CN108276985A - It is a kind of with the sulphur quantum dot of fluorescent characteristic, preparation method and applications - Google Patents
It is a kind of with the sulphur quantum dot of fluorescent characteristic, preparation method and applications Download PDFInfo
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Abstract
The present invention relates to a kind of with the sulphur quantum dot of fluorescent characteristic, preparation method and applications, and sulphur quantum dot is spherical structure, from inside to outside successively including core, adsorption layer and wrapping layer, core are sulphur nanometer core, and adsorption layer is a variety of sulphions, wrapping layer is dispersant formation, grain size 2nm 25nm.Existing sulphur quantum dot does not have fluorescence.The nano sulfur sol being prepared by the method for the invention has good water solubility, fluorescence and stability.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to prepared by a kind of structure of the sulphur quantum dot with fluorescent characteristic
Method and regulation and control method, the nano-sulfur quantum dot fluorescence is strong, and stability is good and can be dissolved in water.
Background technology
Currently, due to the excellent performance of nano material, sizable concern, the fluorescence semiconductor amount of nano material are caused
Son point generates various infusive application prospects, especially its application in biology and medically.However, in vitro and body
It is interior in use, since the known toxicity of many materials and potential environmental hazard greatly limit the hair of these materials
Exhibition, therefore, finding, there is the research of the excellent nano material of similar optical property still to continue.Currently, the silicon of quantum size, gold
Nano-cluster and research based on carbon nano dot have attracted extensive research.
Elementary sulfur is a kind of important element, has unique chemical property and bioactivity, and be widely used, such as
Antiseptic, preparation, modification and the preparation of lithium battery nanocomposite of carbon nano tube, there is very important application.
Sulphur can be used as fungicide in the application of agriculture field to many plant diseases.
The sulfur nano particles of different sizes and shapes are prepared by different methods, and there are many kinds for sulfur nano particles at present
Preparation method aoxidizes H such as the hydrolysis of thiosulfate with Fe metallo-chelates2S gases are ultrasonically treated sulphur cystine solution, table
Face aqueous surfactant solutions method, micro-emulsion technology, electrochemical method.Fine magister of sulfur mainly uses chemical vapour deposition technique at present
(CVD), by raw material of sulphur mine difference is obtained by conditions such as temperature control (444.6 DEG C of the boiling point of sulphur), vacuum, inert gas shieldings
The fine sulphur (sublimed sulfur) of grain size.CVD conditions are harsh, of high cost, energy consumption is big, and soft chemical method is then to prepare economical and practical nanometer
The more effective approach of material.In addition, up to now, there are no the reports of nano-sulfur of the synthesis with fluorescent characteristic, especially
Synthesis fluorescence property is good, and the sulphur quantum dot of good water solubility, good dispersion, the good fluorescent characteristic of stability is less.Purport of the present invention
There is very strong fluorescence, preferably the sulphur quantum dot of dispersibility and preferable stability in synthesis, while sulphur quantum dot does not have
Toxicity, preparation method are simple.
Invention content
Description based on background technology, an object of the present invention are to provide a kind of sulphur quantum dot with fluorescent characteristic；
Second object of the present invention is to provide a kind of preparation method of the sulphur quantum dot with fluorescent characteristic, passes through a kind of simple chemistry
Method be prepared it is water-soluble, have fluorescent characteristic and the preferable nano-sulfur quantum dot of stability；The third mesh of the present invention
It is that a kind of method of sulphur quantum dot emission wavelengths of the regulation and control with fluorescent characteristic is provided.
The purpose of the invention is achieved by the following technical solution：
A kind of sulphur quantum dot with fluorescent characteristic, is characterized in that：Sulphur quantum dot is spherical structure, from inside to outside
Include core, adsorption layer and wrapping layer successively, core is sulphur nanometer core, and adsorption layer is a variety of sulphions, and wrapping layer is dispersion dosage form
At, grain size 2nm-25nm.
The material of General Decentralized agent can be selected as：PEG-200, PEG-400 or NH3-PEG-NH3。
The present invention also provides a kind of preparation methods of the sulphur quantum dot with fluorescent characteristic, include the following steps：
1) under normal temperature and pressure, dispersant and water, after being uniformly mixed, mole of sulphur powder and dispersant are added in sulphur powder
Than for (21-0.03)：1；
2) mixture of step 1) is heated, 50 degree of -150 degree of heating temperature is uniformly slow in 1h or so while heating
The molar ratio of slow addition solid base particle or dropwise addition aqueous slkali, sulphur powder and alkali is (1-0.003):1 range；
3) heating while return stirring, 6h-150h；
4) product of step 3 is purified, obtains sulphur quantum dot colloidal sol.
