A new miniature high-pressure diamond anvil cell was designed and constructed using 3D micro laser sintering technology. This is the first application of the use of rapid prototyping technology to construct high-pressure apparatus. The cell is specifically designed for use as an X-ray diffraction cell that can be used with commercially available diffractometers and open-flow cryogenic equipment to collect data at low temperature and high pressure. The cell is constructed from stainless steel 316L and is about 9 mm in diameter and 7 mm in height, giving it both small dimensions and low thermal mass, and it will fit into the cooling envelope of a standard Cryostream cooling system. The cell is clamped using a customized miniature buttress thread of diameter 7 mm and pitch of 0.5 mm enabled by 3D micro laser sintering technology; such dimensions are not attainable using conventional machining. The buttress thread was used as it has favourable uniaxial load properties allowing for higher pressure and better anvil alignment. The clamp can support the load of at least 1.5 kN according to finite element analysis (FEA) simulations. FEA simulations were also used to compare the performance of the standard thread and the buttress thread, and demonstrate that stress is distributed more uniformly in the latter. Rapid prototyping of the pressure cell by the laser sintering resulted in a substantially higher tensile yield strength of the 316L stainless steel (675 MPa compared to 220 MPa for the wrought type of the same material), which increased the upper pressure limit of the cell. The cell is capable of reaching pressures of up to 15 GPa with 600 μm diameter culets of diamond anvils. Sample temperature and pressure changes on cooling were assessed using X-ray diffraction on samples of NaCl and HMT-d.
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Inorg Chem
January 2025
Nikolaev Institute of Inorganic Chemistry, Siberian Branch of the Russian Academy of Science, 630090 Novosibirsk, Russia.
The photoinduced reaction of [Pt(NO)] with pyridine or its derivatives (L) was found to result in the formation of [PtL](NO) salts in high yield. This transformation was successfully probed for methyl- and carboxyethyl-substituted pyridines, and the corresponding [PtL](NO) salts were isolated and fully characterized using single-crystal X-ray diffraction (SCXRD). Anation of the [Pt(py)] cationic complex with N was studied by H NMR spectroscopy in aqueous and water/dimethyl sulfoxide solutions of [Pt(py)](NO).
View Article and Find Full Text PDFDalton Trans
January 2025
Institute of Inorganic Chemistry, Georg-August-Universität Göttingen, Göttingen Tammannstrasse 4, D-37077, Germany.
The reactions of LAlH (L = HC(CMeNAr), Ar = 2,6-PrCH) (1) with diphenylphosphane oxide [PhP(O)H], diphenylphosphinamide [PhP(O)NH], and diaryl/alkyl phosphane [(RO)P(O)H (R = Ph, or Pr)] afford their corresponding compounds with compositions LAl(H)OP(Ph) (2), LAl[OP(Ph)] (3), LAl{[N(H)P(O)(Ph)][OP(Ph)]} (4), LAl(OPr) (5), and LAl(OPh) (6), respectively. These reactions probably undergo a process of dehydrogenation coupling, deaminating dehydrogenation coupling, or chain-breaking coupling. It is noteworthy to mention that the reaction of compound 1 with 2 equiv.
View Article and Find Full Text PDFAcc Chem Res
January 2025
The Wolfson Catalysis Centre, Department of Chemistry, University of Oxford, Oxford OX1 3QR, U.K.
ConspectusThe discovery of reversible hydrogenation using metal-free phosphoborate species in 2006 marked the official advent of frustrated Lewis pair (FLP) chemistry. This breakthrough revolutionized homogeneous catalysis approaches and paved the way for innovative catalytic strategies. The unique reactivity of FLPs is attributed to the Lewis base (LB) and Lewis acid (LA) sites either in spatial separation or in equilibrium, which actively react with molecules.
View Article and Find Full Text PDFDalton Trans
January 2025
Institut für Anorganische und Analytische Chemie, Universität Münster, Corrensstraße 30, 48149 Münster, Germany.
The cadmium-rich intermetallic compounds RhCd ( = Ca, Sr, Y, La-Nd, Sm-Lu) were synthesized from the elements in sealed tantalum tubes. The elements were reacted in an induction furnace and the samples were post-annealed to increase phase purity and crystallinity. The RhCd phases crystallize with the cubic CeCrAl type structure, space group 3̄.
View Article and Find Full Text PDFBiopolymers
March 2025
Guangxi Key Laboratory of Natural Polymer Chemistry and Physics, College of Chemistry and Materials, Nanning Normal University, Nanning, People's Republic of China.
The crosslinked porous corn starch was prepared by two steps: the native corn starch was hydrolyzed by α-amylase and glucoamylase, then the porous corn was crosslinked by sodium trimetaphosphate (STMP). The morphology and size of granules, spherulites, crystal type, molecular structure, swelling properties, thermal stability and adsorption properties of the crosslinked porous starch were investigated. The results indicated that a lot of holes formed in the porous starch, and the particle size of starch granules decreased.
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