Optical and Dimensional Changes Which Accompany the Freezing and Melting of Hevea Rubber

1939 ◽  
Vol 12 (1) ◽  
pp. 18-30 ◽  
Author(s):  
W. Harold Smith ◽  
Charles Proffer Saylor
Keyword(s):  
Optical Properties ◽  
Low Temperatures ◽  
Heat Content ◽  
Uniaxial Crystal ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Changes ◽  
Ether Yield ◽  
The Individual

Abstract At suitable, low temperatures, unvulcanized rubber loses its elasticity and becomes hard and opaque. Similar changes frequently occur in baled rubber which has been tightly compressed before shipment. It is said to be frozen or “boardy.” The phenomenon has been studied by many investigators who have determined changes of volume, softening temperatures, the effects of increasing time of storage at low temperatures, the influence of pressure during freezing, and changes in heat capacity and entropy. These effects have generally been ascribed to a form of crystallization, and x-ray diffraction powder patterns indicate that crystals are present in frozen rubber. When total rubber is stretched, there are changes of volume and of heat content such as attend crystallization. With x-rays a crystal fiber pattern is obtained. It and the powder pattern obtained with frozen, compact rubber have been shown to indicate similar spacings and are assumed to be caused by the same type of crystal, the differences being ascribed to conditions of orientation. Dilute solutions of rubber hydrocarbon in ethyl ether yield small crystals of the hydrocarbon when they are subjected to temperatures between −35° and − 60° C. for several hours. The optical properties and melting points of these crystals and their x-ray diffraction patterns indicate their identity with the crystals in stretched and frozen rubber. Under the best conditions the crystals appear in spherulitic groupings, the individual needles in each spherulite having optical properties that closely approach those of a uniaxial crystal with negative elongation. The crystals of sol rubber which we obtained, melted between 9.5° and 11.0° C. Crystals of gel rubber melted between −2° and 14° C., but the melting ranges within this interval were not the same for all samples. Numerous observations have repeatedly confirmed the data. About 90 per cent of the rubber in solution may be obtained as birefringent material at −65° C. Temperatures between −40° and −50° C. have been preferred, however, because better crystals are obtained in that range.

Masquerade: removing non-sample scattering from integrated reflection intensities

2012 ◽  
Vol 45 (2) ◽  
pp. 292-298 ◽  
Author(s):  
J. A. Coome ◽  
A. E. Goeta ◽  
J. A. K. Howard ◽  
M. R. Probert
Keyword(s):  
Data Collection ◽  
Diffraction Data ◽  
Low Temperatures ◽  
Test Case ◽  
X Rays ◽  
Atmospheric Conditions ◽  
X Ray Diffraction ◽  
New Approach ◽  
X Ray ◽  
Internal Agreement

X-ray diffraction experiments at very low temperatures require samples to be isolated from atmospheric conditions and held under vacuum. These conditions are usually maintainedviathe use of beryllium chambers, which also scatter X-rays, causing unwanted contamination of the sample's diffraction pattern. The removal of this contamination requires novel data-collection and processing procedures to be employed. Herein a new approach is described, which utilizes the differences in origin of scattering vectors from the sample and the beryllium to eliminate non-sample scattering. The programMasqueradehas been written to remove contaminated regions of the diffraction data from the processing programs. Coupled with experiments at different detector distances, it allows for the acquisition of decontaminated data. Studies of several single crystals have shown that this approach increases data quality, highlighted by the improvement in internal agreement factor with the test case of cytidine presented herein.

Three-Dimensional X-Ray Diffraction Microscopy Using High-Energy X-Rays

MRS Bulletin ◽  
2004 ◽  
Vol 29 (3) ◽  
pp. 166-169 ◽  
Author(s):  
Henning F. Poulsen ◽  
Dorte Juul Jensen ◽  
Gavin B.M. Vaughan
Keyword(s):  
Materials Science ◽  
Three Dimensional ◽  
High Energy ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reconstruction Methods ◽  
The Individual ◽  
Individual Grains

