CN102517024A - Method for water-phase microwave preparation of CdSeS quantum dots - Google Patents

Method for water-phase microwave preparation of CdSeS quantum dots Download PDF

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CN102517024A
CN102517024A CN2011104299682A CN201110429968A CN102517024A CN 102517024 A CN102517024 A CN 102517024A CN 2011104299682 A CN2011104299682 A CN 2011104299682A CN 201110429968 A CN201110429968 A CN 201110429968A CN 102517024 A CN102517024 A CN 102517024A
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cadmium chloride
quantum dot
cdses
water
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CN102517024B (en
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周培疆
詹红菊
丁玲
何振宇
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Wuhan University WHU
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Abstract

The invention discloses a method for water-phase microwave preparation of CdSeS quantum dots. The method provided by the invention comprises the following steps of 1, preparing a selenosulfate solution through the reaction of selenium powder and a sodium sulfite solution, 2, weighing cadmium chloride crystals, and carrying out dissolution and volume metering by deionized water to obtain a cadmium chloride solution, 3, adding a certain amount of mercaptopropionic acid into the cadmium chloride solution, 4, adjusting a pH value of the mixed solution obtained by the step 3 to a specific pH value by a sodium hydroxide solution, 5, feeding inert gas into the mixed solution having the specific pH value to remove oxygen, and adding the selenosulfate solution obtained by the step 1 into the oxygen-free mixed solution, 6, loading the mixed solution obtained by the step 5 into a teflon-made digestion tank, and heating for a reaction by a microwave digestion furnace, and 7, cooling the reaction products obtained by the step 6 to a room temperature, adding isopropanol into the cooled reaction products, carrying out purification, and drying by a freezer dryer to obtain solid powder of the CdSeS quantum dots. The method provided by the invention is fast and simple, has easily controllable technological parameters, has a low cost, realizes small sizes and even size distribution of the CdSeS quantum dots obtained by the method, and has a high fluorescent quantum yield. The CdSeS quantum dots obtained by the method can be utilized as a biological fluorescent label material through coupling with biomolecules and can also be utilized for metal ion detection.