Above-mentioned sulphur powder and the molar ratio of dispersant are 5.5:1, the molar ratio of sulphur powder and alkali is 0.44:1.
Above-mentioned steps 2) heating temperature be 65 degree -75 spend.
Above-mentioned dispersant is：PEG-200, PEG-400 or NH3-PEG-NH3。
Above-mentioned sulphur powder is sublimed sulfur crystal form, and alkali is sodium hydroxide, potassium hydroxide, ammonium hydroxide or carbonic acid sodium.
The present invention also provides the preparation methods of another sulphur quantum dot with fluorescent characteristic, include the following steps：
1) sulphur powder, dispersant and water and the mixed liquor of solid base particle or aqueous slkali are placed on polytetrafluoroethylliner liner
Reaction kettle in, wherein the molar ratio of sulphur powder and dispersant be (21-0.03)：1；Sulphur powder and the molar ratio of alkali are (1-0.003):
1；
2) reaction kettle heats reacts two hours at 180 DEG C；
3) product of step 2) is purified, obtains sulphur quantum dot colloidal sol.
The present invention also provides a kind of in sulphur quantum dot preparation process to the regulation and control method of its launch wavelength, including following step
Suddenly：
1) under normal temperature and pressure, dispersant and water, after being uniformly mixed, mole of sulphur powder and dispersant are added in sulphur powder
Than being 5.5:1.
2) mixture of step 1) is heated, 50 degree of -150 degree of heating temperature is uniformly slow in 1h or so while heating
The molar ratio of slow addition solid base particle or dropwise addition aqueous slkali, sulphur powder and alkali is 0.44:1 range；
3) regulate and control：
The time that control is heated to reflux stirring is 6h-30h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 540nm-
560nm；
The time that control is heated to reflux stirring is 30h-75h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 480nm-
540nm；
The time that control is heated to reflux stirring is 75h-100h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 450nm-
480nm；
The time that control is heated to reflux stirring is 100h-150h, and the maximum emission wavelength of the sulphur quantum dot of preparation exists
420nm-450nm。
It is applied in biomarker analysis using the sulphur quantum dot of the present invention.
Beneficial effects of the present invention：
The nano sulfur sol being prepared by the method for the invention has good water solubility, fluorescence and stability.
Description of the drawings
The structural schematic diagram of Fig. 1 sulphur quantum dots；1- cores, 2- adsorption layers, 3- wrapping layers；
Fig. 2 is the fluorogram of nano-sulfur quantum dot prepared by the embodiment of the present invention 5, under corresponding fluorescent lamp and ultraviolet lamp
Photo；
Fig. 3 is the microscopic appearance (transmission electron microscope picture) of the nano-sulfur quantum dot prepared in the embodiment of the present invention 7；
Fig. 4 a are the Raman figures of sublimed sulfur, and Fig. 4 b are the Raman figures of the sulphur quantum dot prepared in embodiment 7；
Fig. 5 is the XPS figures of the sulphur quantum dot prepared in the embodiment of the present invention 7；
Fig. 6 is that figure A, B, C are that sulphur quantum dot prepared by embodiment 6 places first day respectively, the 9th day, the 19th day glimmering
Photostability figure；
Fig. 7 is the regulation process schematic diagram of sulphur quantum dot emission wavelengths of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
As shown in Figure 1, a kind of sulphur quantum dot with fluorescent characteristic, sulphur quantum dot is spherical structure, from inside to outside successively
Including core 1, adsorption layer 2 and wrapping layer 3, core are sulphur nanometer core, and adsorption layer is a variety of sulphions, and wrapping layer is that dispersant is formed
, grain size 2nm-25nm.The average grain diameter for the sulphur quantum dot being typically prepared is 10nm.
