Melt Crystallization Behavior and Spherulitic Morphology of Poly(Trimethylene Terephthalate)/Poly(Propylene Glycol) Copolymers with Different Poly(Propylene Glycol) Molecular WeightsLi, Peng; Yao, Chenguang; Yang, Guisheng

Polymer-Plastics Technology and Engineering, 2018, vol 57, 8, pp. 775-790

DOI:10.1080/03602559.2017.1354219

Abstract

Poly(trimethylene terephthalate)/poly(propylene glycol) (PTT/PPG) copolymers with different PPG molecular weights (400–4,000 g /mol) were successfully synthesized and characterized. Double melting endotherms during isothermal melt crystallization were observed by differential scanning calorimetry. Middle-temperature melting endotherms in all copolymers were stronger than that in PTT homopolymer and became smaller with the increasing PPG molecular weight. Nonisothermal crystallization kinetics of all samples were analyzed by Ozawa and Mo models. Polarized optical microscopy micrographs revealed that ring-banded spherulitic morphology was relatively easier to be observed in copolymers with higher PPG molecular weight at lower crystallization temperature, and PPG molecular weight nearly had no influence on the band spacing.

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Mirror type	Figure	Optic efficiency (calculated over mirror length for 70µm source)
Standard Montel mirrors		Eff = 42%
Xenocs FOX 3D mirrors		Eff = 62%


Model	Beam size at focus (mm) with 60 µm source	Divergence (mrad)	Typical application
FOX 3D Cu 14-39 (♦)	0.19 x 0.19	5.4	Protein crystallography (♦) Powder diffraction
FOX 3D Cu 12-53	0.3 x 0.3	3	Protein crystallography (Long Unit Cells) Powder diffraction
FOX 3D Mo 10-31	0.13 x 0.13	4	Small molecule crystallography High pressure diffraction
FOX 3D Ag 10-30	0.13 x 0.13	3	Small molecule crystallography High pressure diffraction
FOX 3D Cr 8-30	0.20 x 0.20	6	Protein crystallography (S-SAD) Stress analysis
FOX 1D Cu 12-53	0.3	3	XRD, Powder Diffraction


Model	Beam size at focus (mm) with 60 µm source	Divergence (mrad)	Typical application
FOX 2D Mo 25-25 (♦)	0.08 x 0.08	5	Small mollecule crystallography High pressure crystallography
FOX 2D Cu 25-25 (♦)	0.08 x 0.08	5.3	Protein crystallography (♦) Micro Diffraction, Reflectometry
FOX 3D Cu 21-21 HC (♦)	0.08 x 0.08	70 x 35	Rapid x-ray Reflectometry (full beam) Scanning x-ray Reflectometry (with slit) Micro-XRF
FOX 3D Cu 28-10	0.04 x 0.04	17	Stress Analysis, Micro-diffraction, Micro-XRF
FOX 3D Cr 30-8	0.04 x 0.04	17	Stress Analysis, Micro-diffraction, Micro-XRF


Model	Beam size at focus (mm) with 60 µm source	Divergence (mrad)	Typical application
FOX 2D Cu 12-INF (♦)	1.2 x 1.2	1	Small angle x-ray scattering (♦) High resolution x-ray diffraction (♦) Surface scattering (♦) Thin film analysis (reflectometry stress) (♦) Microdiffraction on synchrotron (♦)
FOX 2D Mo 25-INF (♦)	0.85 x 1.3	0.5	Small angle x-ray scattering High resolution x-ray diffraction Surface scattering
FOX 2D 12-60 L (♦)	0.18 x 0.2	0.5 x 2	High resolution diffraction Small sample analysis
FOX 1D Cu 12-INF (♦)	1.2	0.8	High resolution x-ray diffraction, Powder diffraction, Reflectometry, Small angle x-ray scattering

Melt Crystallization Behavior and Spherulitic Morphology of Poly(Trimethylene Terephthalate)/Poly(Propylene Glycol) Copolymers with Different Poly(Propylene Glycol) Molecular Weights
Li, Peng; Yao, Chenguang; Yang, Guisheng

Abstract

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Element of interest	Reference
O, F, Na, Mg, Al, Si, P, S	XAN-1
Nitrogen	XAN-2
Carbon	XAN-3
Boron	XAN-4
Mg, Al , Si	XAN-5
Be	XAN-6


