Hot‐Injection Synthesis of PbE (E= S, Se) Nanoparticles from Dichalcogenoimidophosphinato Lead (II) Complexes

Boadi, Nathaniel Owusu; Saah, Selina Ama; Helliwell, Madeleine; Awudza, Johannes A. M.

doi:10.1002/slct.201903649

Cited by 6 publications

(4 citation statements)

References 45 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…e EDAX quantification on the thin films (Figure 6) indicated the formation of PbSe (52%:48%) at all the deposition temperatures. e thin films were lead rich, which is similar to our earlier reports [24,25,34,36,37].…”

Section: Sem Micrographs Of the In Filmssupporting

confidence: 91%

“…Ternary lead sulphide selenide (PbS x Se 1−x ) nanocrystals and thin films [4,[18][19][20] have not been studied extensively relative to PbS and PbSe [21][22][23][24][25][26][27][28]. Nanocrystalline semiconductor alloys give an alternative route to quantum confinement effects and bandgap tuning and thus produce new materials with unique properties [29,30].…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePⁱPr₂)₂N)(S₂CNHexMe)]

Boadi

Saah

Mensah

et al. 2020

Advances in Materials Science and Engineering

Self Cite

View full text Add to dashboard Cite

In this study, [Pb((SePiPr2)2N)(S2CNHexMe)], a novel complex, was synthesised by refluxing [Pb(S2CNHexMe)2] and [Pb((SePiPr2)2N)2] complexes for 2 hours in chloroform and precipitating with methanol. The microelemental analysis, FT-IR, and NMR spectroscopies were performed on the complex and the melting point was determined. The crystal structure of this new compound has been determined. The structure showed a distorted square pyramidal geometry with 2 sulphur and 2 selenium atoms coordinating the central atom at the base of the pyramid and a lone pair occupying the axial position of the lead atom. The complex was used to deposit lead chalcogenide thin films by the aerosol-assisted chemical vapour deposition (AACVD) method at 300, 350, 400, and 450°C. The thin films matched with the powder X-ray diffraction (pXRD) pattern for cubic PbSe with a (200) preferred orientation at all the deposition temperatures. The scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDAX) indicated that cubic PbSe crystals were formed.

show abstract

Section: Sem Micrographs Of the In Filmssupporting

confidence: 91%

Section: Introductionmentioning

confidence: 99%

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePⁱPr₂)₂N)(S₂CNHexMe)]

Boadi

Saah

Mensah

et al. 2020

Advances in Materials Science and Engineering

Self Cite

View full text Add to dashboard Cite

show abstract

“…Lead sulfide semiconductor has a narrow gap [8,13,14], which makes it different from other semiconductors. e bandgap of PbS is affected by temperature and particle size [12,15]. e high sensitivity of the properties of PbS to particle size makes it well suited for nanostructured devices [12].…”

Section: Introductionmentioning

confidence: 99%

Synthesis of a Novel Single-Source Precursor for the Production of Lead Chalcogenide Thin Films

Boadi

Saah

Awudza

2020

Journal of Chemistry

Self Cite

View full text Add to dashboard Cite

A novel complex [Pb((SePiPr2)2N) (S2CNEt2)] has been synthesized and characterized by microelemental analysis, melting point NMR, and FT-IR spectroscopies. Its crystal structure has also been successfully determined using single-crystal X-ray crystallography. The structure indicates a distorted square pyramidal geometry with the four basal atoms being noncoplanar. The complex was used as a single-source precursor for the deposition of lead chalcogenide thin films on glass substrates at 300, 350, 400, and 450°C by AACVD. The films were characterized by SEM, EDX, and XRD. The XRD peaks matched with cubic PbSe at all temperatures. The SEM micrographs showed the formation of cubes with the lower temperatures (300–350°C) showing well-resolved cubes while with the higher temperatures (400–450°C) showing poorly resolved cubes. The EDX analyses confirmed the formation of PbSe thin films at all the deposition temperatures.

