CN108276985B - Sulfur quantum dot with fluorescence characteristic and preparation method thereof - Google Patents
Sulfur quantum dot with fluorescence characteristic and preparation method thereof Download PDFInfo
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention relates to a sulfur quantum dot with fluorescence characteristic and a preparation method thereof, wherein the sulfur quantum dot is of a spherical structure and sequentially comprises a core, an adsorption layer and a coating layer from inside to outside, the core is a sulfur nano core, the adsorption layer is a plurality of sulfur ions, and the coating layer is formed by a dispersing agent and has the particle size of 2nm-25 nm. The existing sulfur quantum dots have no fluorescence. The nano sulfur sol prepared by the method has good water solubility, fluorescence and stability.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a structure, a preparation method and a regulation and control method of a sulfur quantum dot with fluorescence characteristics.
Background
At present, due to the excellent performance of the nano-materials, considerable attention is paid, and fluorescent semiconductor quantum dots of the nano-materials have various exciting application prospects, particularly the application of the fluorescent semiconductor quantum dots in biology and medicine. However, in vitro and in vivo use, the development of many materials is largely limited by their known toxicity and potential environmental hazards, and research to find superior nanomaterials with similar optical properties continues. At present, the research of quantum-sized silicon, gold nanoclusters and carbon nanodots based attracts extensive research.
The element sulfur is an important element, has unique chemical property and biological activity, and has wide application, such as antibacterial agent, preparation and modification of nano carbon nano tube and preparation of nano composite material for lithium battery, which has very important application. The application of sulfur in the agricultural field can be used as a bactericide for many plant diseases.
Sulfur nanoparticles of different sizes and shapes are prepared by different methods, and currently, there are many methods for preparing sulfur nanoparticles, such as hydrolysis of thiosulfate and oxidation of H with Fe metal chelate2S gas, ultrasonic processing of a sulfocystine solution, a surfactant aqueous solution method, a micro-emulsification technology and an electrochemical method. At present, the preparation of fine sulfur is mainly carried outChemical Vapor Deposition (CVD) is a method of obtaining fine sulfur (sublimed sulfur) of different particle sizes from sulfur ore by controlling the temperature (boiling point of sulfur 444.6 ℃), vacuum, inert gas protection, etc. CVD conditions are harsh, high cost and large energy consumption, and the soft chemistry principle is a more effective way to prepare economical and practical nano materials. In addition, no report has been made so far on the synthesis of nano sulfur having fluorescence characteristics, and particularly, fewer sulfur quantum dots are used for synthesizing the fluorescence characteristics of good fluorescence performance, good water solubility, good dispersibility and good stability. The invention aims to synthesize the sulfur quantum dots with strong fluorescence, better dispersibility and better stability, and meanwhile, the sulfur quantum dots have no toxicity and the preparation method is simple.
Disclosure of Invention
Based on the description of the background art, one of the objects of the present invention is to provide a sulfur quantum dot having fluorescent characteristics; the second purpose of the invention is to provide a preparation method of the sulfur quantum dot with the fluorescence characteristic, which is to prepare the nanometer sulfur quantum dot which is soluble in water, has the fluorescence characteristic and has better stability by a simple chemical method; the third purpose of the invention is to provide a method for regulating and controlling the emission wavelength of the sulfur quantum dot with fluorescence characteristics.
The purpose of the invention is realized by the following technical scheme:
a sulfur quantum dot with fluorescence characteristics, which is characterized in that: the sulfur quantum dots are of a spherical structure and sequentially comprise a core, an adsorption layer and a wrapping layer from inside to outside, wherein the core is a sulfur nano core, the adsorption layer is a plurality of sulfur ions, and the wrapping layer is formed by a dispersing agent and has a particle size of 2-25 nm.
