研究目的
To synthesize and characterize CdO nanoparticles using a simple and cost-effective thermal decomposition method of a Cd-HMTA precursor complex.
研究成果
Pure, crystalline, and cubic CdO nanoparticles with an average size of 22.7-30.9 nm and mesoporous structure (surface area 58.4 m2/g, pore diameter 4.7 nm) were successfully synthesized. The method is simple, cost-effective, and eco-friendly, and can be extended to other metal oxides.
研究不足
The thermal decomposition pattern is complex with overlapping steps, and the method's robustness and reproducibility may be a concern. The use of a fast heating rate in TGA may cause baseline drift away from equilibrium conditions.
1:Experimental Design and Method Selection:
The study uses thermal decomposition of a precursor complex synthesized from cadmium nitrate and hexamethylenetetramine in ethanol at room temperature, followed by calcination at 500°C for 2 hours to produce CdO nanoparticles. Characterization techniques include elemental analysis, mass spectrometry, FTIR, TGA, XRD, SEM, HRTEM, N2 physisorption, and SAED.
2:Sample Selection and Data Sources:
The precursor is synthesized from analytical grade Cd(NO3)2·6H2O, hexamethylenetetramine, and ethanol obtained from Sigma Aldrich. No further purification is done.
3:List of Experimental Equipment and Materials:
Equipment includes Flash 2000 Thermo Scientific analyzer for elemental analysis, Micro-Mass LCT Premier mass spectrometer for mass spectrometry, PerkinElmer Spectrum Two UATR-FT-IR spectrometer for FTIR, Pyris 6 PerkinElmer TGA 4000 thermal analyzer for TGA, Bruker D8 Advance X-ray diffractometer for XRD, JEOL JSM-7600F field-emission scanning electron microscope for SEM and EDX, JEOL JEM-2100F microscope for TEM and HRTEM, Micromeritics ASAP 2020 instrument for N2 physisorption. Materials include Cd(NO3)2·6H2O, hexamethylenetetramine, ethanol, ceramic crucible, silica gel for desiccation.
4:Experimental Procedures and Operational Workflow:
Precursor synthesis involves dissolving HMTA in ethanol with sonication, adding cadmium nitrate solution dropwise under stirring, filtering and washing the precipitate, and drying. CdO synthesis involves grinding the precursor, calcining in a furnace at 500°C for 2 hours, and cooling. Characterization involves specific procedures for each technique as described.
5:Data Analysis Methods:
Particle size calculated using Debye-Scherrer equation from XRD data, size distribution from TEM images using ImageJ software, surface area and pore size from BET and BJH methods using N2 physisorption data.
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Flash 2000 Thermo Scientific analyzer
Flash 2000
Thermo Scientific
Elemental analysis (C, H, N) of the precursor
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PerkinElmer Spectrum Two UATR-FT-IR spectrometer
Spectrum Two
PerkinElmer
Recording FT-IR spectra from 4000 to 400 cm?1
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Pyris 6 PerkinElmer TGA 4000 thermal analyzer
TGA 4000
PerkinElmer
Thermogravimetric analysis (TGA)
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Bruker D8 Advance X-ray diffractometer
D8 Advance
Bruker
Recording XRD diffractogram using Cu Kα radiation
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JEOL JSM-7600F field-emission scanning electron microscope
JSM-7600F
JEOL
Obtaining SEM images and EDX spectra
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JEOL JEM-2100F microscope
JEM-2100F
JEOL
Transmission electron microscopy (TEM) and high resolution TEM (HRTEM)
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Micro-Mass LCT Premier mass spectrometer
LCT Premier
Waters Corporation
Mass spectrometry of the precursor complex
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Micromeritics ASAP 2020 instrument
ASAP 2020
Micromeritics
N?-physisorption experiment for surface area and pore diameter determination
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ImageJ software
Determining particle size distribution from TEM images
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Cd(NO3)2·6H2O
Sigma Aldrich
Chemical precursor for synthesis
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Hexamethylenetetramine
Sigma Aldrich
Ligand for precursor complex synthesis
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Ethanol
Sigma Aldrich
Solvent for synthesis
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