Crystallized Rubber

1932 ◽  
Vol 5 (3) ◽  
pp. 245-248
Author(s):  
R. Pummerer ◽  
G. von Susich

Abstract In recent years various attempts have been made to crystallize natural rubber by some means other than by stretching. In the present paper the results of these experiments are described, together with some new observations, in order to settle the present status of the problem. The processes of crystallization are divided into three groups and discussed individually. 1. Spontaneous crystallization under conditions which vary but little from the normal conditions. 2. Crystallization from solution after purification. 3. Crystallization of a solution of purified rubber by cooling to a low temperature. It is a generally known fact that after storage for a year, plantation rubber becomes stiff, inelastic, and opaque. A rubber altered in this way is known as “frozen” rubber, because this change has been observed most frequently after storage in a cold place. The x-ray investigations of Katz and Bing have rendered it certain that during “freezing” there is crystallization of the rubber, because when subjected to x-rays frozen rubber shows crystalline interferences from which the same crystal lattice is calculated as that which is formed on stretching, except that the degree of orientation in frozen rubber differs from that of stretched rubber. This is seen in x-ray diagrams, where the nearly point interferences of the stretched samples lie on the same Debye-Scherrer circles as those of frozen rubber. There have been rather exhaustive investigations on those changes in frozen rubber which appear on warming, viz., during transformation of the crystalline to the amorphous state (the “fusion process”), and which are characterized by disappearance of the crystal interferences and by a discontinuous change in the heat content, specific gravity, hardness, and light absorption.

1955 ◽  
Vol 28 (3) ◽  
pp. 728-731 ◽  
Author(s):  
V. I. Kasatochkin ◽  
B. V. Lukin

Abstract The x-ray diffraction pattern of amorphous rubber, which is an amorphous ring, resembles the pattern of low-molecular liquids. In our previous work, it was established that the diffraction pattern observed is due to the coherent scattering of only those segments of the molecular chains in which the aggregation is analogous to that of low-molecular liquids, and is determined by the presence of a pseudo-order. A large part of the links of the molecular chains, owing to the prevailing disorder, scatters the x-rays incoherently, like scattering by a gas. For one component of amorphous rubber, the concept of “liquid phase” was introduced, and, for the other, that of “gaseous phase”, thereby subdividing them according to the type of scattering of x-rays. Amorphous rubber, according to our data, contains a large number of chair segments which are characterized by a high degree of disorder. The presence of such a disordered molecular phase is a general and characteristic property of high-molecular substances, and is caused by natural obstacles in the dense packing of the large molecules. This characteristic of molecular aggregation is undoubtedly reflected in the physical-mechanical properties of polymers.


1939 ◽  
Vol 12 (1) ◽  
pp. 18-30 ◽  
Author(s):  
W. Harold Smith ◽  
Charles Proffer Saylor

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.


1997 ◽  
Vol 53 (1) ◽  
pp. 135-142 ◽  
Author(s):  
D. L. Corker ◽  
A. M. Glazer ◽  
J. Dec ◽  
K. Roleder ◽  
R. W. Whatmore

The crystal structure of the perovskite lead zirconate PbZrO3 has been redetermined using single-crystal X-ray diffraction (Mo Kα radiation, λ = 0.71069 Å). Single-crystal data at 100 K: space group. Pbam, a = 5.884 (1), b = 11.787 (3), c = 8.231 (2) Å, V = 570.85 Å3 with Z = 8, μ = 612.6 cm−1, D x = 8.06 Mg m−3, F(000) = 1168, final R = 0.033, wR = 0.061 over 555 reflections with I > 2σ(I). An investigation is made into previous contradicting reports of a possible disorder in the O atoms and their origin by examining the crystal pseudo-symmetry. Information distinguishing an ordered and disordered oxygen substructure is shown to reside in weak l odd reflections. Because of their extremely low intensities these reflections have not contributed sufficiently in previous X-ray structure investigations and hence, to date, conclusive evidence differentiating between ordered and disordered models has not been possible. By collecting single-crystal X-ray data at low temperature and by using exceptionally long scans on selected hkl, l odd, reflections, a new accurate structure determination is presented and discussed, showing the true ordered oxygen positions. Because of the large difference in scattering factors between lead and oxygen when using X-rays, a neutron diffraction Rietveld refinement using polycrystalline samples (D1A instrument, ILL, λ = 1.90788 Å) is also reported as further evidence to support the true ordered oxygen structure revealed by the low-temperature X-ray analysis.


Author(s):  
D. Chambellan ◽  
O. Gal ◽  
S. Legoupil ◽  
A. Vabre

X-rays techniques are widely used in the non-destructive evaluation field for mechanical inspection. However, development of new x-ray detectors and sources over the last decade has let to an intensive use of this technique in other fields. In this paper, we describe the use of X-rays techniques in the field of fluid flow engineering (fluidics and heat transfer). This technique is very attractive since measurements can be performed even if pressure, temperature require the use of opaque walls. In addition the X-ray technique is well suited to multiphase flows where optical technique can not be used if void fraction is larger than few percents. Specific gravity, mass or void fraction are the main accessible parameters.


2020 ◽  
Vol 1 (2) ◽  
pp. 167-176 ◽  
Author(s):  
Ahmad R. Kirmani ◽  
Emily F. Roe ◽  
Christopher M. Stafford ◽  
Lee J. Richter

Process-structure-transport relationships in low-temperature-processed, blade-coated In2O3 transistors using sol–gel and combustion chemistries are explored with X-ray scattering techniques. Electron mobility of ≈4.5 cm2 V−1 s−1 is achieved at ≈220 °C.


