EM observation on poly(β-alanine) crystal formed by the thermal solid State polymerization

1990 ◽  
Vol 48 (4) ◽  
pp. 858-859
Author(s):  
Hirokazu Kimura ◽  
Hiroshi Sakabe ◽  
Hitoshi Morita ◽  
Takashi Itoh ◽  
Takashi Konishi
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Single Crystal ◽  
Single Crystals ◽  
Water Solution ◽  
Aminocaproic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Solid State Polymerization

It is well known that several ω-amino acids are polymerized in the solid state. A single crystal of ε-aminocaproic acid has been reported to be polymerized in the solid state to be the biaxially oriented nylon 6. We also reported in the previous paper that the thermal solid state polymerization of glycine single crystal produced poly(glycine-I) crystal.In this paper,structure of poly(β-alanine) polymerized in the solid state is investigated by means of scanning electron microscopy (SEM).transmission electron microscopy (TEM) and X-ray diffraction.Commercial β-alanine (Nakarai Tesque,Inc.,Kyoto) was recrystallized three times from the distilled-water solution (lg/ml) at 80°C. The single crystal continued to grow gradually during 24 hr. The obtained single crystals with rhombic habit had clear cleavage planes. These single crystals about 10 mm in size were used as the original specimens. The polymerization procedure was carried out on the single crystals at temperatures between 140 and 170°C in an evacuated and subsequently sealed tube.

Determination of Dislocation Densities in Hexagonal Close-Packed Metals using X-Ray Diffraction and Transmission Electron Microscopy

1991 ◽  
Vol 35 (A) ◽  
pp. 593-599 ◽  
Author(s):  
M. Griffiths ◽  
J.E. Winegar ◽  
J.F. Mecke ◽  
R.A. Holt
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Single Crystal ◽  
Plastic Anisotropy ◽  
Zirconium Alloys ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hexagonal Close Packed ◽  
Transmission Electron ◽  
Dislocation Densities

AbstractX-ray diffraction (XRD) line-broadening analysis has been used to determine dislocation densities in zirconium alloys with hexagonal closepacked (hep) crystal structures and a complex distribution of dislocations reflecting the plastic, anisotropy of the material. The validity of the technique has been assessed by comparison with direct measurements of dislocation densities in deformed polycrystalline and neutron-irradiated single crystal material using transmission electron microscopy (TEM). The results show that-there is good agreement between the XRD and TEM for measurements on the deformed material whereas there is a large discrepancy for measurements on the irradiated single crystal; the XRD measurements significantly underestimating the TEM observations.

Preparation of PVC/Kaolin Nanocomposites through Solid State Shear Compounding Based on Pan-Milling

2011 ◽  
Vol 694 ◽  
pp. 350-354 ◽  
Author(s):  
Kan She Li ◽  
Ying Hong Chen ◽  
Hong Mei Niu ◽  
Jian Jun Chen
Keyword(s):  
Electron Microscopy ◽  
Tensile Strength ◽  
Solid State ◽  
Impact Strength ◽  
Ambient Temperature ◽  
Mechanical Tests ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Filled Composite

Solid state shear compounding technology (S3C) based on pan-milling is an effective method to prepare polymer/layered mineral composites with nano intercalating structure. The PVC/Kaolin compounding powders were successfully prepared by pan-milling at ambient temperature, and then the PVC/Kaolin nanocomposites were processed by moulding The structure and properties of PVC/Kaolin compounding powder and nanocomposites were investigated by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and mechanical tests. The results showed that the mechanical properties of PVC/Kaolin nanocomposites prepared through S3C based on pan-milling 30 cycles at ambient temperature including elongation, tensile strength and notched impact strength were remarkably improved compared with conventional filled composites. The elongation of PVC / Kaolin nanocomposites with 4 %wt. Kaolin was 274.6%, which is 187.3 % higher than that for a conventional filled composite. The tensile strength was 54.0 MPa, which is 6.3 MPa higher than that for a conventional filled composite. The tensile strength of the nanocomposites with 8 %wt. Kaolin was 57.5 MPa, which is 9.1 MPa higher than that for a conventional filled composite. At the same time, the notched impact strength was 4.9 kJ/m2, which is 1.0 kJ/m2 higher than a conventional filled composite. Strengthening and toughening for PVC were synchronously realized. XRD, SEM and TEM verified that S3C based on pan-milling realized synchronously pulverizing, dispersion and compounding of PVC with kaolin Through 25-30 cycles pan-milling, PVC and Kaolin powders imbedded each other and made into uniform PVC/Kaolin compounding powders and nanocomposites. The strip flake of Kaolin particles with thickness less than 50 nanometer and the aspect ratio of 10 times dispersed homogeneously in the PVC matrix.

