CN102517024B - Method for water-phase microwave preparation of CdSeS quantum dots - Google Patents

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

Info

Publication number
CN102517024B
CN102517024B CN2011104299682A CN201110429968A CN102517024B CN 102517024 B CN102517024 B CN 102517024B CN 2011104299682 A CN2011104299682 A CN 2011104299682A CN 201110429968 A CN201110429968 A CN 201110429968A CN 102517024 B CN102517024 B CN 102517024B
Authority
CN
China
Prior art keywords
solution
cadmium chloride
quantum dot
cdses
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN2011104299682A
Other languages
Chinese (zh)
Other versions
CN102517024A (en
Inventor
周培疆
詹红菊
丁玲
何振宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan University WHU
Original Assignee
Wuhan University WHU
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan University WHU filed Critical Wuhan University WHU
Priority to CN2011104299682A priority Critical patent/CN102517024B/en
Publication of CN102517024A publication Critical patent/CN102517024A/en
Application granted granted Critical
Publication of CN102517024B publication Critical patent/CN102517024B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Luminescent Compositions (AREA)

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, the quantum point grain diameter synthesized 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 for the detection of metal ion.
Background technology
The CdSe quantum dot is because having the adjustable characteristics of luminescence of size (light emitting region covers the whole visible region from the blue light to ruddiness), and the wide emission full width at half maximum (FWHM) that excites scope, relative narrower and the high characteristics such as luminescent quantum productive rate become one of quantum dot of people's most study.And the high quality CdSe quantum dot synthesized now directly synthesizes all by organic synthesis the quantum dot obtained in water, not only peak width at half height is very wide, and quantum yield is low, can't be applied to biomarker.Therefore in water, how to synthesize 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 before use in PBS solution or, in deionized water, obtains the CdSeS quantum dot solution.This quantum dot preparation technology is simple fast, processing parameter is easy to control, without last handling process, desired raw material is cheap, the quantum point grain diameter synthesized little (2-4nm) and size-grade distribution are than homogeneous, fluorescence quantum yield higher (≈ 30%), by with the biomolecules coupling after can be used as the biological fluorescent labelling material, also can be for the detection of metal 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, the close europeanized reagent of Tianjin section development centre), Cadmium chloride fine powder (CdCl 22.5H 2O, Chemical Reagent Co., Ltd., Sinopharm Group), thiohydracrylic acid (MPA, Japan), all the other are the aqueous solution.In the present invention, with thiohydracrylic acid, be stablizer and sulphur source, the sodium thiosulfate of take is selenium source, by microwave heating, prepare the CdSeS alloy quantum dot, the quantum dot obtained 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%).The 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 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 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) reaction prepare sodium thiosulfate solution: take respectively 0.7890~2.3670g selenium powder and 2.5208~7.5624g S-WAT in the 250mL there-necked flask, add wherein 60~80mL deionized water, water-bath backflow (80~95 ℃) reaction 8~10h becomes light yellow transparent liquid to solution, stopped heating.Naturally cooling to after normal temperature (20-25 ℃, below identical) in the volumetric flask that proceeds to 100mL and be settled to scale with deionized water, is the sodium thiosulfate solution of 0.10~0.30mol/L, and reaction equation is as follows:
Se+Na 2SO 3=Na 2SeSO 3
2. take 0.2284~2.2835g Cadmium chloride fine powder (CdCl 22.5H 2O) crystal, be settled to 100mL with deionized water dissolving, obtains 0.01~0.10mol/L cadmium chloride solution;
3. take 0.1061~1.0614g thiohydracrylic acid (MPA), be settled to 100mL with the deionized water dilution, obtain the thiohydracrylic acid solution of 0.01~0.10mol/L;
4. remove ionized water 95~200mL, add respectively successively 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, with the sodium hydroxide solution of 1~5mol/L, regulating the pH value is 8-10, after passing into nitrogen 10-30min, add 0.104mL0.10~0.30mol/L sodium thiosulfate solution, continue ventilatory response 4-6min;
5. the mixed solution in step 4 is sub-packed in the tetrafluoroethylene counteracting tank with every tank 50ml, in 120~150 ℃ of lower microwave heating 20-40min, namely 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 to purify, namely obtain CdSeS quantum dot pressed powder after being placed in again the lyophilizer inner drying after first freezing in the refrigerator of-20 ℃.Powder is again water-soluble, with the ethanolic soln of rhodamine 6G, make reference, in the 354nm place, measure uv-absorbing, and excite and measure the fluorescence emission peak peak area with 354nm, record its fluorescence quantum yield and be about 30%, higher than the bibliographical information value.Under the JEM-2100 high resolution transmission electron microscopy, observe its pattern and particle diameter, 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, require the absolute anaerobic of precursor solution, so sodium selenide or the necessary fresh preparation of Selenium hydride.And the selenium source in present method is sodium thiosulfate solution, after hydrothermal method is synthetic, be mixed with certain density storing solution, be placed in brown bottle and refrigerate in refrigerator, stability high (undergoing no deterioration in some months), can ready access upon use, has simplified synthesis step.
3. adopt standby this quantum dot of micro-those legal systems, be different from the conventional heating mode, rate of heating is fast, and generated time is short, and the quantum dot size-grade distribution homogeneous synthesized, and degree of 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 be directly used in cell marking.
Embodiment
Embodiment 1:
Below by embodiment, further illustrate outstanding feature of the present invention, 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, the close europeanized reagent of Tianjin section development centre), Cadmium chloride fine powder (CdCl 22.5H 20, Chemical Reagent Co., Ltd., Sinopharm Group), thiohydracrylic acid (MPA, Japan), all the other are the aqueous solution.
In 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 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) reaction prepare sodium thiosulfate solution: take respectively 2.3670g selenium powder and 7.5624g S-WAT in the 250mL there-necked flask, add wherein the 80mL deionized water, 80~95 ℃ of back flow reaction 8 of water-bath or 9 or 10h to solution, become light yellow transparent liquid, stopped heating.Naturally cool to after room temperature (20-25 ℃, below identical) in the volumetric flask that proceeds to 100mL and be settled to scale with deionized water, being the sodium thiosulfate solution of 0.30mol/L, reaction equation is as follows:
Se+Na 2SO 3=Na 2SeSO 3
2. take 0.2284g Cadmium chloride fine powder (CdCl 22.5H 2O) crystal, be settled to 100mL with deionized water dissolving, obtains the 0.01mol/L cadmium chloride solution;
3. take 0.1061g thiohydracrylic acid (MPA), be settled to 100mL with the deionized water dilution, obtain the thiohydracrylic acid solution of 0.01mol/L;
4. remove ionized water 140mL, add respectively successively the cadmium chloride solution of 20mL0.01mol/L, the thiohydracrylic acid solution of 40mL0.01mol/L, with the sodium hydroxide solution of 1mol/L, regulating the pH value is 8 or 8.5, after passing into nitrogen 30min, add 0.667mL0.30mol/L sodium thiosulfate solution, continue ventilatory response 5min;
5. above-mentioned mixed solution is sub-packed in the tetrafluoroethylene counteracting tank with every tank 50ml, in 120 ℃ of lower microwave heating 40min, namely 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 obtained is 11.7~13.4%.
Embodiment 2:
A kind of CdSeS alloy quantum dot, it consists of: selenium powder (Se, the close europeanized reagent of Tianjin section development centre), Cadmium chloride fine powder (CdCl 22.5H 2O, Chemical Reagent Co., Ltd., Sinopharm Group), thiohydracrylic acid (MPA, Japan), all the other are the aqueous solution.
In 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 is 9~9.5.
A kind of microwave assisted synthesizing method of CdSeS alloy quantum dot, the steps include:
1. take respectively 1.1835g selenium powder and 3.7812g S-WAT 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, stopped heating.Naturally cool to after room temperature (20~25 ℃) in the volumetric flask that proceeds to 100mL and be settled to scale with deionized water, being the sodium thiosulfate solution of 0.15mol/L, reaction equation is as follows:
Se+Na 2SO 3=Na 2SeSO 3
2. get anaerobic deionized water 200mL, add respectively successively the cadmium chloride solution of 2.5mL0.10mol/L, the thiohydracrylic acid solution of 6mL0.10mol/L, with the sodium hydroxide solution of 5mol/L, regulating the pH value is 9 or 9.5, after passing into nitrogen 30min, add 0.208mL0.15mol/L sodium thiosulfate solution, continue ventilatory response 5min;
3. above-mentioned mixed solution is sub-packed in the tetrafluoroethylene counteracting tank with every tank 50ml, in 130 ℃ of lower microwave heating 30~40min, namely 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 obtained is 27.3~30.8%.
Other implementation step is identical with embodiment 1.
Embodiment 3:
1. take respectively 2.3670g selenium powder and 7.5624g S-WAT in the 250mL there-necked flask, add wherein the 80mL deionized water, 90 ℃ of back flow reaction 8 of water-bath 9 or 10h to the solution clear, the completely dissolve of black selenium powder, remove the thermal source stopped heating.Naturally cool to after room temperature (20~25 ℃) in the volumetric flask that proceeds to 100mL and be settled to scale with deionized water, being the sodium thiosulfate solution of 0.30mol/L, reaction equation is as follows:
Se+Na 2SO 3=Na 2SeSO 3
2. get anaerobic deionized water 200mL, add respectively successively the cadmium chloride solution of 2.5mL0.10mol/L, the thiohydracrylic acid solution of 6mL0.10mol/L, with the sodium hydroxide solution of 5mol/L, regulating the pH value is 8 or 9 or 10, after passing into nitrogen 30min, add 0.166mL0.30mol/L sodium thiosulfate solution, continue ventilatory response 5min;
3. above-mentioned mixed solution is sub-packed in the tetrafluoroethylene counteracting tank with every tank 50ml, in 140 ℃ of lower microwave heating 20~25min, namely 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 obtained 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 react with S-WAT and prepare sodium thiosulfate solution: take respectively 0.7890 ~ 2.3670g selenium powder and 2.5208 ~ 7.5624g S-WAT in the 250mL there-necked flask, add wherein the 80mL deionized water, water-bath back flow reaction 8 ~ 10h becomes light yellow transparent liquid to solution, stopped heating, naturally cool to after normal temperature in the volumetric flask that proceeds to 100mL and be settled to scale with deionized water, be the sodium thiosulfate solution of 0.10~0.30mol/L, reaction equation is as follows:
Se+Na 2SO 3?=?Na 2SeSO 3
B, take 0.2284~2.2835g Cadmium chloride fine powder crystal, be settled to 100mL with deionized water dissolving, obtain 0.01~0.10mol/L cadmium chloride solution;
C, take 0.1061~1.0614g thiohydracrylic acid, be settled to 100mL with the deionized water dilution, obtain the thiohydracrylic acid solution of 0.01~0.10mol/L;
D, remove ionized water 95~200mL, add respectively successively 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, with the sodium hydroxide solution of 1~5mol/L, regulating the pH value is 8-10, after passing into nitrogen 10-30 min, add 0.104mL0.10~0.30mol/L sodium thiosulfate solution, continue ventilatory response 4-6min;
E, the mixed solution in the D step is sub-packed in the tetrafluoroethylene counteracting tank with every tank 50ml, in 120-150 ℃ of lower microwave heating 20-40min, namely 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, add Virahol purify and lyophilize after namely obtain CdSeS quantum dot pressed powder.
CN2011104299682A 2011-12-19 2011-12-19 Method for water-phase microwave preparation of CdSeS quantum dots Expired - Fee Related CN102517024B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011104299682A CN102517024B (en) 2011-12-19 2011-12-19 Method for water-phase microwave preparation of CdSeS quantum dots