AbstractThree-dimensional x-ray diffraction (3DXRD) microscopy is a tool for fast and nondestructive characterization of the individual grains, subgrains, and domains inside bulk materials. The method is based on diffraction with very penetrating hard x-rays (E ≥ 50 keV), enabling 3D studies of millimeter-to-centimeter-thick specimens.The position, volume, orientation, and elastic and plastic strain can be derived for hundreds of grains simultaneously. Furthermore, by applying novel reconstruction methods, 3D maps of the grain boundaries can be generated. The 3DXRD microscope in use at the European Synchrotron Radiation Facility in Grenoble, France, has a spatial resolution of ∼5 μm and can detect grains as small as 150 nm. The technique enables, for the first time, dynamic studies of the individual grains within polycrystalline materials. In this article, some fundamental materials science applications of 3DXRD are reviewed: studies of nucleation and growth kinetics during recrystallization, recovery, and phase transformations, as well as studies of polycrystal deformation.

Study of Structural Detail by X-rays of Wavelength Greater than 4Å

1970 ◽  
Vol 14 ◽  
pp. 275-292
Author(s):  
H. K. Herglotz
Keyword(s):  
High Intensity ◽  
Interplanar Distance ◽  
X Rays ◽  
X Ray Diffraction ◽  
Photographic Recording ◽  
X Ray ◽  
Dimensional Changes ◽  
Long Wavelength ◽  
Extra Effort ◽  
Structural Research

AbstractSome branches of structural research could benefit from supplemental information provided by “soft” x-rays. Little use is made of these wavelengths because they are difficult to generate at high intensity, hard to collimate, need vacuum for propagation, and are heavily absorbed in the sample. None of these difficulties is insurmountable, however, and it will be shown that the information to be gained is often worth the extra effort.A few theoretical and experimental examples with silver L-radiation (λ ≈ 4.15Å) and aluminum K-radiation (λ ≈ 8.34Å) demonstrate that valuable semiquantitative information on the size and number of aperiodic scatterers in solid samples can be extracted. Other examples show the superior sensitivity of these longer wavelengths to dimensional changes in periodic lattices. Applicability of long-wavelength diffraction is restricted to values of interplanar distance d > λ/2. Valuable information about lattice imperfection can be gained from broadening of the reflection at larger glancing angles. It is shown that the heavy absorption of these wavelengths in the sample is not necessarily prohibitive.The instrumentation used in these studies was designed for routine operation by laboratory personnel without special training. It consists of a demountable high-intensity x-ray source and a multipurpose highvacuum camera. Operation of the x-ray unit resembles that of commercial x-ray diffraction instruments. Because of its greater-flexibility, photographic recording has been practiced so far but could be replaced by electronic readout.

An introduction to three-dimensional X-ray diffraction microscopy

2012 ◽  
Vol 45 (6) ◽  
pp. 1084-1097 ◽  
Author(s):  
Henning Friis Poulsen
Keyword(s):  
Materials Science ◽  
Strain Tensor ◽  
Three Dimensional ◽  
X Rays ◽  
Reconstruction Algorithms ◽  
X Ray Diffraction ◽  
Synchrotron Source ◽  
X Ray ◽  
The Individual ◽  
Diffraction Microscopy

Three-dimensional X-ray diffraction microscopy is a fast and nondestructive structural characterization technique aimed at studies of the individual crystalline elements (grains or subgrains) within millimetre-sized polycrystalline specimens. It is based on two principles: the use of highly penetrating hard X-rays from a synchrotron source and the application of `tomographic' reconstruction algorithms for the analysis of the diffraction data. In favourable cases, the position, morphology, phase and crystallographic orientation can be derived for up to 1000 elements simultaneously. For each grain its average strain tensor may also be derived, from which the type II stresses can be inferred. Furthermore, the dynamics of the individual elements can be monitored during typical processes such as deformation or annealing. A review of the field is provided, with a viewpoint from materials science.

X-ray diffraction properties of curved crystal diffractors

1992 ◽  
Vol 50 (2) ◽  
pp. 1734-1735
Author(s):  
W. Z. Chang ◽  
D. B. Wittry
Keyword(s):  
Diffraction Theory ◽  
X Rays ◽  
Diffraction Image ◽  
X Ray Diffraction ◽  
Rocking Curve ◽  
X Ray ◽  
Bent Crystal ◽  
Diffraction Geometry ◽  
Crystal Parameter ◽  
Quantitative Procedure

Since Du Mond and Kirkpatrick first discussed the principle of a bent crystal spectrograph in 1930, curved single crystals have been widely utilized as spectrometric monochromators as well as diffractors for focusing x rays diverging from a point. Curved crystal diffraction theory predicts that the diffraction parameters - the rocking curve width w, and the peak reflection coefficient r of curved crystals will certainly deviate from those of their flat form. Due to a lack of curved crystal parameter data in current literature and the need for optimizing the choice of diffraction geometry and crystal materials for various applications, we have continued the investigation of our technique presented at the last conference. In the present abstract, we describe a more rigorous and quantitative procedure for measuring the parameters of curved crystals.The diffraction image of a singly bent crystal under study can be obtained by using the Johann geometry with an x-ray point source.

