Method for preparing mononuclear AgInS2 quantum dot

Abstract

The invention discloses a method for preparing mononuclear AgInS2 quantum dots, comprising the following steps of: (1) adding AgNO3, InCl3, oleic acid, dodecyl mercaptan and solvent octadecene in a reaction container, to obtain an Ag and In precursor mixed liquor; (2) adding sulfur powder into oleylamine, and heating until the sulfur powder is fully dissolved, to obtain an S precursor solution; (3) under protection of argon, heating the Ag and In precursor mixed liquor from room temperature to 50-80 DEG C, and maintaining for 10-60min, in order to discharging air; and then raising temperature to 100-120 DEG C, maintaining for 1-5min, and injecting the S solution, wherein a mol ratio of Ag to S is 1:2, and reaction time is 5-90min; (4) sampling, and dissolving a sample into hexane, to obtain a AgInS2 quantum dot solution; and (5) adding waterless ethanol into the AgInS2 quantum dot solution obtained in the step (4), and centrifugally separating to obtain the mononuclear AgInS2 quantum dots. The method of the invention further raises fluorescent quantum yield of the mononuclear AgInS2 quantum dots prepared by a thermal injection method, in order to reach practical application requirement.

Description

(1) Technical field

[0001] The invention relates to a ternary chalcogenide AgInS 2 The preparation method, especially involves a hot injection method to prepare highly efficient fluorescent AgInS 2 quantum dot method. (2) Background technology

[0002] Semiconductor Nanocrystals, also known as Quantum Dots, are a new type of semiconductor nanomaterial with a radius smaller than or close to the exciton Bohr radius of bulk materials. It is mainly a nanoparticle composed of II-VI, III-V or I-III-VI elements, whose small size makes the quasi-continuous energy band evolve into a molecular-like discrete energy level structure, showing strong The quantum confinement effect of the material makes the electronic structure, optical, magnetic and other properties of the material tunable, so that it has a series of novel properties such as light, sound, electricity, magnetism, catalysis and chemical activity. In recent years, quantum dots have become the focus of scientific researcher...

Examples

Embodiment 1

[0037] In the first step, weigh 17.1mg (0.1mmol) AgNO 3 , 88.4 mg (0.4 mmol) InCl 3 , 169.5 mg (0.6 mmol) of oleic acid and 209.7 mg (1 mmol) of dodecyl mercaptan were placed in a 100 mL three-necked flask, and 8 mL of octadecene solvent was added.

[0038] In the second step, 26.2 mg (0.8 mmol) of sulfur powder was weighed, dissolved in 2 mL of oleylamine, and placed in a 50° C. water bath to fully dissolve the sulfur powder in oleylamine.

[0039] In the third step, under the conditions of magnetic stirring and argon protection, heat the precursor solution in the first step to 60°C for 30 minutes, then continue to heat up to 100-120°C, and after stabilizing for 2 minutes, inject the second step Dissolve S powder in oleylamine, and start timing.

[0040] The fourth step is to take samples when the reaction time is 5min, 10min, 15min, 20min, 30min, 45min, 60min, 90min. Take 0.5mL reaction solution and dissolve in 0.5mL n-hexane to prepare AgInS 2 Quantum dot solution.

[...

Embodiment 2

[0047] In the first step, weigh 17.1mg (0.1mmol) AgNO 3 , 88.6mg (0.4mmol) InCl 3 , 169.8mg (0.6mmol) of oleic acid and 408.4mg (2mmol) of dodecyl mercaptan were placed in a 100mL three-necked flask, and 8mL of octadecene solvent was added.

[0048] In the second step, 25.8mg (0.8mmol) of sulfur powder was weighed, dissolved in 2mL of oleylamine, and placed in a 50°C water bath to fully dissolve the sulfur powder in oleylamine.

[0049] In the third step, under the conditions of magnetic stirring and argon protection, heat the precursor solution in the first step to 60°C for 30min, then continue to heat up to 110°C, and after stabilizing for 2min, inject the solution in the second step. Based on the S powder of oleylamine, start timing.

[0050] The fourth step is to take samples when the reaction time is 5min, 10min, 15min, 20min, 30min, 45min, 60min, 90min. Take 0.5mL reaction solution and dissolve in 0.5mL n-hexane to prepare AgInS 2 Quantum dot solution.

[0051] In t...

Embodiment 3

[0054] In the first step, weigh 16.8mg (0.1mmol) AgNO3 , 88.7mg (0.4mmol) InCl 3 , 170.8mg (0.6mmol) of oleic acid and 609.2mg (3mmol) of dodecyl mercaptan were placed in a 100mL three-necked flask, and 8mL of octadecene solvent was added.

[0055] In the second step, 26.1mg (0.8mmol) of sulfur powder was weighed, dissolved in 2mL of oleylamine, and placed in a 50°C water bath to fully dissolve the sulfur powder in oleylamine.

