研究目的
To develop a general synthesis method for phase-pure 2D Ruddlesden-Popper hybrid perovskite halides from a dynamic equilibrium, enabling controlled and discriminating synthesis for all compositions within the homologous series.
研究成果
A synthetic approach using a solvent-antisolvent pair to induce a controlled dynamic equilibrium for precipitation is presented for obtaining phase-pure Ruddlesden-Popper type hybrid organic-inorganic perovskite halides. The method is applicable to various bulky organic cations and allows for the rapid discovery of new 2D HOIPs and Ruddlesden-Popper phases.
研究不足
The synthesis requires precise control over reagent concentrations and solvent-antisolvent ratios to achieve phase purity. The method may be limited by the solubility of the n = 1 member of the series and the potential for co-precipitation of impurity phases such as PbI2.
1:Experimental Design and Method Selection:
The synthesis involves preparing a solution of Pb2+ in aqueous HI, adding reagents in stoichiometric amounts for the desired phase, establishing a dynamic equilibrium between an initial precipitate and solute cations, and adding acetic acid as an antisolvent to lower the molar solubility of the target higher n-member.
2:Sample Selection and Data Sources:
Samples were prepared using PbO, methylammonium chloride, and various bulky ammonium cations (n-butylammonium, iso-butylammonium, benzylammonium) in stabilized HI (57 wt% in H2O, <
3:5% H3PO2). List of Experimental Equipment and Materials:
Bruker D8 Discover DaVinci Powder X-ray Diffractometer, Bruker D8 Quest ECO diffractometer for SCXRD, Agilent (Cary) 500 Scan UV-Vis-NIR spectrophotometer, NexION 350D mass spectrometer for ICP-MS.
4:Experimental Procedures and Operational Workflow:
Detailed synthesis procedures for each compound are provided, including the addition of reagents, stirring, filtering, washing, and drying.
5:Data Analysis Methods:
Powder X-ray diffraction for phase purity confirmation, single crystal X-ray diffraction for structural determination, ICP-MS for molar solubility studies, photoluminescence and absorbance spectra for optical properties.
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