研究目的
Investigating the growth of β-phase NaYF4:Yb3+,Er3+ upconversion nanoparticles synthesized by the thermal decomposition method using a combination of in situ and offline analytical methods for determining the application-relevant optical properties, size, crystal phase, and chemical composition.
研究成果
The study demonstrates the potential of in situ luminescence spectroscopy for real-time quality control of UCNP synthesis, enabling the optimization of the reaction time required for completion of the formation of ?-phase UCNPs. The good correlation of optical and sizing techniques underlines the capability of in situ measurements for the online control of UCNP synthesis and the reaction progress as well as UCNP quality.
研究不足
The study focuses on the synthesis of β-phase NaYF4:Yb3+,Er3+ upconversion nanoparticles using the thermal decomposition method. The applicability of the findings to other synthesis methods or nanoparticle systems is not explored. Additionally, the study does not address the scalability of the synthesis process for industrial applications.
1：Experimental Design and Method Selection:
The synthesis was carried out in a mixture of oleic acid and 1-octadecene. The reaction mixture was heated to 300 °C, 315 °C or 325 °C under reflux while applying a gentle flow of argon. The formation of the nanoparticles was allowed to proceed while the upconversion luminescence (UCL) was monitored in situ with a CCD spectrometer.
2：Sample Selection and Data Sources:
Samples were taken from the reaction mixture in regular intervals and subsequently analysed using TEM, SAXS, and luminescence spectroscopy.
3：List of Experimental Equipment and Materials:
Materials included YCl3·6H2O, YbCl3·6H2O, ErCl3·6H2O, oleic acid, NaOH, 1-octadecene, NH4F, chloroform, cyclohexane, acetone, and ethanol. Equipment included a Philips CM200 LaB6 microscope for TEM, a four-crystal monochromator (FCM) beamline for SAXS, and an Ocean Optics CCD spectrometer QE65000 for in situ luminescence measurements.
4：Experimental Procedures and Operational Workflow:
The synthesis involved heating the reaction mixture to remove methanol, then heating to the reaction temperature under argon flow. Samples were taken periodically, and the reaction was monitored until completion.
5：Data Analysis Methods:
The size distribution was derived from TEM data measuring the diameter of single nanoparticles. SAXS data were interpreted in terms of least-squares fitting of a model function describing spherical particles with a Gaussian size distribution.
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