The materials of the general dispersant may be selected as: PEG-200, PEG-400 or NH3-PEG-NH3。
The invention also provides a preparation method of the sulfur quantum dot with the fluorescence characteristic, which comprises the following steps:
1) adding a dispersing agent and water into sulfur powder at normal temperature and normal pressure, and uniformly stirring and mixing, wherein the molar ratio of the sulfur powder to the dispersing agent is (21-0.03): 1;
2) heating the mixture obtained in the step 1) at 50-150 ℃, uniformly and slowly adding solid alkali particles or dropwise adding an alkali solution into the mixture for about 1 hour while heating, wherein the molar ratio of the sulfur powder to the alkali is (1-0.003):1 range;
3) heating while refluxing and stirring for 6-150 h;
4) and (4) purifying the product obtained in the step (3) to obtain the sulfur quantum dot sol.
The molar ratio of the sulfur powder to the dispersant is 5.5:1, and the molar ratio of the sulfur powder to the alkali is 0.44: 1.
The heating temperature of the step 2) is 65-75 ℃.
The dispersant is: PEG-200, PEG-400 or NH3-PEG-NH3。
The sulfur powder is in a sublimed sulfur crystal form, and the alkali is sodium hydroxide, potassium hydroxide, ammonia water or sodium carbonate.
The invention also provides another preparation method of the sulfur quantum dot with the fluorescence characteristic, which comprises the following steps:
1) placing a mixed solution of sulfur powder, a dispersing agent, water and solid alkali particles or an alkali solution in a reaction kettle with a polytetrafluoroethylene inner container, wherein the molar ratio of the sulfur powder to the dispersing agent is (21-0.03): 1; the molar ratio of the sulfur powder to the alkali is (1-0.003) 1;
2) heating the reaction kettle at 180 ℃ for reaction for two hours;
3) purifying the product obtained in the step 2) to obtain the sulfur quantum dot sol.
The invention also provides a method for regulating and controlling the emission wavelength of the sulfur quantum dots in the preparation process, which comprises the following steps:
1) at normal temperature and normal pressure, adding a dispersing agent and water into sulfur powder, and stirring and mixing uniformly, wherein the molar ratio of the sulfur powder to the dispersing agent is 5.5: 1.
2) Heating the mixture obtained in the step 1) at 50-150 ℃, uniformly and slowly adding solid alkali particles or dropwise adding an alkali solution into the mixture for about 1 hour while heating, wherein the molar ratio of the sulfur powder to the alkali is 0.44: 1;
3) regulating and controlling:
controlling the heating reflux stirring time to be 6-30 h, wherein the maximum emission wavelength of the prepared sulfur quantum dots is 540-560 nm;
controlling the heating reflux stirring time to be 30-75 h, and controlling the maximum emission wavelength of the prepared sulfur quantum dots to be 480-540 nm;
controlling the heating reflux stirring time to be 75-100 h, and controlling the maximum emission wavelength of the prepared sulfur quantum dots to be 450-480 nm;
the heating reflux stirring time is controlled to be 100-150 h, and the maximum emission wavelength of the prepared sulfur quantum dot is 420-450 nm.
The sulfur quantum dot is applied to biomarker analysis.
The invention has the beneficial effects that:
the nano sulfur sol prepared by the method has good water solubility, fluorescence and stability.
Drawings
FIG. 1 is a schematic diagram of the structure of a sulfur quantum dot; 1-core, 2-adsorption layer, 3-wrapping layer;
FIG. 2 is a fluorescent image of the nano-sulfur quantum dots prepared in example 5 of the present invention, corresponding to photographs under a fluorescent lamp and an ultraviolet lamp;
FIG. 3 is a microscopic morphology (transmission electron microscopy) of the nano-sulfur quantum dots prepared in example 7 of the present invention;
FIG. 4a is a Raman plot of sublimed sulfur, and FIG. 4b is a Raman plot of the sulfur quantum dots prepared in example 7;
FIG. 5 is an XPS plot of sulfur quantum dots prepared in example 7 of the present invention;
FIG. 6 is a graph of FIG. A, B, C showing the fluorescence stability of the sulfur quantum dots prepared in example 6 placed on the first day, the ninth day and the nineteenth day, respectively;
FIG. 7 is a schematic diagram of the process for controlling the emission wavelength of the sulfur quantum dot of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in figure 1, the sulfur quantum dot with the fluorescent characteristic is of a spherical structure and sequentially comprises a core 1, an adsorption layer 2 and a coating layer 3 from inside to outside, wherein the core is a sulfur nano core, the adsorption layer is a plurality of sulfur ions, and the coating layer is formed by a dispersing agent and has the particle size of 2nm-25 nm. The average particle size of the prepared sulfur quantum dots is generally 10 nm.