2021 ◽  
Vol 22 (2) ◽  
pp. 307-312
Author(s):  
B.K. Ostafiychuk ◽  
V.V. Moklyak ◽  
V.D. Fedoriv ◽  
A.B. Hrubiak ◽  
Yu.V. Yavorskyi ◽  
...  

In article present the results of low-temperature Mossbauer studies of iron (III) oxide/hydroxide nanocomposite synthesized by the method of deposition. Based on these studies, the composition of the synthesized composite was revealed. The nanodispersed composite with a specific surface 280 m2/g is a hematite in the weakly disordered crystalline state (CSR 10 nm), and a lepidocrocite in the X-ray amorphous state (particles size 3-4 nm). The relative integral intensity of the Zeeman sextet, which corresponds to the magnetically ordered phase of hematite, is practically unchanged and is about 17%. The tendency to divide the magnetically ordered component into two sextets, which differ in quadrupole splitting QS= –0.21 mm/s and QS= 0.21 mm/s, respectively, is observed starting from a temperature of 190 K. As a result of annealing of the synthesized material at a temperature of 200°C, a slight redistribution (≈ 5%) of the content of paramagnetic and magnetically ordered components was recorded, which indicates the structural stability of the nanoparticles of the lepidocrocite γ-FeOOH phase at this temperature. Increase of  annealing temperatures to 500oC leads to the predicted course of the phase transition γ-FеООH ® α-Fе2О3. The mechanism of growth of hematite crystallites during sintering due to fixation side faces of larger α-Fe2O3 phase of nanoparticles of the γ-FeOOH phase with simultaneous transformation of their crystal structure to side faces of larger α-Fe2O3 phase particles is presented.


1994 ◽  
Vol 144 ◽  
pp. 82
Author(s):  
E. Hildner

AbstractOver the last twenty years, orbiting coronagraphs have vastly increased the amount of observational material for the whitelight corona. Spanning almost two solar cycles, and augmented by ground-based K-coronameter, emission-line, and eclipse observations, these data allow us to assess,inter alia: the typical and atypical behavior of the corona; how the corona evolves on time scales from minutes to a decade; and (in some respects) the relation between photospheric, coronal, and interplanetary features. This talk will review recent results on these three topics. A remark or two will attempt to relate the whitelight corona between 1.5 and 6 R⊙to the corona seen at lower altitudes in soft X-rays (e.g., with Yohkoh). The whitelight emission depends only on integrated electron density independent of temperature, whereas the soft X-ray emission depends upon the integral of electron density squared times a temperature function. The properties of coronal mass ejections (CMEs) will be reviewed briefly and their relationships to other solar and interplanetary phenomena will be noted.


Author(s):  
R. H. Duff

A material irradiated with electrons emits x-rays having energies characteristic of the elements present. Chemical combination between elements results in a small shift of the peak energies of these characteristic x-rays because chemical bonds between different elements have different energies. The energy differences of the characteristic x-rays resulting from valence electron transitions can be used to identify the chemical species present and to obtain information about the chemical bond itself. Although these peak-energy shifts have been well known for a number of years, their use for chemical-species identification in small volumes of material was not realized until the development of the electron microprobe.


Author(s):  
E. A. Kenik ◽  
J. Bentley

Cliff and Lorimer (1) have proposed a simple approach to thin foil x-ray analy sis based on the ratio of x-ray peak intensities. However, there are several experimental pitfalls which must be recognized in obtaining the desired x-ray intensities. Undesirable x-ray induced fluorescence of the specimen can result from various mechanisms and leads to x-ray intensities not characteristic of electron excitation and further results in incorrect intensity ratios.In measuring the x-ray intensity ratio for NiAl as a function of foil thickness, Zaluzec and Fraser (2) found the ratio was not constant for thicknesses where absorption could be neglected. They demonstrated that this effect originated from x-ray induced fluorescence by blocking the beam with lead foil. The primary x-rays arise in the illumination system and result in varying intensity ratios and a finite x-ray spectrum even when the specimen is not intercepting the electron beam, an ‘in-hole’ spectrum. We have developed a second technique for detecting x-ray induced fluorescence based on the magnitude of the ‘in-hole’ spectrum with different filament emission currents and condenser apertures.


Author(s):  
S. Edith Taylor ◽  
Patrick Echlin ◽  
May McKoon ◽  
Thomas L. Hayes

Low temperature x-ray microanalysis (LTXM) of solid biological materials has been documented for Lemna minor L. root tips. This discussion will be limited to a demonstration of LTXM for measuring relative elemental distributions of P,S,Cl and K species within whole cells of tobacco leaves.Mature Wisconsin-38 tobacco was grown in the greenhouse at the University of California, Berkeley and picked daily from the mid-stalk position (leaf #9). The tissue was excised from the right of the mid rib and rapidly frozen in liquid nitrogen slush. It was then placed into an Amray biochamber and maintained at 103K. Fracture faces of the tissue were prepared and carbon-coated in the biochamber. The prepared sample was transferred from the biochamber to the Amray 1000A SEM equipped with a cold stage to maintain low temperatures at 103K. Analyses were performed using a tungsten source with accelerating voltages of 17.5 to 20 KV and beam currents from 1-2nA.


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