研究目的
To design and assemble a coordination polymer with noncentrosymmetric structure based on an achiral carboxyphosphinate ligand for potential applications in nonlinear optics and luminescence.
研究成果
The coordination polymer [Mn(HL)2]n exhibits a noncentrosymmetric layered structure with (43)2(46(cid:2)66(cid:2)83) topology, stabilized by C-H…π interactions. It demonstrates SHG activity phase-matchable with an efficiency of 0.8 times urea and luminescence with a red-shifted emission at 457 nm due to intra-ligand transitions. This work provides an example for designing SHG-active materials using asymmetric phosphinate ligands, suggesting future exploration of similar systems for improved nonlinear optical properties.
研究不足
The study is limited to one specific coordination polymer based on manganese and the H2L ligand; it does not explore variations in metal ions or ligands. The SHG efficiency is relatively low (0.8 times that of urea), and the luminescence properties are specific to this compound. Potential optimizations could include testing other reaction conditions or ligands to enhance properties.
1：Experimental Design and Method Selection:
Hydrothermal synthesis was used to react MnSO4 with the achiral 2-carboxyethyl(phenyl)phosphinate ligand (H2L) to form the coordination polymer [Mn(HL)2]n. The method was chosen to facilitate crystal growth under controlled temperature and pressure conditions.
2：Sample Selection and Data Sources:
The samples were synthesized from commercially purchased reagents, including MnSO4 and H2L ligand, without further purification. Data were collected from single-crystal X-ray diffraction, elemental analysis, IR spectroscopy, TGA, PXRD, photoluminescence spectroscopy, and SHG measurements.
3：List of Experimental Equipment and Materials:
Equipment includes a Bruker Apex-II diffractometer for X-ray diffraction, Perkin-Elmer 240 C for elemental analysis, Nicolet 5700 spectrometer for FT-IR, Diamond TG 6000 for TGA, Bruker Advance D8 for PXRD, Perkin Elmer LS55 for photoluminescence, and a Q-switched Nd:YAG laser for SHG measurements. Materials include MnSO4, H2L ligand, distilled water, KBr pellets, and glass boxes for sample packing.
4：Experimental Procedures and Operational Workflow:
A mixture of MnSO4 and H2L in distilled water was sealed in a Teflon-lined autoclave and heated at 120°C for 2 days. After cooling, orange crystals were filtered, washed, and dried. Various characterizations were performed: X-ray diffraction for structure determination, elemental analysis for composition, IR for functional groups, TGA for thermal stability, PXRD for phase purity, photoluminescence for emission properties, and SHG for nonlinear optical response using sieved particle sizes.
5：Data Analysis Methods:
Data were analyzed using software such as SAINT and SADABS for X-ray data reduction, SHELXS and SHELXL for structure solution and refinement. Statistical analysis was not explicitly mentioned; results were interpreted based on experimental measurements and comparisons with standards like urea for SHG.
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Bruker Apex-II diffractometer
Apex-II
Bruker
Used for X-ray single crystal diffraction data collection.
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Perkin-Elmer 240 C instrument
240 C
Perkin-Elmer
Used for elemental analysis.
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Bruker Advance D8 diffractometer
Advance D8
Bruker
Used for powder X-ray diffraction pattern collection.
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Perkin Elmer LS55 fluorescence spectrometer
LS55
Perkin Elmer
Used for photoluminescence analysis.
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Nicolet 5700 spectrometer
5700
Nicolet
Used for FT-IR spectrum recording with KBr pellets.
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Diamond TG 6000 unit
TG 6000
Diamond
Used for thermogravimetric analysis.
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Q-switched Nd:YAG solid-state laser
Used to generate 1064 nm radiation for SHG measurements.
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photmultiplier tube
Used to detect second harmonic radiation in SHG measurements.
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oscilloscope
Used to display detected signals in SHG measurements.
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Teflon-lined autoclave
Used for hydrothermal synthesis reactions.
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