Description

A kind of water microwave preparation of CdSeS quantum dot
Technical field
The present invention relates to the synthetic of fluorescent nano material; The water microwave preparation that more specifically relates to a kind of CdSeS quantum dot; Quantum point grain diameter that synthesizes little (2-4nm) and size-grade distribution homogeneous; Fluorescence quantum efficiency is higher, after modifying, can be used as the biological fluorescent labelling material, also can be used for the detection of metals ion.
Background technology
The characteristics of luminescence (light emitting region cover whole visible region from blue light to ruddiness) of CdSe quantum dot because of having size adjustable, wide emission full width at half maximum (FWHM) that excites scope, relative narrower and high characteristics such as luminescent quantum productive rate become people and study one of maximum quantum dot.And the high quality CdSe quantum dot that synthesizes now is all by organic synthesis, the directly synthetic quantum dot that obtains of aqueous phase, and not only peak width at half is very wide, and quantum yield is low, can't be applied to biomarker.Therefore how aqueous phase synthesizes the focus that high-quality CdSe quantum dot has become research.
Summary of the invention
The objective of the invention is to be to provide a kind of microwave-assisted preparation method of CdSeS alloy quantum dot, this powder is dissolved in the PBS solution before use or in the deionized water, gets the CdSeS quantum dot solution.This quantum dot preparation technology is simple fast; Processing parameter is easy to control, need not last handling process, and desired raw material is cheap; Quantum point grain diameter that synthesizes little (2-4nm) and size-grade distribution are than homogeneous; Fluorescence quantum yield higher (≈ 30%), through with the biomolecules coupling after can be used as the biological fluorescent labelling material, also can be used for the detection of metals ion.
In order to realize above-mentioned purpose, the present invention adopts following technical measures:
Its technical conceive is: a kind of CdSeS alloy quantum dot, it consists of: selenium powder (Se, Tianjin section close europeanized reagent development centre), Cadmium chloride fine powder (CdCl 22.5H 2O, Chemical Reagent Co., Ltd., Sinopharm Group), (MPA, Japan), all the other are the aqueous solution to thiohydracrylic acid.Among the present invention; Use thiohydracrylic acid to be stablizer and sulphur source; With the sodium thiosulfate is selenium source, prepares the CdSeS alloy quantum dot through microwave heating, and the quantum dot that obtains is particle diameter little (2-4nm) and size-grade distribution homogeneous not only; Fluorescence quantum efficiency higher (30%-40%, pertinent literature is reported as 25%).This method has overcome the synthetic CdSeS quantum dot long reaction time of hydrothermal method, and size-grade distribution is wide, the limitation that quantum yield is not high.
In the described CdSeS alloy quantum dot, selenium powder (Se), Cadmium chloride fine powder (CdCl 22.5H 2O), the molar ratio of thiohydracrylic acid (MPA) is 1/5～1/10: heat 20-40min under 1: 1.7～2.4,120～150 ℃ conditions.
Described pH value of solution value is 8-10.
A kind of water microwave preparation of CdSeS quantum dot the steps include:
1. selenium powder (Se) and S-WAT (Na 2SO 3) prepared in reaction sodium thiosulfate solution: take by weighing 0.7890～2.3670g selenium powder and 2.5208～7.5624g S-WAT respectively in the 250mL there-necked flask; To wherein adding 60～80mL deionized water; Water-bath (80～95 ℃) reaction 8～10h that refluxes becomes light yellow transparent liquid to solution, stops heating.Naturally cooling in the volumetric flask that changes 100mL behind the normal temperature (20-25 ℃, below identical) over to and with deionized water and be settled to scale, is the sodium thiosulfate solution of 0.10～0.30mol/L, and reaction equation is following:
Se+Na 2SO 3＝Na 2SeSO 3；
2. take by weighing 0.2284～2.2835g Cadmium chloride fine powder (CdCl 22.5H 2O) crystal is settled to 100mL with deionized water dissolving, obtains 0.01～0.10mol/L cadmium chloride solution;
3. take by weighing 0.1061～1.0614g thiohydracrylic acid (MPA), be settled to 100mL, get the thiohydracrylic acid solution of 0.01～0.10mol/L with the deionized water dilution;