show abstract

“…A search of the Cambridge Structural Database (CSD) showed that although imidodiphosphinate ligands with S 2 - and Se 2 -donor atom sets are well studied, there are comparatively a few reported structures of mixed Se/S donor imidodiphosphinate ligands. The bis((diisopropylthiophosphoryl)(diisopropylselenophosphoryl)amido-S,Se) metal chelates are limited to Pb 2+ , Zn 2+ , Ni 2+ , Pt 2+ , Ga 3+ , and In 3+ . ,− The manganese(II)-coordinated compound 2 is thus unique. Bis(P,P,P′,P′-tetraisopropyldiselenoimidodiphosphinato) metal chelates with various divalent metal ions including, but not limited to, Ni 2+ , Hg 2+ , Pt 2+ , Cd 2+ , Sn 2+ , Pb 2+ , and Co 2+ have been reported; ,− the Mn 2+ chelate is, however, previously unknown.…”

Section: Resultsmentioning

confidence: 99%

Precursor Engineering for the Synthesis of Mixed Anionic Metal (Cu, Mn) Chalcogenide Nanomaterials via Solvent-Less Synthesis

et al. 2022

View full text Add to dashboard Cite

Metal–organic ligands with mixed chalcogenides are potential compounds for the preparation of mixed anionic metal chalcogenide alloys. However, only a few of such ligands are known, and their complexes are not well explored. We have prepared homo- and hetero-dichalcogenoimidodiphosphinate [(EE′P i Pr2NH)] (E, E′ = Se, Se; S, S; S, Se) complexes of manganese and copper through metathetical reactions. The X-ray single crystal structure of [Mn{(SeP i Pr2)2N}2] 1 revealed a triclinic crystal system, with a MnSe4 core unit, whereas the crystal structure determination of [Mn{(SP i Pr2)(SeP i Pr2)N}2] 2 indicated a triclinic crystal system with a Mn(S/Se)2 unit. Both metal centers are tetrahedral, with two deprotonated bidentate ligands forming the coordination sphere. The free ligand was found to exhibit a gauche configuration in the solid state. The energies of the various rotamers of dithio-analogue were studied by DFT calculations. The decomposition behavior of complexes with homo- and heterochalcogenides was investigated, and the complexes were employed as single-source precursors to generate manganese and copper chalcogenides through solvent-less melt reactions between 500 and 550 °C. The deposited powders were characterized by powder X-ray diffraction (p-XRD), scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDAX), transmission electron microscopy (TEM), and elemental mapping. MnS, MnSe2, and MnSSe phases were obtained from the decomposition of respective manganese complexes. In contrast, the decomposition of copper-based complexes yielded Cu2–x Se and the sulfur-doped Cu3Se2 phase from seleno- and mixed thio/seleno-complexes of Cu, respectively. The morphology ranged from random sheet-like structures to agglomerated platelets, while the selected area electron diffraction (SAED) revealed the crystalline nature of the materials. Depending on the nature of the complex and the temperature, different amounts of phosphorus were present as an impurity in the synthesized products.

show abstract

Hot‐Injection Synthesis of PbE (E= S, Se) Nanoparticles from Dichalcogenoimidophosphinato Lead (II) Complexes

Cited by 6 publications

References 45 publications

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePⁱPr₂)₂N)(S₂CNHexMe)]

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePⁱPr₂)₂N)(S₂CNHexMe)]

Synthesis of a Novel Single-Source Precursor for the Production of Lead Chalcogenide Thin Films

Precursor Engineering for the Synthesis of Mixed Anionic Metal (Cu, Mn) Chalcogenide Nanomaterials via Solvent-Less Synthesis

Contact Info

Product

Resources

About

Hot‐Injection Synthesis of PbE (E= S, Se) Nanoparticles from Dichalcogenoimidophosphinato Lead (II) Complexes

Cited by 6 publications

References 45 publications

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePiPr2)2N)(S2CNHexMe)]

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePiPr2)2N)(S2CNHexMe)]

Synthesis of a Novel Single-Source Precursor for the Production of Lead Chalcogenide Thin Films

Precursor Engineering for the Synthesis of Mixed Anionic Metal (Cu, Mn) Chalcogenide Nanomaterials via Solvent-Less Synthesis

Contact Info

Product

Resources

About

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePⁱPr₂)₂N)(S₂CNHexMe)]

Aerosol‐Assisted Chemical Vapour Deposition of Lead Chalcogenide Thin Films from [Pb((SePⁱPr₂)₂N)(S₂CNHexMe)]