Синтез и свойства коллоидных квантовых точек на основе халькогенидов ртути / Synthesis and properties of colloidal quantum dots based on mercury chalcogenides тема диссертации и автореферата по ВАК РФ 00.00.00, кандидат наук Мардини Алаа Алддин

• Мардини Алаа Алддин
• кандидат наук
• 2024

Оглавление диссертации кандидат наук Мардини Алаа Алддин

Contents

Abstract

Chapter 1. Introduction to the mercury chalcogenides CQDs preparation methods

1.1 HgTe CQDs

1.1.1 Preparation and characterization of HgTe CQDS in aqueous solutions

1.1.2 Preparation and characterization of HgTe CQDS in organic mediums

1.1.2.1 Tri-n-octylphosphine telluride (TOPTe)

1.1.2.2 Bis(trimethylsilyl) telluride (TMS)2Te

1.1.2.3 Bis(trimethylsilyl) telluride (TMS)2Te and tri-n-octylphosphine telluride (TOPTe)

1.1.2.4 Tri-butylphosphine telluride (TBPTe)

1.1.3 Preparation and characterization of HgTe CQDS using aprotic solvents

1.2 HgTe NPLs

1.3 HgS CQDs

1.3.1 Preparation and characterization of HgS CQDS in aqueous solutions

1.3.2 Preparation and characterization of HgS CQDS in organic mediums

1.3.2.1 Bis(trimethylsilyl) sulfide (TMS)2S

1.3.2.2 Tri-n-octylphosphine sulfide (TOPS)

1.3.2.3 Phosphine-free precursors of sulfide

Chapter 2. The experimental section

2.1 Synthesis of HgTe CQDs

2.1.1 Synthesis of the tellurium precursors

2.1.2 Synthesis of HgTe CQDs

2.2 Preparation of telluride NCs using (Cy)3PTe/THF Precursor

2.2.1 Synthesis of PbTe CQDs

2.2.2 Synthesis of CdTe CQDs

3

2.2.3 Synthesis of ZnTe CQDs

2.3 Synthesis of HgS CQDs

2.3.1 Synthesis of the THF solution of tricyclohexylphosphine sulfide

2.3.2 Synthesis of HgS CQDs

Chapter 3. Results, Discussion, and Conclusion

3.1. Investigation of tellurium precursors using NMR spectroscopy

3.1.1 Investigation of TOPTe using 31P and 125Te NMR spectroscopy

3.1.2 Investigation of TDMAPTe using 31P NMR spectroscopy

3.1.3 Investigation of (Cy)sPTe using *H, 13C, 31P and 125Te, COSY and HSQC NMR spectroscopy

3.2 Characterization of HgTe CQDs

3.2.1 Investigation of the quantum confinement effect of HgTe QDs

3.2.2 Investigation of the chemical composition and crystal shape of HgTe NCs

3.2.3 Investigation of the kinetics of growth of HgTe CQDs

3.2.4 Optical properties of HgTe CQDs

3.3 Characterization of telluride NCs prepared using (Cy)3PTe/THF precursor

3.3.1 Characterization and optical properties of PbTe CQDs

3.3.2 Characterization and optical properties of CdTe CQDs

3.3.3 Characterization of ZnTe CQDs

3.4 Characterization of HgS CQDs

3.4.1 Investigation of the quantum confinement effect, chemical composition, and crystal structure of HgS CQDs

3.4.2 Optical properties of HgS CQDs

3.5 Conclusion

References

4

List of abbreviations

List of figures

List of tables

Publications

Введение диссертации (часть автореферата) на тему «Синтез и свойства коллоидных квантовых точек на основе халькогенидов ртути / Synthesis and properties of colloidal quantum dots based on mercury chalcogenides»

