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Experiments were carried out to grow 3.Nitroaniline (m.NA) crystals doped with 4.Nitroaniline (p.NA) and 2.chloro 4.Nitroaniline (CNA). The measured undercooling for m.NA, p.NA, and CNA were 0.21 tm K, 0.23 tm K, and 0.35 tm K respectively, where tm represents the melting temperature of the pure component. Because of the crystals' large heat of fusion and large undercooling, it was not possible to grow good quality crystals with low thermal gradients. In the conventional two-zone Bridgman furnace we had to raise the temperature of the hot zone above the decomposition temperature of CNA, p.NA, and m.NA to achieve the desired thermal gradient. To avoid decomposition, we used an unconventional Bridgman furnace. Two immiscible liquids, silicone oil and ethylene glycol, were used to build a special two-zone Bridgman furnace. A temperature gradient of 18 K/cm was achieved without exceeding the decomposition temperature of the crystal. The binary crystals, m.NA-p.NA and m.NA-CNA, were grown in centimeter size in this furnace. X-ray and optical characterization showed good optical quality.
Stromatolites have been a major focus in the search for ancient microbial life, however, the organic carbon biosignatures of dolomitized stromatolites have not yet been fully characterized or correlated with their dolomitizing conditions. Although dolomitization rarely preserves microbial morphology, the presence of organic carbon can provide valuable information for characterization of fossils’ biogenicity, syngenicity, and indigeneity to their host rock. The Cambrian Allentown Formation in New Jersey, USA, is an excellent example of dolomitized stromatolites and thrombolites containing diagenetically modified microbial biosignatures. Based on XRD and EPMA data, the dolomite composition is typically stoichiometric, with varying degrees of cationic ordering. The outcrop underwent early dolomitization in a marginal-marine setting and later burial diagenesis resulting in multi-generational dolomite formation: (1) 2 microspar dolomite formed by early diagenetic replacement at or near the surface, (2) zoned dolomite formed penecontemporaneously with the microspar phase as rhombohedral crystals by infilling primary pore spaces within the microspar matrix. The rhombic crystals continued to grow outward in alternating stages of Fe-enriched and -depleted fluids, which were preserved in zoned rims and revealed by cathodoluminescence, and (3) saddle dolomite formed during late stage deep burial with Fe- and Mn-rich fluids, and occurs as a void-filling, high-temperature phase. Organic carbon, characterized using confocal Raman microscopy, has an exclusive distribution within the microspar dolomite, and the D and G bands’ characteristics reveal similar thermal alteration to the host rock, indicating that the mapped organic carbon is indigenous and syngenetic with the Cambrian carbonates. The findings presented in this study reveal organic matter found within microspar of various dolomitized facies deriving from different source pools of organic carbon. This study sheds light on biosignatures in secondary dolostones and may aid biosignature detection in older carbonate rocks on Earth and Mars.
The Fe 3+ /Fe T ratios (Fe 3+ /[Fe 2+ +Fe 3+ ]) in minerals can be used to understand their crystallization and post-crystallization conditions. However, as natural minerals are often zoned and contain inclusions, bulk techniques, e.g., wet chemistry, may not provide accurate Fe 3+ /Fe T values for a single phase of interest. We determined Fe 3+ /Fe T ratios of amphiboles in different crystallographic orientations by single-crystal synchrotron Mössbauer spectroscopy (SMS) in energy and time domain modes from four volcanic localities (Long Valley Caldera, Mount St. Helens, Lassen Volcanic Center, U.S.A., and Mt. Pinatubo, Philippines). The high spatial resolution (as low as 12 × 12 μm spot size) and standard-free nature of SMS allow the detection of intra-grain compositional heterogeneities in Fe 3+ /Fe T with relatively low uncertainties. Here, we combine SMS with major element compositions, water contents, and hydrogen isotope compositions to document the Fe 3+ /Fe T ratios as a function of mineral composition and post-crystallization dehydrogenation. Spectra were fitted with up to five distinct sites: ferrous iron on M(1), M(2), M(3), and ferric iron on M(2) and M(3), consistent with X-ray diffraction studies on single crystals of amphibole. The Fe 3+ /Fe T ratios range from 0.14 ± 0.03 (Long Valley Caldera), 0.51 to 0.63 ± 0.02 (representing intra-grain heterogeneities, Mount St. Helens) to 0.86 ± 0.03 (Lassen Volcanic Center). The latter grain experienced post-crystallization dehydrogenation, shown by its low water content (0.6 ± 0.05 wt%) and its elevated hydrogen isotope composition (δD = +25 ± 3‰ relative to SMOW). The Fe 3+ /Fe T ratios of 0.62 ± 0.01 and 0.20 ± 0.01 of two Mt. Pinatubo grains correlate with high-Al 2 O 3 cores and low-Al 2 O 3 rims and smaller phenocrysts in the sample, respectively. This study shows that SMS is capable of distinguishing two different domains with dissimilar Fe 3+ /Fe T values formed under different crystallization conditions, demonstrating that SMS in combination with major element, water, and hydrogen isotope compositions allows the interpretation of amphibole Fe 3+ /Fe T ratios in the context of crystallization and post-crystallization processes.