[0056] In the third step, under the conditions of magnetic stirring and argon protection, heat the precursor solution in the first step to 60°C for 30min, then continue to heat up to 110°C, and after stabilizing for 2min, inject the solution in the second step. Based on the S powder of oleylamine, start timing.

[0057] The fourth step is to take samples when the reaction time is 5min, 10min, 15min, 20min, 30min, 45min, 60min, 90min. Take 0.5mL reaction solution and dissolve in 0.5mL n-hexane to prepare AgInS 2 Quantum dot solution.

[0058] In the...

(1) Technical field

[0001] The invention relates to a ternary chalcogenide AgInS 2 The preparation method, especially involves a hot injection method to prepare highly efficient fluorescent AgInS 2 quantum dot method. (2) Background technology

[0002] Semiconductor Nanocrystals, also known as Quantum Dots, are a new type of semiconductor nanomaterial with a radius smaller than or close to the exciton Bohr radius of bulk materials. It is mainly a nanoparticle composed of II-VI, III-V or I-III-VI elements, whose small size makes the quasi-continuous energy band evolve into a molecular-like discrete energy level structure, showing strong The quantum confinement effect of the material makes the electronic structure, optical, magnetic and other properties of the material tunable, so that it has a series of novel properties such as light, sound, electricity, magnetism, catalysis and chemical activity. In recent years, quantum dots have become the focus of scientific researcher...

Examples

Embodiment 1

[0037] In the first step, weigh 17.1mg (0.1mmol) AgNO 3 , 88.4 mg (0.4 mmol) InCl 3 , 169.5 mg (0.6 mmol) of oleic acid and 209.7 mg (1 mmol) of dodecyl mercaptan were placed in a 100 mL three-necked flask, and 8 mL of octadecene solvent was added.

[0038] In the second step, 26.2 mg (0.8 mmol) of sulfur powder was weighed, dissolved in 2 mL of oleylamine, and placed in a 50° C. water bath to fully dissolve the sulfur powder in oleylamine.

[0039] In the third step, under the conditions of magnetic stirring and argon protection, heat the precursor solution in the first step to 60°C for 30 minutes, then continue to heat up to 100-120°C, and after stabilizing for 2 minutes, inject the second step Dissolve S powder in oleylamine, and start timing.

[0040] The fourth step is to take samples when the reaction time is 5min, 10min, 15min, 20min, 30min, 45min, 60min, 90min. Take 0.5mL reaction solution and dissolve in 0.5mL n-hexane to prepare AgInS 2 Quantum dot solution.

[...

Embodiment 2

[0047] In the first step, weigh 17.1mg (0.1mmol) AgNO 3 , 88.6mg (0.4mmol) InCl 3 , 169.8mg (0.6mmol) of oleic acid and 408.4mg (2mmol) of dodecyl mercaptan were placed in a 100mL three-necked flask, and 8mL of octadecene solvent was added.

[0048] In the second step, 25.8mg (0.8mmol) of sulfur powder was weighed, dissolved in 2mL of oleylamine, and placed in a 50°C water bath to fully dissolve the sulfur powder in oleylamine.

[0049] In the third step, under the conditions of magnetic stirring and argon protection, heat the precursor solution in the first step to 60°C for 30min, then continue to heat up to 110°C, and after stabilizing for 2min, inject the solution in the second step. Based on the S powder of oleylamine, start timing.

[0050] The fourth step is to take samples when the reaction time is 5min, 10min, 15min, 20min, 30min, 45min, 60min, 90min. Take 0.5mL reaction solution and dissolve in 0.5mL n-hexane to prepare AgInS 2 Quantum dot solution.

[0051] In t...

Embodiment 3

[0054] In the first step, weigh 16.8mg (0.1mmol) AgNO3 , 88.7mg (0.4mmol) InCl 3 , 170.8mg (0.6mmol) of oleic acid and 609.2mg (3mmol) of dodecyl mercaptan were placed in a 100mL three-necked flask, and 8mL of octadecene solvent was added.

[0055] In the second step, 26.1mg (0.8mmol) of sulfur powder was weighed, dissolved in 2mL of oleylamine, and placed in a 50°C water bath to fully dissolve the sulfur powder in oleylamine.

[0056] In the third step, under the conditions of magnetic stirring and argon protection, heat the precursor solution in the first step to 60°C for 30min, then continue to heat up to 110°C, and after stabilizing for 2min, inject the solution in the second step. Based on the S powder of oleylamine, start timing.

[0057] The fourth step is to take samples when the reaction time is 5min, 10min, 15min, 20min, 30min, 45min, 60min, 90min. Take 0.5mL reaction solution and dissolve in 0.5mL n-hexane to prepare AgInS 2 Quantum dot solution.

[0058] In the...

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