The facility of adjusting the optical features of colloidal quantum dots is one of their most important discovered properties [1]. By merging all known materials that can be prepared as CQDs with quantum confinement, the energy of the optical transition can be adjusted from a few millielectron volts (far infrared) up to several electron volts (ultraviolet) [2]. After the discovery of the optical properties of inorganic CQDs in the visible range [3], the possibility of detecting these properties in the infrared range has become one of the most promising applications of nanocrystals and a key benefit compared to organic materials [4]. The implementations of CQDs in the infrared window have initially been focused on the absorption of the infrared radiation of the solar spectrum for solar cell applications [2]. Later, the possibility of designing infrared detectors in various ranges of IR wavelengths has also been investigated, including near-infrared (NIR, 0.7-1.4 ^m) [5-7], short-wavelength infrared (SWIR, 1.4-3 ^m) [8-10], mid-wavelength infrared (MWIR, 3-8 ^m) [11-14] to even long-wavelength infrared (LWIR, 8-15 ^m) [15, 16]. Mercury chalcogenides (HgX: HgS, HgSe, and HgTe) have the ability to process this part of the electromagnetic range because they gather between IR-tunable optical properties and photoconduction [17]. As a bulk material, HgTe exists as a semi-metal with almost zero band gap. If this material is made in the form of nano-sized particles and quantum confinement occurs, the band gap widens and the material can exhibit the properties of a semiconductor with potential absorption peaks that cover the whole infrared window [1]. Different telluride precursors were used in the synthesis of HgTe CQDs. The previous works showed that the preparation of HgTe CQDs was performed using hydrogen telluride H2Te in the aqueous solution [8, 18, 19]. Meanwhile, tri-n-octylphosphine telluride TOPTe [1, 13, 20-24] and bis(trimethylsilyl) telluride (TMS)2Te [25, 26] were employed in the organic medium. Compared to aqueous routes, non-aggregated, faceted, and sphere-shaped HgTe QDs were obtained using organic methods. More improvement in the non-aggregation and sphericity of the prepared QDs was achieved using the (TMS)2Te precursor. As for HgS NCs, two crystalline forms of bulk mercury sulfide, a-HgS and P-HgS, were observed [27]. Both structures have uses in infrared technology [15, 28]. Sulfur [1, 29, 30], thioacetamide (TAA) [31], sodium sulfide (SS) [27, 32], ammonium sulfide (AS) [33], tri-n-octylphosphine sulfide (TOPS) [28], and bis(trimethylsilyl) sulfide (TMS)2S [34, 35] were utilized as sulfide precursors. Only (TMS)2S produced high-

monodispersed and highly colloidally stable HgS CQDs [35]. However, the high cost and poor stability of (TMS)2X (X: Te, S) [36] make the synthesis of mercury chalcogenides CQDs impractical, at least on an industrial scale. An urgent need has emerged to find new alternatives that can be used instead of common telluride and sulfide precursors in the QDs preparation. Solid-structured phosphine chalcogenide precursors are one of the alternative materials that have never been tested in the synthesis of metal chalcogenide NCs.

Aim and Objectives of the dissertation

The aim of this work is the preparation and characterization of mercury chalcogenide CQDs using solid-structured phosphine-chalcogen precursors.

In order to achieve this goal, the following objectives were completed:

• Preparation of tricyclohexylphosphine telluride using different solvents such as THF, 1,4-dioxane, and toluene.

• Characterization of the pure (Cy)sPTe crystals using *H, 13C, COSY, HSQC, 31P, and 125Te NMR spectroscopy.

• Investigation of the reactivity of the obtained tricyclohexylphosphine telluride solutions (in THF, 1,4-dioxane, and toluene) compared to TOPTe/TOP and TDMAPTe/THF in the synthesis of HgTe CQDs.

• Examination of the efficiency of the prepared (Cy)3PTe/THF precursor in the synthesis of other telluride QDs such as PbTe, CdTe, and ZnTe.

• Characterization of the prepared telluride NCs utilizing transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-Vis-NIR spectroscopy, fluorescence spectroscopy, Fourier-transform infrared spectroscopy (FT-IR), and Raman spectroscopy.

• Exploring the possible use of tricyclohexylphosphine sulfide in THF (Cy)3PS/THF as a novel phosphine-sulfur precursor in the synthesis of HgS CQDs.

The scientific novelty of the work

Applying solid-structured phosphine chalcogenide precursors, such as (Cy)3PX (X: Te, S), is one of the new trends in QDs synthesis that have never been explored before. Due to the steric effect of the cyclohexyl substituents, the tricyclohexylphosphine, as a white, solid substance, can withstand brief contact with air. As a result, the preparation of the corresponding chalcogen precursor may be performed considerably more simply than using trimethylsilyl (TMS) or other common phosphines, such as trioctylphosphine (TOP), which easily oxidize or even ignite when in contact with air. In addition, the solvent-limited reactivity of such precursors allows one to modify the characteristics of the prepared QDs to be suitable for different IR applications.

The practical importance of the work

Solid-structured phosphine-chalcogen precursors, such as (Cy)3PX (X: Te, S), will be the best alternative materials compared to common chalcogenide ones (TOPX and (TMS)2X), as they are cheaper, easier-handled, and have solvent-limited reactivity.

Statements to be defended

1. Successfully applying (Cy)3PX (X: Te, S) for the first time in the preparation of HgX (X: Te, S) CQDs.

2. Establishing the relationship between the chemical reactivity of the telluride precursor and the kinetics of the growth of HgTe CQDs. Under the same empirical conditions, the more reactive phosphine-telluride precursor produced the larger-sized HgTe CQDs.