Single Crystal Formation by Solid-State Reaction Between p-Benzoquinone and 2,4,5-Trichlorophenol

2002 ◽  
Vol 55 (4) ◽  
pp. 271 ◽  
Author(s):  
N. B. Singh ◽  
A. Pathak ◽  
R. Fröhlich
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Single Crystal ◽  
Single Crystals ◽  
Solid State Reaction ◽  
Carbonyl Oxygen ◽  
Crystal Formation ◽  
X Ray Diffraction ◽  
X Ray

Vapours of p-benzoquinone (BQ) have been found to react with solid 2,4,5-trichlorophenol (TCP). The reaction product (BQ-TCP) separated in the form of monoclinic single crystals, the structure of which was determined by X-ray diffraction to reveal that the two molecules are linked by a single hydrogen bond between the carbonyl oxygen of BQ and the phenolic hydrogen of TCP.

Solid-state reaction of Pt thin film with single-crystal (001) β–SiC

1994 ◽  
Vol 9 (3) ◽  
pp. 648-657 ◽  
Author(s):  
J.S. Chen ◽  
E. Kolawa ◽  
M-A. Nicolet ◽  
R.P. Ruiz ◽  
L. Baud ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Single Crystal ◽  
Atomic Scale ◽  
Solid State Reactions ◽  
Main Reaction ◽  
Main Reaction Product ◽  
X Ray Diffraction ◽  
X Ray ◽  
Amorphous Interlayer

Thermally induced solid-state reactions between a 70 nm Pt film and a single-crystal (001) β-SiC substrate at temperatures from 300 °C to 1000 °C for various time durations are investigated by 2 MeV He backscattering spectrometry, x-ray diffraction, secondary ion mass spectrometry, scanning electron microscopy, and cross-sectional transmission electron microscopy. Backscattering spectrometry shows that Pt reacts with SiC at 500 °C. The product phase identified by x-ray diffraction is Pt3Si. At 600–900 °C, the main reaction product is Pt2Si, but the depth distribution of the Pt atoms changes with annealing temperature. When the sample is annealed at 1000 °C, the surface morphology deteriorates with the formation of some dendrite-like hillocks; both Pt2Si and PtSi are detected by x-ray diffraction. Samples annealed at 500–900 °C have a double-layer structure with a silicide surface layer and a carbon-silicide mixed layer below in contact with the substrate. The SiC—Pt interaction is resolved at an atomic scale with high-resolution electron microscopy. It is found that the grains of the sputtered Pt film first align themselves preferentially along an orientation of {111}Pt//{001}SiC without reaction between Pt and SiC. A thin amorphous interlayer then forms at 400 °C. At 450 °C, a new crystalline phase nucleates discretely at the Pt-interlayer interface and projects into or across the amorphous interlayer toward the SiC, while the undisturbed amorphous interlayer between the newly formed crystallites maintains its thickness. These nuclei grow extensively down into the substrate region at 500 °C, and the rest of the Pt film is converted to Pt3Si. Comparison between the thermal reaction of SiC-Pt and that of Si–Pt is discussed.

SOLID STATE AMORPHIZATION IN MECHANICALLY ALLOYED Al–Ti–Si NANOCOMPOSITES

2005 ◽  
Vol 04 (05n06) ◽  
pp. 1025-1028
Author(s):  
I. MANNA ◽  
P. NANDI ◽  
B. BANDYOPADHYAY ◽  
P. M. G. NAMBISSAN ◽  
K. GHOSHRAY ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Amorphous Solid ◽  
Positron Annihilation Spectroscopy ◽  
Intermetallic Phases ◽  
X Ray Diffraction ◽  
Mechanically Alloyed ◽  
X Ray ◽  
Transmission Electron ◽  
State Amorphization

The microstructural evolution at different stages of milling of a ternary powder blend of Al 50 Ti 40 Si 10 composition was monitored by X-ray diffraction, high-resolution transmission electron microscopy, positron annihilation spectroscopy and 27 Al nuclear magnetic resonance. Ball-milling leads to alloying, nanocrystallization and partial solid state amorphization, either followed or accompanied by strain-induced nucleation of nanocrystalline intermetallic phases from an amorphous solid solution.