Model	Beam size at focus (µm)	Divergence (mrad)	Flux (ph/sec)	Typical application
GeniX 3D Cu High Flux *	< 190	6	> 400 x 10⁶	Protein crystallography Micro stress analysis Powder diffraction
GeniX 3D Mo High Flux	< 130	5	> 25 x 10⁶	Small Molecule crystallography High pressure
GeniX 3D Cr High Flux	< 190	6	> 300 x 10⁶	Stress Analysis
GeniX 3D Cu High Convergence *	60	70 x 35	> 400 x 10⁶	Rapid X-ray Reflectometry (full beam) Scanning x-ray reflectometry (with slit) Micro x-ray fluorescence Small spot diffraction on thin film
GeniX 3D Cu Low Convergence *	< 250	3	> 120 x 10⁶	Small Angle X-ray Scattering Protein Crystallography



Source	Microfocus sealed tube: Cu, 30W/30µm, point focus. ( DIN EN 12543-5) MetalJet source D2+ (Ga). Motorized Dual source or triple source (Cu/Mo/Cr/Ga).
Optics	Patented 2D single reflection multilayer optics.
Detector	In-vacuum motorized 3-axis detectors for 2D SAXS/WAXS (Q-Xoom): --Pilatus3 R 300K hybrid photon counting detector --Eiger2 R (1M, 4M) hybrid photon counting detectors Optional WAXS detectors for SWAXS: --Pilatus3 R 100K hybrid photon counting detector --Motorized 3-axis Eiger2 R 500K hybrid photon counting detector
Sample chamber	Large vacuum chamber. On-axis sample viewing (parallax free). Attachments for operation of sample in air.
Key features	Clean Beam technology: high flux and low background beamline. Beamstopless measurement: SAXS acquisition continuously without any beamstop. Q-Xoom: Automatic change of measurement configuration over all instrument Q-range with no movement of sample measuring position. Virtual detector mode: surfaces of detection > 200 mm² x 200 mm².
Measurement capability	Nanoparticles size up to 300 nm, 500 nm or 900 nm in diameter depending on Xeuss model. Nanoparticles size up to > 2.5 microns with optional motorized Bonse-Hart module for automatic sequential USAXS/SAXS/WAXS measurements. Scattering measurements up to 2Ɵ>70° with Q-Xoom. Qmax > 49 nm^-1
Sample environment	Standard holders (multi-samples): solids, capillaries, powders. Sample holders for powders and gels. Flowcells for liquids: --- Low noise flowcell --- Capillary flowcell --- Automatic Sample Changer --- BioCube measuring cell with dynamic monitoring (compatible with pipetting robot) Temperature stages: --- Multi-purpose X-Ray Temperature Stage (-30°C to 150°C) --- High temperature sample stage (-150°C to 350°C) --- Extended high temperature sample stage (amb - 1000°C) Tensile Stage (00-600N). Humidity stage (10%-90% from ambient to 60°C). Shear stage Temperature compatible GiSAXS stage Other sample stages available under request
Software	Acquisition software with automatic data reduction in absolute units and live data display. XSACT (X-ray Scattering Analysis and Calculation Tool) for data analysis and interpretation.
General parameters	Models & Footprint : Xeuss 3.0 C (1 m x 3 m), HR (1 m x 5 m), UHR (1 m x 8 m). Maximum power consumption: < 3000 W (single phase power)



Source and optics	Microfocus sealed tube: Cu, 30W/30µm, point focus. ( DIN EN 12543-5) Patented 2D single reflection multilayer optics.
Detector	Dectris Pilatus 3 hybrid photon counting detectors. Two fixed detectors for continuously and simultaneously. SAXS and WAXS acquisition up to 2θ=60°.
Beam Path	Windowless beam path entirely under vacuum from beam delivery system to detector sensor
Key features	Clean Beam technology: high flux and low background beamline. Beamstopless measurement: SAXS acquisition continuously without any beamstop. Virtual detector mode: > 200° azimuth coverage with rotation of sample.
Measurement capability	Nanoparticles size up to 250 nm in diameter.
Sample environment	Standard holders: solids, capillaries, powders. Sample holders for powders and gels. Flow cells for liquids: --- Low noise flow cell --- Capillary flow cell Automatic Sample Changer Temperature stages: --- Multi-purpose X-Ray Temperature Stage (-20°C to 150°C) --- High temperature sample stage (-150°C to 350°C) --- Extended high temperature sample stage (amb - 700°C) Tensile Stage (0-200N). GiSAXS stage compatible with high temperature sample stage. Custom stages on request.
Software	Acquisition software with automatic data reduction in absolute units and live data display. XSACT (X-ray Scattering Analysis and Calculation Tool) for data analysis and interpretation.
General parameters	Fooprint: < 1x1 m². Weight: ~ 520 kg. Maximum power consumption: < 2000 W (single phase power). Self-contained: no external fluids required.
Warranty	Two years warranty and three years on X ray source.