Structural and optical properties of Tin Oxide and Indium doped SnO2 thin films deposited by thermal evaporation technique

2016 ◽  
Vol 12 (3) ◽  
pp. 4394-4399
Author(s):  
Sura Ali Noaman ◽  
Rashid Owaid Kadhim ◽  
Saleem Azara Hussain
Keyword(s):  
Thin Films ◽  
Optical Properties ◽  
Tin Oxide ◽  
Thermal Evaporation ◽  
Pure Sno2 ◽  
X Ray Diffraction ◽  
Structural And Optical Properties ◽  
X Ray ◽  
Evaporation Technique ◽  
Sno2 Thin Films

Tin Oxide and Indium doped Tin Oxide (SnO2:In) thin films were deposited on glass and Silicon  substrates  by  thermal evaporation technique.  X-ray diffraction pattern of  pure SnO2 and SnO2:In thin films annealed at 650oC and the results showed  that the structure have tetragonal phase with preferred orientation in (110) plane. AFM studies showed an inhibition of grain growth with increase in indium concentration. SEM studies of pure  SnO2 and  Indium doped tin oxide (SnO2:In) ) thin films showed that the films with regular distribution of particles and they have spherical shape.  Optical properties such as  Transmission , optical band-gap have been measured and calculated.

scholarly journals Study on the Electrical, Structural, Chemical and Optical Properties of PVD Ta(N) Films Deposited with Different N2 Flow Rates

Coatings ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 937
Author(s):  
Yingying Hu ◽  
Md Rasadujjaman ◽  
Yanrong Wang ◽  
Jing Zhang ◽  
Jiang Yan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Optical Properties ◽  
Photoelectron Spectroscopy ◽  
Crystal Size ◽  
Silicon Substrates ◽  
X Ray Diffraction ◽  
Dc Magnetron Sputtering ◽  
Flow Rates ◽  
X Ray ◽  
N2 Flow Rate

By reactive DC magnetron sputtering from a pure Ta target onto silicon substrates, Ta(N) films were prepared with different N2 flow rates of 0, 12, 17, 25, 38, and 58 sccm. The effects of N2 flow rate on the electrical properties, crystal structure, elemental composition, and optical properties of Ta(N) were studied. These properties were characterized by the four-probe method, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and spectroscopic ellipsometry (SE). Results show that the deposition rate decreases with an increase of N2 flows. Furthermore, as resistivity increases, the crystal size decreases, the crystal structure transitions from β-Ta to TaN(111), and finally becomes the N-rich phase Ta3N5(130, 040). Studying the optical properties, it is found that there are differences in the refractive index (n) and extinction coefficient (k) of Ta(N) with different thicknesses and different N2 flow rates, depending on the crystal size and crystal phase structure.

scholarly journals Physical and chemical imaging of adhesive interfaces with soft X-rays

2021 ◽  
Vol 2 (1) ◽  
Author(s):  
Hiroyuki Yamane ◽  
Masaki Oura ◽  
Osamu Takahashi ◽  
Tomoko Ishihara ◽  
Noriko Yamazaki ◽  
...  
Keyword(s):  
Molecular Level ◽  
Covalent Bond ◽  
Chemical Imaging ◽  
Diglycidyl Ether ◽  
X Rays ◽  
X Ray ◽  
Covalent Bond Formation ◽  
Chemical States ◽  
The Individual ◽  
Physical And Chemical

AbstractAdhesion is an interfacial phenomenon that is critical for assembling carbon structural composites for next-generation aircraft and automobiles. However, there is limited understanding of adhesion on the molecular level because of the difficulty in revealing the individual bonding factors. Here, using soft X-ray spectromicroscopy we show the physical and chemical states of an adhesive interface composed of a thermosetting polymer of 4,4’-diaminodiphenylsulfone-cured bisphenol A diglycidyl ether adhered to a thermoplastic polymer of plasma-treated polyetheretherketone. We observe multiscale phenomena in the adhesion mechanisms, including sub-mm complex interface structure, sub-μm distribution of the functional groups, and molecular-level covalent-bond formation. These results provide a benchmark for further research to examine how physical and chemical states correlate with adhesion, and demonstrate that soft X-ray imaging is a promising approach for visualizing the physical and chemical states at adhesive interfaces from the sub-mm level to the molecular level.