The material of General Decentralized agent is mostly：PEG-200、PEG-400、NH3-PEG-NH3。
Embodiment 2：A kind of preparation method of the sulphur quantum dot with fluorescent characteristic, includes the following steps：
1) under normal temperature and pressure, dispersant and water, after being uniformly mixed, mole of sulphur powder and dispersant are added in sulphur powder
Than for (21-0.03)：1；
2) mixture of step 1) is heated, 6 degree of -150 degree of heating temperature is uniformly slow in 1h or so while heating
The molar ratio of slow addition solid base particle or dropwise addition aqueous slkali, sulphur powder and alkali is (1-0.003):1 range；When with heating
Between difference, solution colour gradually becomes shallower as by dark red orange, until light yellow.
3) heating while return stirring, 15h-150h.
4) purification process such as the product of step 3 is centrifuged or is dialysed, obtain sulphur quantum dot colloidal sol.
On the basis of embodiment 2, the optimization of reaction condition is carried out, has obtained following example 3-22：
Embodiment 23：A kind of preparation method of the sulphur quantum dot with fluorescent characteristic, includes the following steps：1) by sulphur powder,
Dispersant and water and the mixed liquor of solid base particle or aqueous slkali are placed in the reaction kettle of polytetrafluoroethylliner liner, wherein sulphur
The molar ratio of powder and dispersant is 5.5：1；Sulphur powder and the molar ratio of alkali are 0.44:1；2) reaction kettle heats reacts two at 180 DEG C
Hour；3) product of step 2) is purified, obtains sulphur quantum dot colloidal sol.
As shown in Fig. 2, the nano-sulfur quantum dot prepared in embodiment 5 is in 380nm, 400nm, under 420nm excitation wavelengths
Fluorogram；Interior illustration is the photo under corresponding fluorescent lamp and ultraviolet lamp.As can be seen that the sulphur quantum dot of synthesis is in 380nm,
Under 400nm, 420nm excitation wavelength, maximum fluorescence emission peak is at 500nm.Sulphur quantum dot is deep orange under fluorescent light, in purple
It is in light green blue under outer lamp.
Fig. 3 is the microscopic appearance (transmission electron microscope picture) of the nano-sulfur quantum dot prepared in the embodiment of the present invention 7, from Fig. 3
It can be seen that sulfur content point integral particle is relatively uniform and dispersed preferable, sulphur lateral size of dots distribution is in 2-25nm.
It can be seen that there are three significant peaks for sublimed sulfur from Fig. 4 a, respectively in 150cm-1,217cm-1And 471cm-1,
It can be seen that sulphur quantum dot made from embodiment 7 also has same characteristic peak from Fig. 4 b, show that the nano material of synthesis is sulphur object
Matter.
Fig. 5 is the XPS figures of the 2p structure sulphur quantum dots prepared in embodiment 7, and the peak at 163.25eV and 164.2eV is sulphur
Peak at the peak of atom, 167.45eV and 168.3eV is SO2 -Peak, the peak at 169.2eV is SO3 -Peak.
Fig. 6 is that sulphur quantum dot A, B, C prepared by embodiment 6 is that the sulphur quantum dot for preparing places first day respectively, the 9th day,
19th day fluorescent stability figure, as can be seen from Figure, the sulphur quantum dot sample prepared still has very well after placing 19 days
Fluorescence, show good stability.
Embodiment 24：It is a kind of in sulphur quantum dot preparation process to the regulation and control method of its launch wavelength, include the following steps：
1) under normal temperature and pressure, dispersant and water, after being uniformly mixed, mole of sulphur powder and dispersant are added in sulphur powder
Than for (21-0.03)：1；
2) mixture of step 1) is heated, 50 degree of -150 degree of heating temperature is uniformly slow in 1h or so while heating
The molar ratio of slow addition solid base particle or dropwise addition aqueous slkali, sulphur powder and alkali is (1-0.003):1 range；
3) regulate and control：
Under different material molar ratios, the maximum emission wavelength of sulfur content can be regulated and controled by the length in reaction time.
With the lengthening in reaction time, the maximum emission wavelength of obtained sulphur quantum dot is more moved to the directions Lan Bo.
