 48 h.
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4

Characterization of Polymer Materials

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Fourier transform infrared spectroscopy (FTIR) was carried out on a Nicolet 6700 FTIR spectrometer using the attenuated total reflection (ATR) mode with a scan range from 400 to 4000 cm-1. Dynamic mechanical analysis (DMA) was performed on a TA Instruments DMA Q800 with a heating rate of 3 °C min−1 and a frequency of 1 Hz. Double cantilever mode was used for the DMA tests and the specimen dimension was 60 × 15.0 × 2.0 mm3. Stress-relaxation tests were also performed on a TA Instruments DMA Q800. The tests were carried out using the tensile mode with rectangular specimens (12.0 × 6.0 × 1.0 mm3). The specimen was aligned by preloading 10-3 N force and thermally equilibrated for 10 min at each test temperature. The data of relaxation modulus versus time were recorded. Flexural tests, which followed the ASTM D790-03 standard, were performed on the Wance ETM104B-EX electronic universal testing machine with a 2000 N load cell at a crosshead speed of 1 mm min−1. Each reported value was the average of at least three valid specimens. Thermal gravimetric analysis (TGA) was conducted on a TA Instruments TGA Q 500 using nitrogen as the purge gas at a heating rate of 10 °C min-1 from 50 to 800 °C.
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5

Thermal and Viscoelastic Properties of PLA

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Using TA Instruments
DSC Q200, the thermal properties of the samples were studied. Two
tests per sample were performed to create a standard deviation. Approximately,
5 mg was cut from each sample and was encapsulated in aluminum. With
a 50 mL/min–1 nitrogen flow rate, the samples were
ramped at 5.00 °C/min using a heat/cool/heat method. The crystallinity
of the samples was calculated using the following formula where ΔHm is the measured melting enthalpy, ΔHcc is the measured enthalpy of cold crystallization, and
ΔHm0 is the theoretical melting enthalpy of 100%
crystalline PLA, taken
from the literature to be 93.7 J/g4.
Dynamic thermal
analysis (DMA) was performed with the use of a DMA Q800 (TA Instruments,
New Castle, DE). All measurements were carried out at a constant frequency
of 1 Hz and strain amplitude of 0.01%. The temperature range was 30–150
°C, whereas the heating rate was 3 °C/min. The viscoelastic
properties were collected from rectangular samples (3.2 × 12.7
× 50 mm) using the dual cantilever measurement mode.
The
heat deflection temperature (HDT) of the samples was acquired
using TA Instruments DMA Q800 following ASTM D648. The desired stress
of 0.455 MPa was applied to the midsection of the sample, and a heating
rate of 2 °C/min was utilized. The strain rate was measured at
250 μm (0.2% strain), and two tests were performed on each type
of sample.
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6

Tensile and Adhesion Testing of PEDOT:Nafion Fibers

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Tensile testing of PEDOT:Nafion
fibers was performed using a DMA Q800 (TA Instruments) with a ramped
force of 0.5 N min–1. The dynamic characterization
was performed by subjecting a fiber to 100 cycles of 6 s displacement
to 10% strain followed by 30 s release. The electrical resistance
was measured in situ using a Keysight U1253B multimeter collecting
1 data point s–1. Samples of the Nafion/ABS blends
for tensile testing were prepared in a hot press (AB Nike Hydralik)
at 240 °C in two steps, 5 ton for 2 min and 10 tons for 3 min,
with 0.1 mm spacers. The resulting films were cut into strips with
a width of 4 mm and a thickness varying from 0.07 to 0.13 mm. The
Young’s modulus of Nafion/ABS blends was determined from tensile
tests at a force rate of 1 N min–1 using a DMA Q800
(TA Instruments). To test the adhesion between Nafion/ABS blends,
ABS and HIPS, rectangular test strips (30 mm × 5 mm × 0.2
mm) were 3D printed onto printed substrates (thickness 0.2 mm). At
one end, the strips were separated from the substrate by a thin paper.
The loose ends of the strips and the substrate were mounted into a
DMA TA Q800, and peeling tests were performed with a constant displacement
rate of 1 mm min–1.
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7

Dynamic Mechanical Analysis of EFMs

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The mechanical properties of the resulted EFMs were carried out using dynamic mechanical analysis instrument (DMA Q800, TA instruments, New Castle, DE, USA). All the samples were cut into a specific rectangular shape, with a width fixed at 2 mm cut by the tools provided by TA instruments and the length (approximately 1 cm) of the EFMs was detected by the DMA instrument software (DMA Q800). The thickness of the mats was exactly measured by the electronic micrometer (Schut Geometrical Metrology, Netherland). The mechanical properties of the EFMs were studied at RT with a ramp displacement of 100 µm/min in a DMA strain rate mode. Each specimen was measured in triplicate.
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8

Cyclic Tensile Strain Analysis of Rectangular Gels

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Rectangular gels with approximate dimensions of 15 mm × 2 mm × 1 mm were prepared as described above. Samples were subjected to a cyclic tensile strain of 0.01% at 1 Hz while a temperature ramp was applied at 3.0 °C/min using DMA (Q800 DMA, TA). Temperature ranges were selected to accurately capture the full range of glass transition and storage modulus. The glass transition temperature was determined from the maximum value of the tan delta curve and the rubbery modulus E was determined from the plateau of the storage modulus at T = Tg + 40 °C.
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9

Stress Relaxation Behavior of Composite Bars

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Stress relaxation experiments were conducted using dynamic mechanical analysis (Q800 DMA, TA Instruments, New Castle, DE, USA). Composite bar specimens (1 × 3 × 25 mm) were cured for 90 s per side at 600 mW/cm2 and thermally post-cured at 180 °C until >90% conversion was reached in order to prevent additional polymerization during DMA testing. Stress relaxation measurements were performed in tension mode at discrete temperature points between 80 and 155 °C using a fixed 0.05% strain. The relaxation modulus decrease was measured for 30 min per temperature point. The characteristic relaxation time was defined as the time required for the material to relax to 50% of the original modulus, E0.
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10

Comprehensive Surface Morphology Analysis

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Surface morphology was investigated by utilizing JSM-6700F filed emission scanning electron microscope (FE-SEM, JEOL, Japan) after platinum coating (10 nm thickness). AFM images were obtained from an AFM instrument (PSIA XE-100E, Suwon, Korea) using tapping mode. DMA was performed with a TA Instruments Q800 DMA (USA) with a heating rate of 5 °C /min from 25 °C to 160 °C at 1.0 Hz.
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