研究目的
To develop a simple synthesis method for Cu2O and CuO nanocrystals and apply them to H2S gas sensing, with a focus on improving stability through Pd loading.
研究成果
Cu2O and CuO nanocrystals were successfully synthesized using a simple hot-soap method and air oxidation. Pd loading improved sensor stability by facilitating oxygen reaction with H2S and suppressing irreversible sulfide formation. The Pd-loaded sensors exhibited reproducible responses at elevated temperatures (200-250°C), with good sensitivity to dilute H2S. Future work could involve deposition on other semiconductors to enhance performance.
研究不足
The Cu2O NC sensor showed poor stability due to irreversible formation of Cu2S with H2S at low temperatures (50-150°C). Recovery was slow at lower temperatures, and higher operating temperatures (200-250°C) were needed for stable performance, which may limit practical applications. Aggregation of nanocrystals in toluene was observed, and sensor response time was relatively long (e.g., 20 minutes for 90% response).
1：Experimental Design and Method Selection:
The study used a hot-soap method (heating-up method) to synthesize monodispersed Cu2O and CuO nanocrystals, followed by air oxidation for phase conversion. Gas sensing properties were evaluated using resistive-type sensors fabricated by spin coating.
2：Sample Selection and Data Sources:
Copper(II) acetylacetonate and 1,8-octanediol were used as precursors in oleylamine solvent. Pd nanocrystals were synthesized separately. Gas sensing tests used H2S in air at concentrations of 1-8 ppm.
3：List of Experimental Equipment and Materials:
Equipment includes X-ray diffractometer (MiniFlex600), TEM (JEM-2000X), DLS spectrophotometer (Zetasizer Nano ZS), FT-IR spectrometer (FTIR4100), UV-vis spectrometer (V-650), mass flow controllers (SEC-series), multimeter (2701), spin coater, and electric furnace. Materials include Cu(acac)2, oleylamine, 1,8-octanediol, Pd acetate, trioctylphosphine, Au paste (AU-176010), alumina substrates, toluene, hexane, isopropanol.
4：Experimental Procedures and Operational Workflow:
Synthesis involved heating precursors at 160°C under Ar flow, washing with solvents, and air oxidation for CuO. Sensor fabrication involved screen-printing Au electrodes, spin coating nanocrystal suspensions, and heat treatment for ligand removal. Sensing measurements were conducted at 50-250°C with gas flow controlled by mass flow controllers, and electrical resistance was measured.
5：Data Analysis Methods:
XRD for crystallite size (Scherrer's equation), DLS and TEM for particle size, UV-vis for band gap (Tauc plots), FT-IR for ligand presence, and sensor response defined as Rg/Ra.
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X-ray diffractometer
MiniFlex600
Rigaku
Used for X-ray diffraction analysis to determine crystallite size and phase identification of nanocrystals.
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Transmission electron microscope
JEM-2000X
JEOL
Used for imaging and size analysis of nanocrystals.
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Dynamic light scattering spectrophotometer
Zetasizer Nano ZS
Malvern Instruments
Used to measure colloidal size distribution of nanocrystals in solution.
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FT-IR spectrometer
FTIR4100
JASCO
Used for Fourier transform-infrared spectroscopy to detect surface ligands on nanocrystals.
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UV-vis spectrometer
V-650
JASCO
Used for ultraviolet-visible absorbance spectroscopy to analyze band gaps of nanocrystals.
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Multimeter
2701
KEITHLEY
Used to measure electrical resistance of sensor devices under applied voltage.
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Mass flow controller
SEC-series
HORIBA STEC
Used to control flow rates of gases during sensing measurements.
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Au paste
AU-176010
Nilaco
Used for screen-printing Au microelectrodes on alumina substrates.
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