Tri(pyrazolyl)phosphane als Vorstufen für die Synthese von stark emittierenden InP/ZnS‐Quantenpunkten

Panzer, René; Guhrenz, Chris; Haubold, Danny; Hübner, René; Gaponik, Nikolai; Eychmüller, Alexander; Weigand, Jan J.

doi:10.1002/ange.201705650

Cited by 2 publications

(3 citation statements)

References 45 publications

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“…Due to the high reaction temperatures an alloying process near the interface of the core and shell material shifts the (111) reflexes toward the pure zinc‐containing shell material. This can be explained by a partial migration of zinc ions into the InAs core region, as it is also observed in the synthesis of InP/ZnS QDs . TEM measurements of the resulting spherical InAs/ZnS QDs exhibit an increase in the nanoparticle size compared to the original core particles and confirms additionally the growth of a ZnS protective layer (Figure S4, Supporting Information).…”

Section: Resultssupporting

confidence: 59%

“…In recent years group III–V semiconductor materials gained tremendous attention as less toxic surrogates for group II–VI nanomaterials in optoelectronic devices . Thereby, InAs QDs are one of the most promising candidates for near infrared (NIR) and short‐wave infrared applications, such as bioimaging, photovoltaics, photodetectors, and lasers .…”

Section: Introductionmentioning

confidence: 99%

“…In previous work we introduced tripyrazolylphosphanes (P(pyr) 3 , e.g., pyr = 3,5‐dimethylpyrazole, 2 ) for the convenient preparation of a long term stable (>6 months) P(OLA) 3 stock solution and its application for the synthesis of highly emitting InP/ZnS QDs . Derivatives of P(pyr) 3 are accessible on a multigram scale and represent a safe to handle, less toxic surrogate for cancerogenic hexaalkylphosphorous triamide derivatives such as tris‐dimethylaminophosphane (P(NMe 2 ) 3 ) and tris‐diethylaminophosphane (P(NEt 2 ) 3 ).…”

Section: Introductionmentioning

confidence: 99%

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Synthesis of NIR‐Emitting InAs‐Based Core/Shell Quantum Dots with the Use of Tripyrazolylarsane as Arsenic Precursor

Tietze

Panzer

Starzynski

et al. 2018

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arsenic precursor [2,16] besides the less reactive tris(trimethylgermyl)arsane (As(GeMe 3 ) 3 ) [17] or highly toxic arsine gas (AsH 3 ). [18] Recently, Srivastava et al. [19] and Grigel et al. [20] highlighted tris(dimethylamino)arsane (As(NMe 2 ) 3 ) as commercially available pre cursor for the facile synthesis of InAs QDs. Mechanistically, As(NMe 2 ) 3 undergoes a transamination reaction with the solvent and reagent oleylamine (OLAH) to give trioleyl arsane (As(OLA) 3 ) under the release of three equivalents of flammable dimethylamine. The reaction of As(OLA) 3 with indium(III) chloride (InCl 3 ) to InAs QDs does not proceed without the subsequent addition of a reducing agent for which typically diisobutylaluminum hydride (DIBALH) [19] and nowadays also trioleylphosphane (P(OLA) 3 ) [20] or a N,Ndimethylethylamine com plex (DMEAAlH 3 ) [21] are used. In the case of DIBALH and DMEA AlH 3 , the As-N bonds are cleaved to give in situ (OLA) x AsH 3x species which react with the indium precursor to InAs QDs. [22,23] With the applied concentration of DIBALH the size of InAs QDs can be tuned according to the method by Srivastava et al. [19] By contrast, the approach by Grigel et al. [20] applies in situ generated P(OLA) 3 as reducing agent for the InAs QD synthesis (Scheme 1). This species is known to act both, as a remarkably efficient phos phorus precursor and reducing agent for the preparation of InP QDs. [24][25][26] Grigel et al. [20] pointed out that phase pure InAs QDs are obtained since P(OLA) 3 only provides the electrons required for the reduction of As(OLA) 3 to InAs (Scheme 1).In previous work we introduced tripyrazolylphosphanes (P(pyr) 3 , e.g., pyr = 3,5dimethylpyrazole, 2) for the convenient preparation of a long term stable (>6 months) P(OLA) 3 stock solution and its application for the synthesis of highly emitting InP/ZnS QDs. [5,6] Derivatives of P(pyr) 3 are accessible on a multigram scale and represent a safe to handle, less toxic sur rogate for cancerogenic hexaalkylphosphorous triamide deriva tives such as trisdimethylaminophosphane (P(NMe 2 ) 3 ) and tris diethylaminophosphane (P(NEt 2 ) 3 ). Moreover, the release of cor rosive, flammable, and gaseous dialkylamines (Me 2 NH, Et 2 NH) during the transamination with OLAH is prevented. The released pyrazoles can easily be recovered in high yields (>94%) and reused for the precursor synthesis. The tripyrazolylarsane (As(pyr) 3 , e.g., pyr = 3,5dimethylpyrazole, 1) analogues are envisioned to react similarly, thus, representing a convenient to handle and stable arsenic precursor for the InAs QD synthesis. Tris(3,5-dimethylpyrazolyl)arsane (1) is introduced as a low-cost and convenient to handle arsenic precursor for the straight forward synthesis of InAs quantum dots (QDs). Transamination of 1 with the solvent oleylamine (OLAH) gives trioleylarsane (As(OLA) 3 ) which in the presence of the reducing agents diisobutylaluminum hydride (DIBAL-H) or trioleylphosphane (P(OLA) 3 ) yields InAsQDs via a typical hot injection approach. The size of the obtain...

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Section: Resultssupporting

confidence: 59%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Synthesis of NIR‐Emitting InAs‐Based Core/Shell Quantum Dots with the Use of Tripyrazolylarsane as Arsenic Precursor

Tietze

Panzer

Starzynski

et al. 2018

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Inorganic Solid Phosphorus Precursor of Sodium Phosphaethynolate for Synthesis of Highly Luminescent InP-Based Quantum Dots

Shan²,

Cao

et al. 2021

ACS Energy Lett.

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InP-based quantum dots (QDs) have become the most highlighted candidates to be a less-toxic surrogate for Cd- and Pb-based optoelectronic devices. However, the development of InP QDs still lags due to the expensive and flammable phosphorus precursors. Herein, we introduce sodium phosphaethynolate as an alternative, cheap and low-toxic phosphorus source for the synthesis of highly emitting InP-based QDs. The resulting QDs possess a size-tunable photoluminescence wavelength range between 465 and 620 nm and high emission quantum yield between 43 and 97%. The proof-of-concept QD light-emitting diodes applying the InP-based QDs as an emitter layer exhibit a maximum external quantum efficiency of 1.47%, 6.88%, and 13.62% for blue, green, and red devices, respectively. These results prove the applicability and processability of this new phosphorus in the preparation of high-quality InP-based QDs.

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Tri(pyrazolyl)phosphane als Vorstufen für die Synthese von stark emittierenden InP/ZnS‐Quantenpunkten

Cited by 2 publications

References 45 publications

Synthesis of NIR‐Emitting InAs‐Based Core/Shell Quantum Dots with the Use of Tripyrazolylarsane as Arsenic Precursor

Synthesis of NIR‐Emitting InAs‐Based Core/Shell Quantum Dots with the Use of Tripyrazolylarsane as Arsenic Precursor

Inorganic Solid Phosphorus Precursor of Sodium Phosphaethynolate for Synthesis of Highly Luminescent InP-Based Quantum Dots

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