研究目的
To synthesize high-purity single crystals of the sodium molybdenum bronzes NaxMoO3 through high pressure solid-state reaction routes.
研究成果
The results indicate a potential new route not only for preparing alkali molybdenum bronze crystals through solid-state reaction under high pressure and high-temperature condition but also for other bronze materials.
研究不足
The crystal sizes in the final run products are limited to the range of 1–25 μm owning to the widespread nucleation within the sample volume.
1：Experimental Design and Method Selection:
The method is based on a high pressure solid-state reaction between varying phases of sodium molybdate (Na2MoO4), boron (B), and boron oxide (B2O3).
2：3). Sample Selection and Data Sources:
2. Sample Selection and Data Sources: High-purity Na2MoO4·2H2O, B2O3, and B were used as the starting powders.
3：List of Experimental Equipment and Materials:
Multi-anvil apparatus (YL-800t), X-ray diffractometry (X’pert Pro), optical microscope, X-ray photoelectron spectroscopy (XPS, XSAM800).
4：0). Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: The powders were wet grounded, compacted into green bodies, placed in a capsule made of NaCl, and then contained in a pyrophyllite high pressure cell. The cell was compressed to a predetermined pressure, heated to a set temperature, maintained for 10–60 min, quenched to room temperature, and then slowly decompressed to ambient pressure.
5：Data Analysis Methods:
The phase compositions were determined by X-ray diffractometry, and the microstructures were analyzed using an optical microscope. The chemical compositions were determined by X-ray photoelectron spectroscopy.
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Na2MoO4·2H2O
Alddin
Starting powder for the synthesis of NaxMoO3 crystals.
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B2O3
Alddin
Starting powder for the synthesis of NaxMoO3 crystals.
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B
～2 μm
Alddin
Starting powder for the synthesis of NaxMoO3 crystals.
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Multi-anvil apparatus
YL-800t
Guilin Guiye Heavy Industries Co. Ltd., China
Used for high pressure synthesis experiments.
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X-ray diffractometry
X’pert Pro
PANalytical, Almelo, the Netherlands
Used to determine the phase compositions of the high pressure sintered samples.
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Optical microscope
Aopu Photoelectric Co., Chongqing, China
Used to analyze the microstructures of the samples.
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X-ray photoelectron spectroscopy
XSAM800
Kratos, Manchester, U.K.
Used to determine the chemical compositions of the samples.
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