Typical materials for dispersants are: PEG-200, PEG-400, NH3-PEG-NH3。
Example 2: a preparation method of a sulfur quantum dot with fluorescence characteristics comprises the following steps:
1) adding a dispersing agent and water into sulfur powder at normal temperature and normal pressure, and uniformly stirring and mixing, wherein the molar ratio of the sulfur powder to the dispersing agent is (21-0.03): 1;
2) heating the mixture obtained in the step 1) at the temperature of 6-150 ℃, uniformly and slowly adding solid alkali particles or dropwise adding an alkali solution into the mixture for about 1 hour while heating, wherein the molar ratio of the sulfur powder to the alkali is (1-0.003):1 range; the solution gradually faded from dark red orange to light yellow with different heating time.
3) Heating while refluxing and stirring for 15-150 h.
4) And (4) performing purification methods such as centrifugation or dialysis on the product obtained in the step (3) to obtain the sulfur quantum dot sol.
On the basis of example 2, optimization of the reaction conditions was carried out, giving the following examples 3-22:
example 23: a preparation method of a sulfur quantum dot with fluorescence characteristics comprises the following steps: 1) placing a mixed solution of sulfur powder, a dispersing agent, water and solid alkali particles or an alkali solution in a reaction kettle with a polytetrafluoroethylene inner container, wherein the molar ratio of the sulfur powder to the dispersing agent is 5.5: 1; the molar ratio of the sulfur powder to the alkali is 0.44: 1; 2) heating the reaction kettle at 180 ℃ for reaction for two hours; 3) purifying the product obtained in the step 2) to obtain the sulfur quantum dot sol.
As shown in fig. 2, the fluorescence patterns of the nano sulfur quantum dots prepared in example 5 at excitation wavelengths of 380nm, 400nm and 420 nm; the inset is a photograph under the corresponding fluorescent and ultraviolet lamps. It can be seen that the maximum fluorescence emission peak of the synthesized sulfur quantum dot is 500nm under the excitation wavelengths of 380nm, 400nm and 420 nm. Under a fluorescent lamp, the sulfur quantum dots are dark orange, and under an ultraviolet lamp, the sulfur quantum dots are light green blue.
Fig. 3 is a microscopic morphology (transmission electron microscope image) of the nano sulfur quantum dots prepared in the embodiment 7 of the present invention, and it can be seen from fig. 3 that the sulfur quantum dots have relatively uniform overall particles and relatively good dispersibility, and the diameter distribution range of the sulfur quantum dots is 2-25 nm.
From FIG. 4a, it can be seen that the sublimed sulfur has three marked peaks at 150cm-1,217cm-1And 471cm-1From fig. 4b, it can be seen that the sulfur quantum dot prepared in example 7 also has the same characteristic peak, indicating that the synthesized nano material is a sulfur substance.
FIG. 5 is an XPS graph of a 2 p-structured sulfur quantum dot prepared in example 7, peaks at 163.25eV and 164.2eV are peaks of a sulfur atom, and peaks at 167.45eV and 168.3eV are peaks of SO2 -Peak of (3), peak at 169.2eV is SO3 -Peak of (2).
Fig. 6 is a graph of the fluorescence stability of the prepared sulfur quantum dot A, B, C of example 6 on the first day, the ninth day and the nineteenth day, respectively, and it can be seen that the prepared sulfur quantum dot sample still has good fluorescence and shows good stability after being placed for 19 days.