The Evaluation of TiTe2 as a Diffusion Barrier in the Formation of Low Thermal Conductivity Nanolaminates with Bi2Te3 and Sb2Te3

2010 ◽  
Vol 74 ◽  
pp. 38-47
Author(s):  
Clay Mortensen ◽  
Paul Zschack ◽  
David C. Johnson
Keyword(s):  
Thermal Conductivity ◽  
Diffusion Barrier ◽  
Self Assembly ◽  
Low Temperatures ◽  
Annealing Temperature ◽  
The Self ◽  
High Angle ◽  
X Ray Diffraction ◽  
Amorphous Precursor ◽  
X Ray

The evolution of designed [(Ti-Te)]x[(Sb-Te)]y, [(Bi-Te)]x[(Sb-Te)]y, [(Ti-Te)]w[(Bi-Te)]x[(Sb-Te)]y and [(Ti-Te)]w[(Bi-Te)]x[(Ti-Te)]y[(Sb-Te)]z precursors were followed as a function of annealing temperature and time using both low and high angle x-ray diffraction techniques to probe the self assembly into nanolaminate materials. The [(Bi-Te)]x[(Sb-Te)]y precursors were found to interdiffuse at low temperatures to form a (BixSb1-x)2Te3 alloy. The [(Ti-Te)]x[(Bi-Te)]y and [(Ti-Te)]x[(Sb-Te)]y precursors formed ordered nanolaminates [{(TiTe2)}1.35]x[Bi2Te3]y and [{(TiTe2)}1.35]x[Sb2Te3]y respectively. The [(Ti-Te)]w[(Bi-Te)]x[(Sb-Te)]x precursors formed [{(TiTe2)}1.35]w[(Bi0.5Sb0.5)2Te3]2x nanolaminates on annealing, as the bismuth and antimony layers interdiffused. Over the range of TiTe2 thicknesses used in [(Ti-Te)]w[(Bi-Te)]x[(Ti-Te)]y[(Sb-Te)]z precursors, Bi and Sb were found to interdiffuse through the 2-4 nm thick Ti-Te layers, resulting in the formation of (BixSb1-x)2Te3 alloy layers as part of the final nanolaminated products. When the Bi-Te and Sb-Te thicknesses were equal in the amorphous precursors, symmetric [{(TiTe2)}1.35]m[(Bi0.5Sb0.5)2Te3]n nanolamiantes were formed. When the thicknesses of Bi-Te and Sb-Te layers were not equal in the amorphous precursor, asymmetric [(TiTe2)1.35]m[(BixSb1-x)2Te3]n[(TiTe2)1.35]m[(BixSb1-x)2Te3]p nanolaminates were formed. These results imply that to form (A)w(B)x(C)y nanolaminates using designed layered precursors all three components must be immiscible. To form (A)x(B)y(A)x(C)z nanolaminates, the components must be immiscible or the precursor to the A component and the A component itself must be an effective interdiffusion barrier preventing B and C from mixing.

Investigation of the phase shift in X-ray forward diffraction using an X-ray interferometer

1998 ◽  
Vol 5 (3) ◽  
pp. 967-968 ◽  
Author(s):  
Keiichi Hirano ◽  
Atsushi Momose
Keyword(s):  
Phase Shift ◽  
Silicon Crystal ◽  
Dynamical Theory ◽  
Perfect Crystal ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bragg Geometry

The phase shift of forward-diffracted X-rays by a perfect crystal is discussed on the basis of the dynamical theory of X-ray diffraction. By means of a triple Laue-case X-ray interferometer, the phase shift of forward-diffracted X-rays by a silicon crystal in the Bragg geometry was investigated.

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