Method for synthesizing water-soluble Pt: ZnSe(S) alloyed nanometer crystal by using hydro-thermal method

Abstract

The invention belongs to the technical field of a preparation method for nanometer luminescent materials and particularly relates to a method for synthesizing a water-soluble Pt: ZnSe(S) alloyed nanometer crystal by using a hydro-thermal method. The water-soluble Pt: ZnSe(S) alloyed nanometer crystal is prepared by using ultrapure water as a solvent and using inorganic metal water-soluble compounds such as zinc salt and platinum salt, selenium powder and sulfydryl-containing carboxylic acid reagents as raw materials. According to the method, the expensive and dangerous organic metal precursoris replaced by the cheap raw material, so that the method is environmentally-friendly and the preparation cost is lowered. The operation is simple and safe and the repeatability is excellent. The shape of the synthesized nanometer crystal is fine and the quantum yield is about 25%.

Description

technical field

[0001] The invention relates to a method for preparing a nano-luminescent material. Water-soluble Pt:ZnSe(S) alloy nano-crystals are synthesized by a hydrothermal method. Background technique

[0002] Semiconductor nanocrystals have the characteristics of high quantum efficiency, wide and continuous excitation spectrum, symmetrical and narrow emission spectrum, the color of emitted light changes with particle size, and good photochemical stability. Compared with traditional fluorescent dyes, they have incomparable advantages. . If the problems of biocompatibility and biotoxicity can be solved, quantum dots will play a huge role in cell recognition, cell staining, disease diagnosis, and real-time monitoring of the migration of biological components. With the gradual deepening of research, semiconductor nanocrystals as biomarkers have become an emerging, cutting-edge and most active research field in analytical science.

[0003] At present, the application of...

Examples

Embodiment 1

[0032] 1. First mix 0.439g zinc acetate and 1.0614g 3-mercaptopropionic acid, dilute to 50ml with water, mix and stir for 5 minutes.

[0033] 2. Add 10ml of 0.001M platinum tetrachloride solution to the solution in step 1, and continue stirring for 5 minutes.

[0034] 3. The pH of the solution in step 2 was adjusted to 8 with sodium hydroxide solution, at this time, argon gas was passed into the alkaline solution, and oxygen was removed by bubbling for 10 minutes to obtain an oxygen-free aqueous solution.

[0035] 4. Under the protection of argon, dissolve 0.079g of selenium powder and 0.0757g of sodium borohydride in 5ml of ultrapure water, heat to 40°C, and react for 30 minutes to prepare NaHSe stock solution.

[0036] 5. Quickly inject the NaHSe stock solution prepared in step 4 into the alkaline anaerobic aqueous solution prepared in step 3.

[0037] 6. Continue to stir under the protection of argon for 10 minutes, transfer the solution to a 200ml polytetrafluoroethylene ...

Embodiment 2

[0040] 1. First mix 0.6585g of zinc acetate and 0.9553g of 3-mercaptopropionic acid, add water to dilute to 60ml, mix and stir for 10 minutes.

[0041] 2. Add 10ml of 0.002M platinum tetrachloride solution to the solution in step 1, and continue stirring for 5 minutes.

[0042] 3. The pH of the solution in step 2 was adjusted to 9 with sodium hydroxide solution, at this time, argon gas was passed into the alkaline solution, and oxygen was removed by bubbling for 20 minutes to obtain an oxygen-free aqueous solution.

[0043] 4. Under the protection of argon, dissolve 0.079g of selenium powder and 0.1136g of sodium borohydride in 1ml of ultrapure water, heat to 50°C, and react for 1 minute to prepare NaHSe stock solution.

[0044] 5. Quickly inject the NaHSe stock solution prepared in step 4 into the alkaline anaerobic aqueous solution prepared in step 3.

[0045] 6. Continue to stir under the protection of argon for 20 minutes, transfer the solution to a 200ml polytetrafluoroeth...

Embodiment 3

[0048] 1. First mix 1.0975g of zinc acetate and 1.0614g of 3-mercaptopropionic acid, add water to dilute to 70ml, mix and stir for 15 minutes.

[0049] 2. Add 10ml of 0.004M platinum tetrachloride solution to the solution in step 1, and continue stirring for 5 minutes.

[0050] 3. Adjust the pH of the solution in step 2 to 9.5 with sodium hydroxide solution. At this time, nitrogen gas is passed into the alkaline solution, and oxygen is removed by bubbling for 15 minutes to obtain an oxygen-free aqueous solution.