Ge-70 and Ge-74 isotopes were successfully separated from natural Ge, and were zone purified. Several highly enriched, high purity Ge-70 and Ge-74 single crystals were grown by the vertical Bridgman method. The growth system was designed for reliable growth of low dislocation density, high purity Ge single crystals of about 4 g weight. A Ge-70 and a Ge-74 crystal were selected for complete characterization. In spite of the large surface-to-volume ratio of these ingots, both Ge-70 and Ge-74 crystals contain low electrically active chemical net-impurity concentrations of about 2 x 10 exp 12/cu cm, which is 2 orders of magnitude better than that of Ge-74 crystals previously grown by two different groups. Isotopic enrichment of the Ge-70 and the Ge-74 crystals is 96.3 percent and 96.8 percent, respectively. The residual donors and acceptors present in both crystals were identified as phosphorus and copper, respectively. In addition, less than 10 exp 11/cu cm Ga, Al, and In were found in the Ge-70 crystal.
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X-type hexaferrites have been receiving considerable attention due to their promising applications in many magnetic-electronic fields. However, the growth of single-crystal X-type hexaferrite is still a challenge. Herein we reported, for the first time, the preparation of single crystal X-type hexaferrite Sr 2 Co 2 Fe 28 O 46 (Sr 2 Co 2 X) with high-quality and large size using floating-zone method with laser as the heating source. The crystals show rhombohedral symmetry with space group of R-3m (No. 166, a = 5.8935(1) Å and c = 83.7438(17) Å). Co 2+ and Fe 3+ oxidation states were confirmed by the X-ray absorption near-edge spectroscopy. The prepared Sr 2 Co 2 X exhibits a spin reorientation transition from easy-cone to easy-axis at T 2 of 343 K and a ferrimagnetism–paramagnetism transition at Curie temperature (TC) of ~743 K. The spin reorientation transition was accompanied by magnetocaloric effect (MCE). Both conventional and inverse MCEs were observed near T 2 with a magnetic field applied along the c-axis. The maximum value of the magnetic entropy change along the c-axis was evaluated to be 1.1 J/kg·K for a magnetic field change of 5 T.
Despite decades of materials research, the availability of appropriate crystalline radiation-hard scintillators with ultrafast decay times (~10ns) and high light yields (>2000 ph/MeV) are still limited. In this study, we demonstrate the potential of gallium oxide (β-Ga 2 O 3 ) based scintillators for high count rate applications. The low-cost rugged β-Ga 2 O 3 scintillators were grown using the optical float zone (FZ) technique. Several dopants and growth atmospheres were used to demonstrate the balance between ultrafast primary decay time and the light yield of the scintillators. Light yields as high as 6446 ± 716 ph/MeV were obtained with 18.3 ns decay time for 662 keV gamma rays. Decay times as fast as 12ns were obtained with a 3212 ± 357 ph/MeV light yield. An excellent 662 keV gamma energy resolution of 7% was obtained using the β-Ga 2 O 3 :Ce crystals. Even with these excellent scintillation properties, the gamma radiation hardness of β-Ga 2 O 3 crystals was better than the leading radiation-hard lead tungstate (PbWO 4 ) crystals. Twenty-six scintillators fabricated from the grown β-Ga 2 O 3 crystals were tested for radiation hardness with a 60 Co gamma irradiation rate of 14 krad/h with a total radiation dose of 2 Mrad. The scintillation properties of these crystals remained unaffected. To date, no other scintillator has demonstrated such high radiation resistance. Furthermore, these FZ-grown low-cost, non-hygroscopic, and high-density β-Ga 2 O 3 scintillators can replace the existing scintillators in many applications ranging from nuclear and high energy physics experiments to nuclear security.