The time that control is heated to reflux stirring is 15h-30h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 540nm-
560nm；
The time that control is heated to reflux stirring is 30h-75h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 480nm-
540nm；
The time that control is heated to reflux stirring is 75h-100h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 450nm-
480nm；
The time that control is heated to reflux stirring is 100h-150h, and the maximum emission wavelength of the sulphur quantum dot of preparation exists
420nm-450nm。
As shown in fig. 7, embodiment 4,5,7,8 is 5.5 in sulphur powder and the molar ratio of dispersant:1, the molar ratio of sulphur powder and alkali
It is 0.44:1, wherein A) figure be the return stirring time be 30h, the maximum emission wavelength of the sulphur quantum dot of preparation is 550nm；Its
Middle B) figure be 43h the return stirring times, the maximum emission wavelength of the sulphur quantum dot of preparation is 500nm；Wherein C) figure be reflux
Mixing time is 100h, and the maximum emission wavelength of the sulphur quantum dot of preparation is 460nm；Wherein D) figure is the return stirring time to be
The maximum emission wavelength of 125h, the sulphur quantum dot of preparation are 440nm.
It can be seen that the maximum emission wavelength of sulfur content can be regulated and controled by the length in reaction time.With the reaction time
It lengthens, the maximum emission wavelength of obtained sulphur quantum dot is more moved to the directions Lan Bo.Maximum emission wavelength is gradually moved from 550nm
500nm, 460nm and 440nm are moved, solution colour becomes faint yellow from deep orange, and in the UV lamp, solution colour gradually becomes
Navy blue.The regulation and control method that the present embodiment is previously mentioned is to be directed to specific proportioning, is found under other conditions of mixture ratios reaction conditions, is returned
It is related to the amount of sulphur to flow mixing time.The amount of sulphur is smaller, and the appearance required reaction time is shorter；The amount of opposite sulphur is more, goes out
The peak required reaction time is longer.
Embodiment 25：It can be applied in biomarker analysis using the sulphur quantum dot prepared by the present invention.
Claims (10)
1. a kind of sulphur quantum dot with fluorescent characteristic, it is characterised in that：Sulphur quantum dot is spherical structure, is wrapped successively from inside to outside
Core, adsorption layer and wrapping layer are included, core is sulphur nanometer core, and adsorption layer is a variety of sulphions, and wrapping layer is dispersant formation, grain
Diameter 2nm-25nm.
2. the sulphur quantum dot according to claim 1 with fluorescent characteristic, it is characterised in that：Dispersant is：PEG-200、
PEG-400 or NH3-PEG-NH3。
3. a kind of preparation method of the sulphur quantum dot with fluorescent characteristic, includes the following steps：
1) under normal temperature and pressure, dispersant and water are added in sulphur powder, after being uniformly mixed, the molar ratio of sulphur powder and dispersant is
(21-0.03)：1；
2) mixture of step 1) is heated, 50 DEG C -150 DEG C of heating temperature, in 1h or so while heating, uniformly slowly
Solid base particle is added or aqueous slkali is added dropwise, the molar ratio of sulphur powder and alkali is (1-0.003):1 range；
3) heating while return stirring, 6h-150h；
4) product of step 3 is purified, obtains sulphur quantum dot colloidal sol.
4. the preparation method of the sulphur quantum dot according to claim 3 with fluorescent characteristic, it is characterised in that：Sulphur powder with point
The molar ratio of powder is 5.5:1, the molar ratio of sulphur powder and alkali is 0.44:1.
5. the preparation method of the sulphur quantum dot according to claim 4 with fluorescent characteristic, it is characterised in that：Step 2)
Heating temperature is 65 DEG C -75 DEG C.
6. the preparation method of the sulphur quantum dot according to claim 5 with fluorescent characteristic, it is characterised in that：Dispersant
For：PEG-200, PEG-400 or NH3-PEG-NH3。
7. the preparation method of the sulphur quantum dot according to claim 6 with fluorescent characteristic, it is characterised in that：The sulphur powder
For sublimed sulfur crystal form, alkali is sodium hydroxide, potassium hydroxide, ammonium hydroxide or carbonic acid sodium.
8. a kind of preparation method of the sulphur quantum dot with fluorescent characteristic, includes the following steps：
1) sulphur powder, dispersant and water and the mixed liquor of solid base particle or aqueous slkali are placed on the anti-of polytetrafluoroethylliner liner
It answers in kettle, wherein the molar ratio of sulphur powder and dispersant is (21-0.03)：1；Sulphur powder and the molar ratio of alkali are (1-0.003):1；
2) reaction kettle heats reacts two hours at 180 DEG C；
3) product of step 2) is purified, obtains sulphur quantum dot colloidal sol.