scholarly journals Synthesis, Crystal Growth, Structure, Crystalline Perfection, Thermal, Linear and Nonlinear Optical Investigations on 2-Amino-5-Nitropyridine 4-Chlorobenzoic Acid (1:1): A Novel Organic Single Crystal for NLO and Optical Limiting Optical Applications

2021 ◽  
Author(s):  
Sivasubramani Vediyappan ◽  
Arumugam Raja ◽  
Ro Mu Jauhar ◽  
Ramachandran Kasthuri ◽  
Vishwanathan Vijayan ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Single Crystals ◽  
Nonlinear Optical ◽  
Grown Crystal ◽  
Solid State Laser ◽  
X Ray Diffraction ◽  
Chlorobenzoic Acid ◽  
X Ray ◽  
532 Nm

Abstract 2-amino-5-nitropyridine 4-chlorobenzoic acid (1:1) (2A5NP4CBA), a potentially useful organic adduct compound has been synthesized and grown as optically transparent single crystals by conventional slow evaporation solution technique (SEST) for the first time in the literature. The formation of the new crystalline material was confirmed by the single-crystal X-ray diffraction (SXRD) analysis and the crystal structure of the grown crystal was found to be monoclinic. Fourier transform infrared (FTIR) spectrum has been recorded by the KBr pellet technique to determine the various vibrational functional groups in the title material. The powder X-ray diffraction (PXRD) and high-resolution X-ray diffraction (HRXRD) analyses have been carried out and the obtained results reveal that the grown crystal has a single-phase and is free from structural grain boundaries. The obtained less value (32 arc-s) of full width at half maximum (FWHM) for (001) plane indicates the excellent crystalline quality of the title 2A5NP4CBA single crystal. The linear optical properties were evaluated by the UV-vis-NIR absorption and transmittance analyses and the obtained results reveal that the grown crystal possesses more than 70% of optical transmittance window with the cut-off edge at 419 nm. The thermal analysis discloses that the grown crystal possesses good thermal stability of about 187°C. To determine the appropriateness of the grown crystal for the high-power laser application, laser damage threshold (LDT) analysis has been carried out by Nd: YAG laser of a wavelength of 1064 nm. The third-order nonlinear optical coefficients such as nonlinear absorption (β), nonlinear refraction (n 2 ) and nonlinear susceptibility (χ (3) ) have been evaluated by utilizing the single beam Z-scan technique using a solid-state laser of wavelength 532 nm. The calculated ꭓ (3) value is found to be reasonably good compared to other organic single crystals which are reported in the literature. The optical limiting (OL) behavior of the title crystal was evaluated using a solid-state laser at 532 nm and the limiting threshold was found to be 7.8 mW/cm 2 .

Oxide Structures formed on Silver Single Crystals due to Hyperthermal Atomic Oxygen Exposure

2002 ◽  
Vol 751 ◽  
Author(s):  
Long Li ◽  
Judith C. Yang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Single Crystals ◽  
Atomic Oxygen ◽  
X Ray Diffraction ◽  
X Ray ◽  
Optical Scanning ◽  
Transmission Electron ◽  
Oxide Phases ◽  
Ag Substrate

ABSTRACTSilver (100) and (111) single crystals were exposed to a unique laser detonation atomic oxygen source, which produces a high flux of 5 eV atomic oxygen, for seven hours at 220°C. The resultant oxide and oxide-metal interfaces were characterized by optical, scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HREM). The oxide scale was more than 10-micron thick and very weakly attached to the Ag substrate. The silver oxides were complex and surprising, differ in their thickness and the oxide phases due to the orientation of the Ag single crystals. The cross-section TEM studies revealed complex microstructures with many defects, such as micro-twins, porosity and irregular shaped grains.

Solid-state reaction of Ru powder in molten AlxBi1−x

1990 ◽  
Vol 5 (4) ◽  
pp. 746-753 ◽  
Author(s):  
R. W. Johnson ◽  
C. M. Garland
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Solid State ◽  
Alloy System ◽  
Reaction Cross ◽  
X Ray Diffraction ◽  
Cross Sectional ◽  
X Ray ◽  
Transmission Electron ◽  
Metal Solvent

We describe a low-temperature solid-state interdiffusion technique that allows reaction between spatially separated reacting species and its application in the Al–Ru alloy system. This technique uses a liquid-metal solvent (Bi) as a medium for the transfer of Al to the surface of Ru powder where reaction occurs with the formation of nanocrystalline AlxRu1−x product phases. X-ray diffraction measurements are used to follow the time and temperature dependence of the reaction. Cross-sectional transmission electron microscopy allows direct imaging of the growth and morphology of the AlxRu1−x product phases.

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