4. remove ionized water 95～200mL; Add the cadmium chloride solution of 0.520～31.2mL0.01～0.10mol/L, the thiohydracrylic acid solution of 0.884～74.88mL0.01～0.10mol/L successively respectively; Use the sodium hydroxide solution adjusting pH value of 1～5mol/L to be 8-10; Add 0.104mL0.10～0.30mol/L sodium thiosulfate solution after feeding nitrogen 10-30min, continue ventilatory response 4-6min;
5. the mixed solution in the step 4 is sub-packed in the tetrafluoroethylene counteracting tank with every jar of 50ml; In 120～150 ℃ of following microwave heating 20-40min; Promptly make aqueous CdSeS quantum dot, the molar ratio of sodium thiosulfate, Cadmium chloride fine powder, thiohydracrylic acid is respectively 1/5～1/10: 1: 1.7～2.4;
6. add Virahol and purify, promptly obtain CdSeS quantum dot pressed powder after in-20 ℃ refrigerator, placing the lyophilizer inner drying again after earlier freezing.Powder is water-soluble again, make reference with the ethanolic soln of rhodamine 6G, measure uv-absorbing in the 354nm place, and excite mensuration fluorescence emission peak peak area with 354nm, record its fluorescence quantum yield and be about 30%, be higher than the bibliographical information value.Observe its pattern and particle diameter down in the JEM-2100 high resolution transmission electron microscopy, median size is 2-3nm, is significantly less than bibliographical information value (12nm).
The present invention compared with prior art has the following advantages and effect:
1. this quantum dot main raw material source is abundant, cheap, and synthetic cost is low.
2. severe reaction conditions when traditional selenium source (sodium selenide or Selenium hydride etc.) synthesizes quantum dot requires the absolute anaerobic of precursor solution, so sodium selenide or the necessary prepared fresh of Selenium hydride.And the selenium source in present method is a sodium thiosulfate solution, after hydrothermal method is synthetic, is mixed with certain density storing solution, places brown bottle in refrigerator, to refrigerate, and stability high (undergoing no deterioration in the some months) can ready access upon use, has simplified synthesis step.
3. adopt little those these quantum dots of method preparation, be different from conventional type of heating, rate of heating is fast, and generated time is short, and the quantum dot size-grade distribution homogeneous that synthesizes, and percent crystallinity is high.
4. this preparation technology is simple, processing parameter (molar ratio of selenium powder, Cadmium chloride fine powder, thiohydracrylic acid is 1/5～1/10: 1: 1.7～2.4, the pH value is 8～10, be that 20-40min, Heating temperature are 120-150 ℃ heat-up time) easy to control.
5. this quantum point grain diameter little (2-4nm), the size-grade distribution homogeneous, and have higher fluorescence quantum yield (reaching more than 30%), can directly be used for cell marking.
Embodiment
Embodiment 1:
Through embodiment, further illustrate outstanding feature of the present invention below, only be the present invention is described and never limit the present invention.
A kind of CdSeS alloy quantum dot, it consists of: selenium powder (Se, Tianjin section close europeanized reagent development centre), Cadmium chloride fine powder (CdCl 22.5H 20, Chemical Reagent Co., Ltd., Sinopharm Group), (MPA, Japan), all the other are the aqueous solution to thiohydracrylic acid.
In the described CdSeS alloy quantum dot, selenium powder (Se), Cadmium chloride fine powder (CdCl 22.5H 2O), the molar ratio of thiohydracrylic acid (MPA) is 0.2: 1: 2.0, heats 20-40min under 120～150 ℃ of conditions.
Described pH value of solution value is 8-10.
A kind of microwave assisted synthesizing method of CdSeS alloy quantum dot the steps include:
1. selenium powder (Se) and S-WAT (Na 2SO 3) prepared in reaction sodium thiosulfate solution: take by weighing 2.3670g selenium powder and 7.5624g S-WAT respectively in the 250mL there-necked flask; To wherein adding the 80mL deionized water; 80～95 ℃ of back flow reaction 8 of water-bath or 9 or 10h become light yellow transparent liquid to solution, stop heating.Naturally cool in the volumetric flask that changes 100mL after the room temperature (20-25 ℃, below identical) over to and with deionized water and be settled to scale, be the sodium thiosulfate solution of 0.30mol/L, reaction equation is following:
Se+Na 2SO 3＝Na 2SeSO 3；
2. take by weighing 0.2284g Cadmium chloride fine powder (CdCl 22.5H 2O) crystal is settled to 100mL with deionized water dissolving, obtains the 0.01mol/L cadmium chloride solution;
