Facile Conversion of Red Phosphorus into Soluble Polyphosphide Anions by Reaction with Potassium Ethoxide

Dragulescu‐Andrasi, Alina; Miller, L. Zane; Chen, Banghao; McQuade, D. Tyler; Shatruk, Michael

doi:10.1002/ange.201511186

Cited by 14 publications

(12 citation statements)

References 34 publications

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“…There are already many examples for the activation of P white by nucleophilic reagents . Recently, nucleophilic loosening of P–P bonds has also been observed with P red in different organic solvents . Because a decreased reaction rate was observed while lowering the nucleophilicity of the anion, it was assumed that a comparable mechanism might play a role during this synthesis.…”

Section: Resultsmentioning

confidence: 73%

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu_3–xP

Wolff¹,

Pallmann²,

Boucher³

et al. 2016

Inorg. Chem.

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Polycrystalline Cu3-xP was successfully synthesized in different ionic liquids comprising imidazolium and phosphonium cations. The reaction of elemental copper and red phosphorus in trihexyltetradecylphosphonium chloride at 200 °C led to single-phase Cu3-xP (x = 0.05) within 24 h with a quantitative yield (99%). Liquid-state nuclear magnetic resonance spectroscopy of the ionic liquids revealed degeneration of the imidazolium cations under the synthesis conditions, while phosphonium cations remain stable. The solid products were characterized with X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, solid-state nuclear magnetic resonance spectroscopy, and elemental analysis. A reinvestigation of the electronic transport properties of Cu2.95(4)P showed metallic behavior for the bulk material. The formation of CuP2 during the synthesis of phosphorus-rich Cu3-xP (x ≥ 0.1) was observed.

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Section: Resultsmentioning

confidence: 73%

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu_3–xP

Wolff¹,

Pallmann²,

Boucher³

et al. 2016

Inorg. Chem.

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“…Figure 1a schematizes the synthesis of the polyphosphide precursor solution and solution-based fabrication of fibrous phosphorus thin films. For initial polyphosphide-precursor synthesis, the reported chemical route 29 was modified, wherein amorphous red phosphorus reacted with potassium ethoxide to produce potassium mixtures of polyphosphide powder. To eliminate any possible unreacted precursors and byproducts, the as-synthesized polyphosphide powder was further purified by dispersing it in ethanol and removing the insoluble precipitates.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…The polyphosphide precursors were synthesized according to the published literature with slight modifications. 29 All manipulations for the synthesis of the initial polyphosphide precursors were performed under inert N 2 atmosphere by standard Schlenk techniques or in N 2 filled glovebox. At first, 3.2 mmol of KOEt and P red were added in a 100 mL three-neck roundbottom flask.…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

Polyphosphide Precursor for Low-Temperature Solution-Processed Fibrous Phosphorus Thin Films

Ban

et al. 2019

Chem. Mater.

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Crystalline red phosphorus has very recently emerged as a stable and cost-effective semiconductor material. However, despite its potentiality in electronics and optoelectronics, the widespread application of this material is still hampered by the limited synthetic route of the ampoule-based chemical vapor deposition that critically requires mineralizing agents. To address this issue, we report the chemical synthesis of soluble polyphosphide precursors that serve as inks for the solutionprocessed fabrication of crystalline fibrous phosphorus thin films. The purified polyphosphide precursor formed crystalline fibrous phosphorus via thermal annealing at a temperature as low as 250 °C without any mineralizing agents. This anionic polyphosphide functioned as a surface-capping ligand for nanoparticles including metals, semiconductors, and magnets. Therefore, the study investigates the possibility of solution-processed fibrous phosphorus thin films as active channel layers in fieldeffect transistors as well as photodetectors and demonstrates their initial performances on the charge-transport and photoresponsive characteristics of these devices. The effect of semiconducting PbS nanoparticles embedded in the fibrous phosphorus thin films on device performance was also studied. The synthesized polyphosphide precursor offers a vast opportunity for the facile preparation of crystalline red phosphorus and chemical design of nanoparticles.

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“…the polyphosphide anion P 16 2− was prepared in the form of (Bu 4 N) 2 P 16. Specific forms of phosphorus clusters, phosphorus or arsenic nanotubes, nanoribbons and phosphorenes were recently reviewed …”

Section: Resultsmentioning

confidence: 99%

Laser ablation synthesis of arsenic–phosphide As_mP_n clusters from As–P mixtures. Laser desorption ionisation with quadrupole ion trap time‐of‐flight mass spectrometry: The mass spectrometer as a synthesizer

Kubáček

Prokeš

Pamreddy

et al. 2018

Rapid Comm Mass Spectrometry

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Facile Conversion of Red Phosphorus into Soluble Polyphosphide Anions by Reaction with Potassium Ethoxide

Cited by 14 publications

References 34 publications

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu_3–xP

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu_3–xP

Polyphosphide Precursor for Low-Temperature Solution-Processed Fibrous Phosphorus Thin Films

Laser ablation synthesis of arsenic–phosphide As_mP_n clusters from As–P mixtures. Laser desorption ionisation with quadrupole ion trap time‐of‐flight mass spectrometry: The mass spectrometer as a synthesizer

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Facile Conversion of Red Phosphorus into Soluble Polyphosphide Anions by Reaction with Potassium Ethoxide

Cited by 14 publications

References 34 publications

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu3–xP

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu3–xP

Polyphosphide Precursor for Low-Temperature Solution-Processed Fibrous Phosphorus Thin Films

Laser ablation synthesis of arsenic–phosphide AsmPn clusters from As–P mixtures. Laser desorption ionisation with quadrupole ion trap time‐of‐flight mass spectrometry: The mass spectrometer as a synthesizer

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Product

Resources

About

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu_3–xP

Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu_3–xP

Laser ablation synthesis of arsenic–phosphide As_mP_n clusters from As–P mixtures. Laser desorption ionisation with quadrupole ion trap time‐of‐flight mass spectrometry: The mass spectrometer as a synthesizer