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1.
J Mass Spectrom ; 56(8): e4771, 2021 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-34251720

RESUMO

Direct current glow discharge mass spectrometry with an indium-based secondary cathode technique is used to analyze solid, nonconducting, fused high-purity quartz regarding metallic impurities of relevance to the solar industry. Details of the analytical routines are presented. In this work, the secondary cathode design and glow discharge conditions are optimized beyond the commonly applied practices. In addition, relative sensitivity factors (RSFs) for these optimized conditions are established and compared to previously published results. The results indicate that the technique enables stable measurements with detection limits down to the part per billion (ppb) range.

2.
RSC Adv ; 10(48): 29018-29030, 2020 Aug 03.
Artigo em Inglês | MEDLINE | ID: mdl-35520046

RESUMO

Fused silica crucibles are commonly used in the fabrication process of solar grade silicon ingots. These crucibles are manufactured from high purity natural quartz sand and as a consequence, their properties are influenced by the presence of water and hydroxyls in the raw quartz. In this work, diffuse reflectance IR, 1H magic angle spinning NMR, and Raman spectroscopy were used to investigate the influence of thermal treatment on water and hydroxyl groups in high purity natural quartz sand. Most of the water in dry sand is present in the form of closed inclusions within the quartz grains which were detected in Raman imaging studies, even after thermally treating the samples at 600 °C. Only after heating to 900 °C did this water completely vanish, most likely as a result of rupturing of the inclusions. However, newly formed OH groups, identified as isolated and hydrogen bound OH were observed as products of the reaction between water and quartz. Similarly, liquid water was observed in NMR spectra even after treatment at 600 °C while at temperatures >900 °C, only non-interacting silanol groups were present. The comparison of the temperature dependence of the IR and NMR spectra also yields insight into the assignment of the OH stretching mode region of the IR spectrum in this system. The intensity of water related bands decreases while the intensity of OH bands first increases and then decreases with increasing temperature. The band intensity of Al-rich defects as well as the characteristic feature at 3200 cm-1 does not follow the temperature dependence of typical water peaks. It is also shown that leaching the quartz sand in HF solution helps to remove water from inclusions, likely by forming pathways for fluid flow inside the quartz grains. Milling of the samples caused formation of an additional type of hydroxyl group, possibly due to partial amorphisation of the surfaces of the quartz grains surface during the process. The results improve the basis for a knowledge-based processes development for the processing of high purity natural quartz.

3.
Artigo em Inglês | MEDLINE | ID: mdl-25274523

RESUMO

The orientation relations (ORs) of the cubic icosahedral quasicrystal approximant phase α-Al(Fe,Mn)Si have been studied after low temperature annealing of a 3xxx wrought aluminium alloy by transmission electron microscopy. From diffraction studies it was verified that the most commonly observed OR for the α-Al(Fe,Mn)Si dispersoids is [1\bar 11]α // [1\bar 11]Al, (5\bar 2\bar 7)α // (011)Al. This orientation could be explained by assuming that the internal Mackay icosahedron (MI) in the α-phase has a fixed orientation in relation to Al, similar to that of the icosahedral quasi-crystals existing in this alloy system. It is shown that mirroring of the normal-to-high-symmetry icosahedral directions of the MI explains the alternative orientations, which are therefore likely to be caused by twinning of the fixed MI. Only one exception was found, which was related to the Bergman icosahedron internal to the T-phase of the Al-Mg-Zn system.

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