3. take by weighing 0.1061g thiohydracrylic acid (MPA), be settled to 100mL, get the thiohydracrylic acid solution of 0.01mol/L with the deionized water dilution;
4. remove ionized water 140mL; Add the cadmium chloride solution of 20mL0.01mol/L, the thiohydracrylic acid solution of 40mL0.01mol/L successively respectively; Using the sodium hydroxide solution adjusting pH value of 1mol/L is 8 or 8.5; Add 0.667mL0.30mol/L sodium thiosulfate solution after feeding nitrogen 30min, continue ventilatory response 5min;
5. above-mentioned mixed solution is sub-packed in the tetrafluoroethylene counteracting tank with every jar of 50ml, in 120 ℃ of following microwave heating 40min, promptly making concentration is 1.0mmol/L CdSeS quantum dot, sodium thiosulfate (Na 2SeSO 3), Cadmium chloride fine powder (CdCl 22.5H 2O), the molar ratio of thiohydracrylic acid (MPA) is 0.2: 1: 2.0, the quantum dot fluorescence quantum yield that obtains is 11.7～13.4%.
Embodiment 2:
A kind of CdSeS alloy quantum dot, it consists of: selenium powder (Se, Tianjin section close europeanized reagent development centre), Cadmium chloride fine powder (CdCl 22.5H 2O, Chemical Reagent Co., Ltd., Sinopharm Group), (MPA, Japan), all the other are the aqueous solution to thiohydracrylic acid.
In the described CdSeS alloy quantum dot, sodium thiosulfate (Na 2SeSO 3), Cadmium chloride fine powder (CdCl 22.5H 2O), the molar ratio of thiohydracrylic acid (MPA) is 0.125: 1: 2.4, heats 30-40min under 130 ℃ of conditions.
Described pH value of solution value is 9～9.5.
A kind of microwave assisted synthesizing method of CdSeS alloy quantum dot the steps include:
1. take by weighing 1.1835g selenium powder and 3.7812g S-WAT respectively in the 250mL there-necked flask, add the 85mL deionized water, 95 ℃ of back flow reaction 8 of water-bath 9 or 10h to the solution clear, remove thermal source, stop heating.Naturally cool in the volumetric flask that changes 100mL after the room temperature (20～25 ℃) over to and with deionized water and be settled to scale, be the sodium thiosulfate solution of 0.15mol/L, reaction equation is following:
Se+Na 2SO 3＝Na 2SeSO 3；
2. get anaerobic deionized water 200mL; Add the cadmium chloride solution of 2.5mL0.10mol/L, the thiohydracrylic acid solution of 6mL0.10mol/L successively respectively; Using the sodium hydroxide solution adjusting pH value of 5mol/L is 9 or 9.5; Add 0.208mL0.15mol/L sodium thiosulfate solution after feeding nitrogen 30min, continue ventilatory response 5min;
3. above-mentioned mixed solution is sub-packed in the tetrafluoroethylene counteracting tank with every jar of 50ml; In 130 ℃ of following microwave heating 30～40min; Promptly making concentration is 1.25mmol/L CdSeS quantum dot; The molar ratio of Cadmium chloride fine powder, sodium thiosulfate, thiohydracrylic acid was respectively 1: 0.125: 2.4, and the quantum dot fluorescence quantum yield that obtains is 27.3～30.8%.
Other implementation step is identical with embodiment 1.
Embodiment 3:
1. take by weighing 2.3670g selenium powder and 7.5624g S-WAT respectively in the 250mL there-necked flask, to wherein adding the 80mL deionized water, 90 ℃ of back flow reaction 8 of water-bath or 9 or 10h to the solution clear, the completely dissolve of black selenium powder is removed thermal source and is stopped heating.Naturally cool in the volumetric flask that changes 100mL after the room temperature (20～25 ℃) over to and with deionized water and be settled to scale, be the sodium thiosulfate solution of 0.30mol/L, reaction equation is following:
Se+Na 2SO 3＝Na 2SeSO 3；
2. get anaerobic deionized water 200mL; Add the cadmium chloride solution of 2.5mL0.10mol/L, the thiohydracrylic acid solution of 6mL0.10mol/L successively respectively; Using the sodium hydroxide solution adjusting pH value of 5mol/L is 8 or 9 or 10; Add 0.166mL0.30mol/L sodium thiosulfate solution after feeding nitrogen 30min, continue ventilatory response 5min;
3. above-mentioned mixed solution is sub-packed in the tetrafluoroethylene counteracting tank with every jar of 50ml; In 140 ℃ of following microwave heating 20～25min; Promptly making concentration is 1.25mmol/L CdSeS quantum dot; The molar ratio of Cadmium chloride fine powder, sodium thiosulfate, thiohydracrylic acid was respectively 1: 0.2: 2.4, and the quantum dot fluorescence quantum yield that obtains is 20.3～24.6%.
Other implementation step is identical with embodiment 1.

