研究目的
Investigating the formation of highly ordered and nanostructured hexagonal boron nitride (h-BN) at reduced temperatures using molten salt synthesis to overcome the high-temperature requirements of conventional methods.
研究成果
Highly ordered and nanostructured h-BN was successfully synthesized at 1000 °C using molten salt synthesis with a H3BO3:NH4Cl molar ratio of 1:2 and a dwell time of 3 hours. The molten salt facilitates BN formation by decomposing reactants and enhancing layer mobility. This method reduces the synthesis temperature compared to conventional methods, offering a cost-effective approach for h-BN production with potential applications in electronics and thermal management.
研究不足
The synthesis requires specific salt mixtures and controlled atmospheres, which may limit scalability. The presence of oxygen impurities (around 3.2 wt%) could affect material properties. The reaction mechanism is proposed based on observations and literature, but not fully validated experimentally.
1:Experimental Design and Method Selection:
The study employed molten salt synthesis (MSS) to synthesize h-BN at lower temperatures. The rationale was to use a eutectic NaCl-KCl salt mixture to promote reaction kinetics and mass transfer. Theoretical models included thermodynamic and kinetic considerations for reaction mechanisms.
2:Sample Selection and Data Sources:
Reactants were boric acid (H3BO3) and ammonium chloride (NH4Cl) with molar ratios varied from 2:1 to 1:
3:The salt mixture was NaCl-KCl in a
1 molar ratio. Samples were prepared by mixing powders and heat-treating in a nitrogen atmosphere.
4:List of Experimental Equipment and Materials:
Equipment included a tube furnace (Model 1000K, CM Furnaces), X-ray diffractometer (PANalytical X'Pert Diffractometer), FTIR spectrometer (Mattson Instruments Galaxy 5000), FE-SEM (Zeiss-Sigma), EDS detector (Oxford-XmaX80), and TEM (FEI Tecnai G2 F20). Materials included H3BO3 (purity >99.9%, U.S. Borax, Inc.), NH4Cl (purity >99%, Fisher Scientific), NaCl, KCl, methanol, and alumina crucibles.
5:0). Materials included H3BO3 (purity >9%, U.S. Borax, Inc.), NH4Cl (purity >99%, Fisher Scientific), NaCl, KCl, methanol, and alumina crucibles. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Reactant and salt mixtures were layered in an alumina crucible and heated in a tube furnace under nitrogen flow at 10 °C/min to temperatures of 800-1000 °C with dwell times of 1-6 hours. After cooling, products were washed with hot deionized water, filtered, and dried at 110 °C for characterization.
6:Data Analysis Methods:
XRD was used for phase identification, crystallinity, and crystallite size calculation using the Scherrer equation. FTIR identified chemical bonds. SEM and TEM analyzed morphology and microstructure. EDS provided elemental composition.
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X-ray Diffractometer
X'Pert Diffractometer
PANalytical
Phase identification, crystallinity analysis, and crystallite size calculation
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FE-SEM
Sigma
Zeiss
Observation of particle size and morphology
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EDS Detector
XmaX80
Oxford
Elemental composition analysis
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TEM
Tecnai G2 F20 Super-Twin FE-TEM
FEI
Morphology, crystal structure, and lattice distance analysis
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Tube Furnace
1000K
CM Furnaces
Heating samples to high temperatures under controlled atmosphere for synthesis
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FTIR Spectrometer
Galaxy 5000 series
Mattson Instruments
Identification of chemical bonding characteristics
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Boric Acid
U.S. Borax, Inc.
Boron source in reactant mixture
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Ammonium Chloride
Fisher Scientific
Nitrogen source in reactant mixture
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Commercial h-BN
BN150
Kennametal
Reference material for comparison
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