[0051] 4. Under nitrogen protection, dissolve 0.079g of selenium powder and 0.1514g of sodium borohydride in 20ml of ultrapure water, heat to 80°C, and react for 5 minutes to prepare NaHSe stock solution.

[0052] 5. Quickly inject the NaHSe stock solution prepared in step 4 into the alkaline anaerobic aqueous solution prepared in step 3.

[0053] 6. Continue to stir under nitrogen protection for 15 minutes, then transfer the solution to a 200ml polytetrafluoroethyl...

technical field

[0001] The invention relates to a method for preparing a nano-luminescent material. Water-soluble Pt:ZnSe(S) alloy nano-crystals are synthesized by a hydrothermal method. Background technique

[0002] Semiconductor nanocrystals have the characteristics of high quantum efficiency, wide and continuous excitation spectrum, symmetrical and narrow emission spectrum, the color of emitted light changes with particle size, and good photochemical stability. Compared with traditional fluorescent dyes, they have incomparable advantages. . If the problems of biocompatibility and biotoxicity can be solved, quantum dots will play a huge role in cell recognition, cell staining, disease diagnosis, and real-time monitoring of the migration of biological components. With the gradual deepening of research, semiconductor nanocrystals as biomarkers have become an emerging, cutting-edge and most active research field in analytical science.

[0003] At present, the application of...

Examples

Embodiment 1

[0032] 1. First mix 0.439g zinc acetate and 1.0614g 3-mercaptopropionic acid, dilute to 50ml with water, mix and stir for 5 minutes.

[0033] 2. Add 10ml of 0.001M platinum tetrachloride solution to the solution in step 1, and continue stirring for 5 minutes.

[0034] 3. The pH of the solution in step 2 was adjusted to 8 with sodium hydroxide solution, at this time, argon gas was passed into the alkaline solution, and oxygen was removed by bubbling for 10 minutes to obtain an oxygen-free aqueous solution.

[0035] 4. Under the protection of argon, dissolve 0.079g of selenium powder and 0.0757g of sodium borohydride in 5ml of ultrapure water, heat to 40°C, and react for 30 minutes to prepare NaHSe stock solution.

[0036] 5. Quickly inject the NaHSe stock solution prepared in step 4 into the alkaline anaerobic aqueous solution prepared in step 3.

[0037] 6. Continue to stir under the protection of argon for 10 minutes, transfer the solution to a 200ml polytetrafluoroethylene ...

Embodiment 2

[0040] 1. First mix 0.6585g of zinc acetate and 0.9553g of 3-mercaptopropionic acid, add water to dilute to 60ml, mix and stir for 10 minutes.

[0041] 2. Add 10ml of 0.002M platinum tetrachloride solution to the solution in step 1, and continue stirring for 5 minutes.

[0042] 3. The pH of the solution in step 2 was adjusted to 9 with sodium hydroxide solution, at this time, argon gas was passed into the alkaline solution, and oxygen was removed by bubbling for 20 minutes to obtain an oxygen-free aqueous solution.

[0043] 4. Under the protection of argon, dissolve 0.079g of selenium powder and 0.1136g of sodium borohydride in 1ml of ultrapure water, heat to 50°C, and react for 1 minute to prepare NaHSe stock solution.

[0044] 5. Quickly inject the NaHSe stock solution prepared in step 4 into the alkaline anaerobic aqueous solution prepared in step 3.

[0045] 6. Continue to stir under the protection of argon for 20 minutes, transfer the solution to a 200ml polytetrafluoroeth...

Embodiment 3

[0048] 1. First mix 1.0975g of zinc acetate and 1.0614g of 3-mercaptopropionic acid, add water to dilute to 70ml, mix and stir for 15 minutes.

[0049] 2. Add 10ml of 0.004M platinum tetrachloride solution to the solution in step 1, and continue stirring for 5 minutes.

[0050] 3. Adjust the pH of the solution in step 2 to 9.5 with sodium hydroxide solution. At this time, nitrogen gas is passed into the alkaline solution, and oxygen is removed by bubbling for 15 minutes to obtain an oxygen-free aqueous solution.

[0051] 4. Under nitrogen protection, dissolve 0.079g of selenium powder and 0.1514g of sodium borohydride in 20ml of ultrapure water, heat to 80°C, and react for 5 minutes to prepare NaHSe stock solution.

[0052] 5. Quickly inject the NaHSe stock solution prepared in step 4 into the alkaline anaerobic aqueous solution prepared in step 3.

[0053] 6. Continue to stir under nitrogen protection for 15 minutes, then transfer the solution to a 200ml polytetrafluoroethyl...

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