3. Proving the effect of the polarity of the solvent on the chemical reactivity of the (Cy)3PTe precursor. An increase in the chemical reactivity of (Cy)3PTe in the synthesis of HgTe CQDs was observed by changing the solvent from a moderate polar aprotic solvent (THF) to a nonpolar one (toluene).

4. Demonstrating how the reaction temperature affected the chemical reactivity of the telluride precursors, namely TOPTe and (Cy)3PTe, that were applied in the preparation of HgTe CQDs. Larger-sized HgTe CQDs were obtained by increasing the reaction temperature from 60 to 100 oC at the same reaction times.

5. As for tricyclohexylphosphine telluride that was prepared using THF, (Cy)3PTe/THF, an increase in its chemical reactivity in the synthesis of HgTe CQDs by increasing its initial molar ratio relative to mercury precursor from Hg:Te (1:1) to Hg:Te (1:2) was shown.

6. Beside of the preparation of HgTe CQDs using (Cy)3PTe/THF, the dissertation showed successfully employing the titled precursor for the first time in the synthesis of different telluride QDs, namely PbTe, CdTe, and ZnTe CQDs.

Заключение диссертации по теме «Другие cпециальности», Мардини Алаа Алддин

3.5 Conclusion

Tri-n-octylphosphine telluride (TOPTe), tris(dimethylamino)phosphine telluride (TDMAPTe), and tricyclohexylphosphine telluride (Cy)3PTe precursors were prepared and characterized. The characterization of the synthesized precursors was performed mainly applying 31P and 125Te NMR spectroscopy. (Cy)3PTe and TDMAPTe were used for the first time in the synthesis of HgTe CQDs. Tetrahydrofuran (THF), 1,4-dioxane, and toluene were employed as solvents in the preparation of (Cy)3PTe. Meanwhile, only THF was utilized in the synthesis of TDMAPTe. In the synthesis of HgTe CQDs and under the same empirical conditions, the highest chemical reactivity of the studied telluride precursors was observed in the case of using TDMAPTe/THF, followed by TOPTe/TOP. Meanwhile, a lower chemical reactivity was shown in the case of applying (Cy)3PTe prepared in toluene, 1,4-dioxane, and THF respectively. The increasing in the chemical reactivity of (Cy)3PTe in the synthesis of HgTe CQDs by varying the solvent from ethers to toluene highlighted the role of the polarity of the solvent in the chemical reactivity of such precursors. Moreover, it opened the door to overcome the oxygen-sensitivity problem that was observed in the preparation of the common telluride precursors such as TOPTe, TBPTe, and (TMS)2Te. An increase in the chemical reactivity of the (Cy)3PTe/THF precursor was observed as well in the case of raising the reaction temperature or its initial molar ratio. The influence of raising the reaction temperature on the chemical reactivity of the titled precursors was

observed only in the case of using TOPTe and (Cy)3PTe in the preparation of HgTe CQDs. The IR spectra of the produced QDs demonstrated band-edge excitons shifted to longer wavelengths between the near and mid-infrared (1.4-4 ^m) based on the experimental parameters. A comprehensive investigation of the prepared HgTe NCs using HgCl2 and (Cy)3PTe/THF was performed. Sphere-shaped quantum dots with a zinc blende structure of bulk HgTe were observed in the TEM and XRD, respectively. Meanwhile, XPS analysis confirmed that the prepared NCs were mercury-rich and free of tellurites such as HgTeO3 or TeO2. (Cy)3PTe/THF was also successfully applied in the synthesis of different telluride QDs such as PbTe, CdTe, and ZnTe.

In terms of sulfide precursor, (Cy)3PS/THF was applied for the first time in the synthesis of HgS CQDs. The findings revealed that mercury chloride is the best Hg precursor for obtaining QDs with long-wavelength interband absorptions in the near-IR window. The prepared HgS CQDs using (Cy)3PS/THF and HgCh as precursors had inter- and intraband absorption peaks. The interband absorptions were red-shifted to longer wavelengths in the N-IR window between 0.8 and 1.2 ^m. Whereas the red-shifting of the 1Se-1Pe intraband transitions in the mid-IR range was between 3.9 and 5.5 ^m. Sphere-shaped with a cubic structure of bulk P-HgS (metacinnabar) were shown in the TEM and XRD measurements, respectively. While XPS analysis proved that the synthesized NCs were mercury-rich and free of mercury oxide (HgO).

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