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011104299682A CN102517024B (en) 2011-12-19 2011-12-19 Method for water-phase microwave preparation of CdSeS quantum dots

Publications (2)

Publication Number Publication Date
CN102517024A CN102517024A (en) 2012-06-27
CN102517024B true CN102517024B (en) 2013-11-27

Family

ID=46288101

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011104299682A Expired - Fee Related CN102517024B (en) 2011-12-19 2011-12-19 Method for water-phase microwave preparation of CdSeS quantum dots

Country Status (1)

Country Link
CN (1) CN102517024B (en)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104059670B (en) * 2014-06-11 2016-02-24 武汉大学 A kind of aqueous 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
CN106128772B (en) * 2016-07-18 2018-02-06 合肥工业大学 A kind of preparation method of vulcanized lead quantum dot photovoltaic battery
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
CN106847995A (en) * 2017-01-16 2017-06-13 南阳师范学院 Light-sensitive material for preparing the photo resistance of response ultraviolet-visible
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
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
CN108084993B (en) * 2017-12-22 2021-02-12 安徽工业大学 Preparation method of luminous adjustable copper-doped zinc sulfide quantum dot
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
CN110993357B (en) * 2019-12-24 2021-06-01 陕西理工大学 CdS1-xSexPreparation method of alloy quantum dot sensitized photoanode
CN111349968B (en) * 2020-03-29 2022-01-25 四川大学 Synthesis method of selenium cadmium sulfide polycrystal
CN114058368B (en) * 2021-12-20 2023-09-19 河南大学 Quantum dot with alloyed core-shell structure and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101104806A (en) * 2006-07-13 2008-01-16 天津游瑞量子点技术发展有限公司 Method for preparing hydrophilic CdSeS quantum dots
CN102127446A (en) * 2011-01-13 2011-07-20 武汉大学 Aqueous phase preparation method of ZnSe/ZnS core-shell structure quantum dots