Example 24: a method for regulating and controlling the emission wavelength of a sulfur quantum dot in the preparation process of the sulfur quantum dot comprises the following steps:
1) adding a dispersing agent and water into sulfur powder at normal temperature and normal pressure, and uniformly stirring and mixing, wherein the molar ratio of the sulfur powder to the dispersing agent is (21-0.03): 1;
2) heating the mixture obtained in the step 1) at 50-150 ℃, uniformly and slowly adding solid alkali particles or dropwise adding an alkali solution into the mixture for about 1 hour while heating, wherein the molar ratio of the sulfur powder to the alkali is (1-0.003):1 range;
3) regulating and controlling:
the maximum emission wavelength of the sulfur quantum can be regulated and controlled by the length of the reaction time under different raw material molar ratios. As the reaction time is prolonged, the maximum emission wavelength of the obtained sulfur quantum dot is shifted to the blue wave direction.
Controlling the heating reflux stirring time to be 15-30 h, wherein the maximum emission wavelength of the prepared sulfur quantum dots is 540-560 nm;
controlling the heating reflux stirring time to be 30-75 h, and controlling the maximum emission wavelength of the prepared sulfur quantum dots to be 480-540 nm;
controlling the heating reflux stirring time to be 75-100 h, and controlling the maximum emission wavelength of the prepared sulfur quantum dots to be 450-480 nm;
the heating reflux stirring time is controlled to be 100-150 h, and the maximum emission wavelength of the prepared sulfur quantum dot is 420-450 nm.
As shown in FIG. 7, in examples 4, 5, 7, 8, the molar ratio of sulfur powder to dispersant is 5.5:1, and the molar ratio of sulfur powder to alkali is 0.44:1, wherein A) is that the reflux stirring time is 30h, and the maximum emission wavelength of the prepared sulfur quantum dot is 550 nm; wherein, the picture B) shows that the reflux stirring time is 43h, and the maximum emission wavelength of the prepared sulfur quantum dot is 500 nm; wherein, the C) diagram shows that the reflux stirring time is 100h, and the maximum emission wavelength of the prepared sulfur quantum dot is 460 nm; wherein D) is that the reflux stirring time is 125h, and the maximum emission wavelength of the prepared sulfur quantum dot is 440 nm.
It can be seen that the maximum emission wavelength of the sulfur quantum can be regulated by the length of the reaction time. As the reaction time is prolonged, the maximum emission wavelength of the obtained sulfur quantum dot is shifted to the blue wave direction. The maximum emission wavelength is gradually shifted from 550nm to 500nm, 460nm and 440nm, the solution color changes from dark orange to light yellow, and under an ultraviolet lamp, the solution color gradually changes to dark blue. The regulation and control method mentioned in this example is directed to specific mixture ratio, and under other mixture ratio conditions, the reflux stirring time is found to be related to the amount of sulfur. The smaller the amount of sulfur, the shorter the reaction time required for the appearance of a peak; conversely, the larger the amount of sulfur, the longer the reaction time required for the peak to appear.
Example 25: the sulfur quantum dots prepared by the method can be applied to biomarker analysis.
Claims (6)
1. A preparation method of a sulfur quantum dot with fluorescence characteristics comprises the following steps:
1) adding a dispersing agent and water into sulfur powder at normal temperature and normal pressure, and uniformly stirring and mixing, wherein the molar ratio of the sulfur powder to the dispersing agent is (21-0.03): 1, the dispersing agent is: PEG-200, PEG-400 or NH3-PEG-NH3；
2) Heating the mixture obtained in the step 1) at the temperature of 50-150 ℃, uniformly and slowly adding solid alkali particles or dropwise adding an alkali solution into the mixture for about 1 hour while heating, wherein the molar ratio of the sulfur powder to the alkali is (1-0.003):1 range;
3) heating while refluxing and stirring for 6-150 h;
4) and (4) purifying the product obtained in the step (3) to obtain the sulfur quantum dot sol.
2. The method for preparing a sulfur quantum dot having fluorescent properties according to claim 1, wherein: the molar ratio of the sulfur powder to the dispersant is 5.5:1, and the molar ratio of the sulfur powder to the alkali is 0.44: 1.
3. The method for preparing a sulfur quantum dot having fluorescent properties according to claim 2, wherein: the heating temperature of the step 2) is 65-75 ℃.