9. it is a kind of in sulphur quantum dot preparation process to the regulation and control method of its launch wavelength, include the following steps：
1) under normal temperature and pressure, dispersant and water are added in sulphur powder, after being uniformly mixed, the molar ratio of sulphur powder and dispersant is
5.5:1。
2) mixture of step 1) is heated, 50 DEG C -150 DEG C of heating temperature, in 1h or so while heating, uniformly slowly
Solid base particle is added or aqueous slkali is added dropwise, the molar ratio of sulphur powder and alkali is 0.44:1 range；
3) regulate and control：
The time that control is heated to reflux stirring is 6h-30h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 540nm-560nm；
The time that control is heated to reflux stirring is 30h-75h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 480nm-
540nm；
The time that control is heated to reflux stirring is 75h-100h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 450nm-
480nm；
The time that control is heated to reflux stirring is 100h-150h, and the maximum emission wavelength of the sulphur quantum dot of preparation is in 420nm-
450nm。
10. based on application of the sulphur quantum dot in biomarker analysis prepared by claim 4.
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Cited By (10)
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| CN109810553A (en) * | 2019-01-07 | 2019-05-28 | 湖北大学 | A kind of graphene oxide composite hydroxylapatite sulfur loaded quantum dot antimicrobial coating and preparation method thereof |
| CN110129040A (en) * | 2019-05-08 | 2019-08-16 | 桂林理工大学 | A kind of preparation method of water soluble fluorescence sulphur quantum dot |
| CN110171806A (en) * | 2019-05-08 | 2019-08-27 | 桂林理工大学 | A kind of preparation method of water solubility feux rouges sulphur quantum dot |
| CN110387224A (en) * | 2019-07-23 | 2019-10-29 | 江苏海洋大学 | A kind of method and purposes improving sulphur quantum dot fluorescence property |
| CN110395698A (en) * | 2019-07-10 | 2019-11-01 | 清华大学 | A kind of chemical admixture solution and its preparation method and application |
| CN111218272A (en) * | 2020-02-06 | 2020-06-02 | 桂林理工大学 | Preparation method of fluorescent sulfur quantum dots based on sulfur-amine solution |
| CN111218285A (en) * | 2020-02-06 | 2020-06-02 | 桂林理工大学 | Preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed solution |
| CN111420678A (en) * | 2020-01-19 | 2020-07-17 | 西安科技大学 | Based on H2O2Method for preparing nano sulfur materials with different shapes by regulation and control |
| CN112777570A (en) * | 2021-01-19 | 2021-05-11 | 中南大学 | Synthesis of sulfur nanosheets and application thereof in drug delivery |
| CN116814248A (en) * | 2023-06-30 | 2023-09-29 | 常州大学 | Preparation method and application of hybridization sulfur quantum dot with room temperature afterglow |
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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 |
| CN110129040A (en) * | 2019-05-08 | 2019-08-16 | 桂林理工大学 | A kind of preparation method of water soluble fluorescence sulphur quantum dot |
| CN110171806A (en) * | 2019-05-08 | 2019-08-27 | 桂林理工大学 | A kind of preparation method of water solubility feux rouges sulphur quantum dot |
| 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 |
| CN110395698A (en) * | 2019-07-10 | 2019-11-01 | 清华大学 | A kind of chemical admixture solution and its preparation method and application |
| CN110395698B (en) * | 2019-07-10 | 2021-10-08 | 清华大学 | Chemical additive solution and preparation method and application thereof |
| CN110387224A (en) * | 2019-07-23 | 2019-10-29 | 江苏海洋大学 | A kind of method and purposes improving sulphur quantum dot fluorescence property |
| 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 |
| CN111420678A (en) * | 2020-01-19 | 2020-07-17 | 西安科技大学 | Based on H2O2Method for preparing nano sulfur materials with different shapes by regulation and control |
| 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 |
| 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 |
| CN111218285A (en) * | 2020-02-06 | 2020-06-02 | 桂林理工大学 | Preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed solution |
| CN111218272A (en) * | 2020-02-06 | 2020-06-02 | 桂林理工大学 | Preparation method of fluorescent sulfur quantum dots based on sulfur-amine solution |
| CN112777570A (en) * | 2021-01-19 | 2021-05-11 | 中南大学 | Synthesis of sulfur nanosheets and application thereof in drug delivery |
| CN116814248A (en) * | 2023-06-30 | 2023-09-29 | 常州大学 | Preparation method and application of hybridization sulfur quantum dot with room temperature afterglow |
| 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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