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101104806A (en) * 2006-07-13 2008-01-16 天津游瑞量子点技术发展有限公司 Method for preparing hydrophilic CdSeS quantum dots
CN102127446A (en) * 2011-01-13 2011-07-20 武汉大学 Aqueous phase preparation method of ZnSe/ZnS core-shell structure quantum dots

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Tuning the internal structures of CdSeS nanoparticles by using different selenium and sulphur precursors;Xianfeng Chen, et al.;《Materials Science and Engineering B》;20101231;第166卷;第14-18页(2.1. Materials,2.2. Synthesis procedures,3. Results and discussion) *
Xianfeng Chen, et al..Tuning the internal structures of CdSeS nanoparticles by using different selenium and sulphur precursors.《Materials Science and Engineering B》.2010,第166卷

Also Published As

Publication number Publication date
CN102517024A (en) 2012-06-27

Similar Documents

Publication Publication Date Title
CN102517024B (en) Method for water-phase microwave preparation of CdSeS quantum dots
Wang et al. Synthesis and luminescence behavior of Eu3+-doped CaF2 nanoparticles
Yang et al. Fast synthesize ZnO quantum dots via ultrasonic method
CN102517025B (en) Preparation method of ZnSe/ZnS core-shell quantum dots
Niu et al. Controllable synthesis and up-conversion properties of tetragonal BaYF5: Yb/Ln (Ln= Er, Tm, and Ho) nanocrystals
Zhao et al. Cross-relaxation and non-steady-state processes induced up-conversion color modulation in Gd2O3: Ln3+/Er3+ (Ln= Tm, Ho)
Xu et al. Controllable synthesis of all inorganic lead halide perovskite nanocrystals and white light-emitting diodes based on CsPbBr3 nanocrystals
Chen et al. Room-temperature ionic-liquid-assisted hydrothermal synthesis of Ag-In-Zn-S quantum dots for WLEDs
Li et al. Aqueous synthesis of highly monodispersed thiol-capped CdSe quantum dots based on the electrochemical method
CN105199735B (en) A kind of preparation method of solid state quantum point
Jiao et al. Controllable Synthesis of Upconversion Nanophosphors toward Scale‐Up Productions
CN104059670B (en) A kind of aqueous phase preparation method of CdTeSeS alloy quantum dot
Qian et al. Synthesis and downconversion emission property of Yb2O3: Eu3+ nanosheets and nanotubes
Rong et al. Aqueous synthesis of CdSe and CdSe/CdS quantum dots with controllable introduction of Se and S sources
Gao et al. Sol-gel synthesis of β-NaYF4: Yb3+/Nd3+/Tm3+/Mn2+ nanophosphors and color-tunable upconversion luminescence
Zhao et al. Ba2GdF7 nanocrystals: Solution-based synthesis, growth mechanism, and luminescence properties
Wu et al. The photoluminescence properties of Y2O3: Eu3+ prepared by surfactant assisted co-precipitation-molten salt synthesis
Wang et al. Nanocomposites of CsPbBr3 perovskite quantum dots embedded in Gd2O3: Eu3+ hollow spheres for LEDs application
Ma et al. Microwave-assisted preparation of nearly monodisperse flower-like CaF2 microspheres
Zhou et al. Shape-controlled synthesis of one-dimensional cesium lead halide perovskite nanocrystals: methods and advances
Li et al. La3+ as impurity ions for the synthesis of β-NaLuF4 nanocrystals with high luminance and small size
Wang et al. BiPO4: Ln3+ (Ln= Eu, Tb, Eu/Tb) nanorods: Room-temperature synthesis, reaction mechanism, and color-tunable emission
CN104974742A (en) Method for microwave-assisted preparation of CdTeSeS/ZnTe core-shell quantum dot in water
Zhai et al. Hydrothermal synthesis, characterization and luminescence properties of orange–red-emitting phosphors SnO 2: Eu
Gao et al. Simultaneous luminescence enhancement and lifetime tuning of deep UV-NIR upconversion through controlling dopant concentration

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20131127

Termination date: 20191219

CF01 Termination of patent right due to non-payment of annual fee