The dearth of suitable materials significantly restricts the practical development of infrared (IR) laser systems with highly efficient and broadband tuning. Recently, γ-NaAsSe 2 is reported, and it exhibits a large nonlinear second-harmonic generation (SHG) coefficient of 590 pm V —1 at 2 µm. However, the crystal growth of γ-NaAsSe 2 is challenging because it undergoes a phase transition to centrosymmetric δ-NaAsSe 2 . Herein, the stabilization of non-centrosymmetric γ-NaAsSe 2 by doping the As site with Sb, which results in γ-NaAs 0.95 Sb 0.05 Se 2 is reported. The congruent melting behavior is confirmed by differential thermal analysis with a melting temperature of 450 °C and crystallization temperature of 415 °C. Single crystals with dimensions of 3 mm × 2 mm are successfully obtained via zone refining and the Bridgman method. The purification of the material plays a significant role in crystal growth and results in a bandgap of 1.78 eV and thermal conductivity of 0.79 Wm —1 K —1 . The single-crystal SHG coefficient of γ-NaAs 0.95 Sb 0.05 Se 2 exhibits an enormous value of |d 11 | = 648 ± 74 pm V —1 , which is comparable to that of γ-NaAsSe 2 and ≈20× larger than that of AgGaSe 2 . Importantly, the bandgap of γ-NaAs 0.95 Sb 0.05 Se 2 (1.78 eV) is similar to that of AgGaSe 2 , thus rendering it highly attractive as a high-performing nonlinear optical material.
Axisymmetric traveling magnetic fields (TMF) can be beneficial for crystal growth applications. such as the vertical Bridgman, float zone or traveling heater methods. TMF induces a basic flow in the form of a single roll. This type of flow can enhance mass and heat transfer to the growing crystal. More importantly, the TMF Lorentz body force induced in the system can counterbalance the buoyancy forces, so the resulting convection can be much smaller and even the direction of it can be changed. In this presentation, we display basic features of this novel technique. In particular, numerical calculations of the Lorentz force for arbitrary frequencies will be presented along with induced steady-state fluid flow profiles. Also, numerical modeling of the TMF counter-balancing natural convection in vertical Bridgman systems will be demonstrated.
The feasibility and desirability of space growth of bulk IR semiconductor crystals for use as substrates for epitaxial IR detector material were researched. A III-V ternary compound (GaInSb) and a II-VI binary compound were considered. Vapor epitaxy and quaternary epitaxy techniques were found to be sufficient to permit the use of ground based binary III-V crystals for all major device applications. Float zoning of CdTe was found to be a potentially successful approach to obtaining high quality substrate material, but further experiments were required.
Detailed petrologic studies have been made of 15 type IA, Fe-poor, porphyritic olivine chondrules in Semarkona (LL3.0). Major and minor element concentrations in olivines, pyroxenes, and mesostases, and bulk composition so the chondrules are measured along with zoning profiles in the olivine and pyroxene crystals. The mineral compositions and textures are best interpreted in terms of closed system crystallization in which the olivines and pyroxenes crystallized in situ from a melt corresponding to the bulk composition of the chondrule. Relict olivine grains are not found in the chondrules. Crystallization probably occurred at a cooling rate of the order of 1000 C/hr. Precursor materials of the chondrules were composed of two components, one refractory Ca-, Al-, and Ti-rich, and one less refractory Si-, Fe-, Cr-, and Mn-rich. The evidence is consistent with Semarkona being one of the least metamorphosed ordinary chondrites.
PbSnTe single crystals were grown in a new 3 zone furnace. Molecular beam epitaxy (MBE) growth parameters have been established, including beam flux vs. temperature, and growth rates and dopant vs. PbTe flux ratios for the various effusion sources involved. Lattice matching studies were conducted and doping studies were completed. Broad area Pb(1-x)Sn(x)Te double heterostructure lasers were fabricated with active layer compositions up to x equals 0.04 at percent Sn in the active layers. Electrical and optical test data are presented.
An axially traveling magnetic wave induces a meridional basic flow in a molten cylindrical zone. This flow can be beneficial for crystal growth applications. In particular, it can be used to effectively stir the melt in long cylindrical columns. Also, it can beneficially modify the thermal and species concentration fields in the melt and the interface shape of the growing crystal. The basic theory of such an application is developed and preliminary data from a mercury column experiment are also presented.
An axially travelling magnetic wave induces a meridional base flow in an electrically conducting molten cylindrical zone. This flow can be beneficial for crystal growth applications. In particular, it can be effectively used to stir the melt in long cylindrical columns. It can also be tailored to modify the thermal and species concentration fields in the melt and to control the interface shape of the growing crystal. The basic theory of such an application is developed and data from a preliminary mercury column experiment are presented.
An axially traveling magnetic wave induces a meridional base flow in an electrically conducting molten cylindrical zone. This flow can be beneficial for crystal growth applications. In particular, it can be effectively used to stir the melt in long cylindrical columns. It can also be tailored to modify the thermal and species concentration fields in the melt and to control the interface shape of the growing crystal. The basic theory of such an application is developed and data from a preliminary mercury column experiment are presented.