Claims (1)

1. the water microwave preparation of a CdSeS quantum dot the steps include:
A, selenium powder and S-WAT prepared in reaction sodium thiosulfate solution: take by weighing 0.7890 ~ 2.3670g selenium powder and 2.5208 ~ 7.5624g S-WAT respectively in the 250mL there-necked flask; To wherein adding the 80mL deionized water; Water-bath back flow reaction 8 ~ 10h becomes light yellow transparent liquid to solution, stops heating, naturally cools in the volumetric flask that changes 100mL behind the normal temperature over to and with deionized water and is settled to scale; Be the sodium thiosulfate solution of 0.10～0.30mol/L, reaction equation is following:
Se+Na 2SO 3?=?Na 2SeSO 3；
B, take by weighing 0.2284～2.2835g Cadmium chloride fine powder crystal, be settled to 100mL, obtain 0.01～0.10mol/L cadmium chloride solution with deionized water dissolving;
C, take by weighing 0.1061～1.0614g thiohydracrylic acid, be settled to 100mL with the deionized water dilution, the thiohydracrylic acid solution of 0.01～0.10mol/L;
D, remove ionized water 95～200mL; Add the cadmium chloride solution of 0.520～31.2mL0.01～0.10mol/L, the thiohydracrylic acid solution of 0.884～74.88mL0.01～0.10mol/L successively respectively; Use the sodium hydroxide solution adjusting pH value of 1～5mol/L to be 8-10; Add 0.104mL0.10～0.30mol/L sodium thiosulfate solution after feeding nitrogen 10-30 min, continue ventilatory response 4-6min;
E, the mixed solution in the D step is sub-packed in the tetrafluoroethylene counteracting tank with every jar of 50ml; In 120-150 ℃ of following microwave heating 20-40min; Promptly make aqueous CdSeS quantum dot, the molar ratio of sodium thiosulfate, Cadmium chloride fine powder, thiohydracrylic acid is respectively 1/5 ~ 1/10:1:1.7～2.4;
F, adding Virahol are purified and are also promptly obtained CdSeS quantum dot pressed powder after the lyophilize.
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CN105752946A (en) * 2016-01-25 2016-07-13 王博 Method for preparing nano materials for biological labels
CN106128772A (en) * 2016-07-18 2016-11-16 合肥工业大学 A kind of preparation method of vulcanized lead quantum dot photovoltaic battery
CN106847953A (en) * 2017-01-16 2017-06-13 南阳师范学院 Light-sensitive material for preparing the photo resistance of Old plant ultraviolet-visible
CN106847994A (en) * 2017-01-16 2017-06-13 南阳师范学院 Light-sensitive material for preparing the photo resistance of low cost response ultraviolet-visible
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CN106876506A (en) * 2017-01-16 2017-06-20 南阳师范学院 Light-sensitive material for preparing the photo resistance of response ultraviolet-visible
CN108084993A (en) * 2017-12-22 2018-05-29 安徽工业大学 A kind of preparation method for the adjustable Copper-cladding Aluminum Bar ZnS quantum dots that shine
CN109453818A (en) * 2018-11-23 2019-03-12 淮北师范大学 A kind of cadmium sulphur selenium/diethylenetriamine/diamine hybrid inorganic-organic highly effective hydrogen yield material and preparation method thereof
CN110993357A (en) * 2019-12-24 2020-04-10 陕西理工大学 CdS1-xSexPreparation method of alloy quantum dot sensitized photoanode
CN111349968A (en) * 2020-03-29 2020-06-30 四川大学 Synthesis method of selenium cadmium sulfide polycrystal
CN114058368A (en) * 2021-12-20 2022-02-18 河南大学 Alloyed core-shell structure quantum dot and preparation method thereof

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Cited By (17)

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CN104059670A (en) * 2014-06-11 2014-09-24 武汉大学 Water phase preparation method of CdTeSeS alloy quantum dot
CN105752946A (en) * 2016-01-25 2016-07-13 王博 Method for preparing nano materials for biological labels
CN106128772A (en) * 2016-07-18 2016-11-16 合肥工业大学 A kind of preparation method of vulcanized lead quantum dot photovoltaic battery
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CN108084993A (en) * 2017-12-22 2018-05-29 安徽工业大学 A kind of preparation method for the adjustable Copper-cladding Aluminum Bar ZnS quantum dots that shine
CN109453818A (en) * 2018-11-23 2019-03-12 淮北师范大学 A kind of cadmium sulphur selenium/diethylenetriamine/diamine hybrid inorganic-organic highly effective hydrogen yield material and preparation method thereof
CN109453818B (en) * 2018-11-23 2022-07-15 淮北师范大学 Cadmium sulfur selenium/diethylenetriamine/diamine organic-inorganic hybrid high-efficiency hydrogen production material and preparation method thereof
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