4. The method for preparing a sulfur quantum dot having fluorescent properties according to claim 3, wherein: the sulfur powder is in a sublimed sulfur crystal form, and the alkali is sodium hydroxide, potassium hydroxide, ammonia water or sodium carbonate.
5. A preparation method of a sulfur quantum dot with fluorescence characteristics comprises the following steps:
1) placing a mixed solution of sulfur powder, a dispersing agent, water and solid alkali particles or an alkali solution in a reaction kettle with a polytetrafluoroethylene inner container, wherein the molar ratio of the sulfur powder to the dispersing agent is (21-0.03): 1; the molar ratio of the sulfur powder to the alkali is (1-0.003) 1;
2) heating the reaction kettle at 180 ℃ for reaction for two hours;
3) purifying the product obtained in the step 2) to obtain the sulfur quantum dot sol.
6. A method for regulating and controlling the emission wavelength of a sulfur quantum dot in the preparation process of the sulfur quantum dot comprises the following steps:
1) at normal temperature and normal pressure, adding a dispersing agent and water into sulfur powder, and stirring and mixing uniformly, wherein the molar ratio of the sulfur powder to the dispersing agent is 5.5: 1.
2) Heating the mixture obtained in the step 1) at the temperature of 50-150 ℃, uniformly and slowly adding solid alkali particles or dropwise adding an alkali solution into the mixture for about 1 hour while heating, wherein the molar ratio of the sulfur powder to the alkali is 0.44: 1;
3) regulating and controlling:
controlling the heating reflux stirring time to be 6-30 h, wherein the maximum emission wavelength of the prepared sulfur quantum dots is 540-560 nm;
controlling the heating reflux stirring time to be 30-75 h, and controlling the maximum emission wavelength of the prepared sulfur quantum dots to be 480-540 nm;
controlling the heating reflux stirring time to be 75-100 h, and controlling the maximum emission wavelength of the prepared sulfur quantum dots to be 450-480 nm;
the heating reflux stirring time is controlled to be 100-150 h, and the maximum emission wavelength of the prepared sulfur quantum dot is 420-450 nm.
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| CN109810553B (en) * | 2019-01-07 | 2021-09-03 | 湖北大学 | Graphene oxide composite hydroxyapatite sulfur-loaded quantum dot antibacterial coating and preparation method thereof |
| CN110171806B (en) * | 2019-05-08 | 2022-04-22 | 桂林理工大学 | Preparation method of water-soluble red light sulfur quantum dots |
| CN110129040B (en) * | 2019-05-08 | 2022-02-08 | 桂林理工大学 | Preparation method of water-soluble fluorescent sulfur quantum dots |
| CN110395698B (en) * | 2019-07-10 | 2021-10-08 | 清华大学 | Chemical additive solution and preparation method and application thereof |
| CN110387224B (en) * | 2019-07-23 | 2023-01-24 | 江苏海洋大学 | Method for improving fluorescence property of sulfur quantum dots and application |
| CN111420678B (en) * | 2020-01-19 | 2023-02-10 | 西安科技大学 | Based on H 2 O 2 Method for preparing nano sulfur materials with different shapes by regulation and control |
| CN111218272B (en) * | 2020-02-06 | 2022-02-11 | 桂林理工大学 | Preparation method of fluorescent sulfur quantum dots based on sulfur-amine solution |
| CN111218285B (en) * | 2020-02-06 | 2022-02-11 | 桂林理工大学 | Preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed solution |
| CN112777570B (en) * | 2021-01-19 | 2023-03-28 | 中南大学 | Synthesis of sulfur nanosheets and application thereof in drug delivery |
| CN116814248B (en) * | 2023-06-30 | 2024-04-02 | 常州大学 | Preparation method and application of hybridization sulfur quantum dot with room temperature afterglow |
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Effective date of registration: 20210428 Address after: 201100 room 1017, building 1, 199 JiangKai Road, Minhang District, Shanghai Patentee after: Star purple (Shanghai) new material technology development Co.,Ltd. Address before: 710054, No. 58, Yanta Road, Yanta District, Shaanxi, Xi'an Patentee before: XI'AN University OF SCIENCE AND TECHNOLOGY |