CN107955610B - Size-adjustable up-conversion NaYF4Method for preparing nanocrystalline - Google Patents
Size-adjustable up-conversion NaYF4Method for preparing nanocrystalline Download PDFInfo
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/36—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 halogen being the only anion, e.g. NaYF4
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses an up-conversion NaYF with adjustable size4The preparation method of the nanocrystalline comprises the following steps: (1) weighing 0.35 g of sodium hydroxide, and fully dissolving the sodium hydroxide in 10ml of absolute ethyl alcohol to obtain a sodium hydroxide alcohol solution; (2) measuring 8ml of oleic acid, and adding the oleic acid into the sodium hydroxide alcoholic solution prepared in the step (1) to obtain a white viscous solution; (3) preparing 8ml of NaF (0.5mmol/ml) aqueous solution, and adding the aqueous solution into the solution obtained in the step (2) to obtain a mixed solution; (4) 2ml of different Gd prepared3+Slowly adding a rare earth nitrate solution with an ion concentration ratio into the solution obtained in the step (3) to obtain an emulsion; (5) filling the emulsion obtained in the step (4) into a polytetrafluoroethylene liner, placing the polytetrafluoroethylene liner into a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours; (6) alternately cleaning the obtained sample by using absolute ethyl alcohol and deionized water, then collecting the obtained sample by adopting a centrifugal method, and placing the collected sample in a drying oven for drying for 24 hours; the method is relatively simple in operation, free of toxic organic matters, and convenient to popularize and apply, and meets the requirement of environmental protection.
Description
Technical Field
The invention belongs to the technical field of up-conversion fluorescent nano material preparation, and Gd with different concentrations is doped3+Ion implementation of NaYF4The size of the nanocrystalline is adjustable, in particular to an up-conversion NaYF with adjustable size4A method for preparing a nanocrystal.
Background
An up-conversion material is a fluorescent material that converts infrared photons into visible photons or ultraviolet photons by absorbing them. The rare earth doped up-conversion nano material has unique optical characteristics and has wide application value in the aspects of colorful three-dimensional display, solar cells, solid lasers, LEDs, fluorescent labels and the like (Opt Mater 2016; 59: 49-54). In recent years, with the successful preparation of high-quality nanocrystals, the up-conversion nanomaterials as bio-fluorescent labels have been rapidly developed in the aspects of biological detection and the like (Anal Chim Acta 2014; 832: 1-33). Compared with the traditional dye label, the dye label has the advantages of bleaching resistance, high stability, high luminous intensity and the like.
Among the numerous rare earth doped up-conversion matrix materials, NaYF4Has lower phonon energy and higher stability, and is praised as one of the most superior up-conversion matrix materials. NaYF4The structure has two structures, one is a cubic phase structure, and the other is a hexagonal phase structure. Hexagonal NaYF phase4With cubic phase NaYF4Compared with the prior art, the method has higher up-conversion efficiency (Inorg chem 2007; 46: 6329-6337). At present, hexagonal NaYF with different shapes (rod-shaped, tubular, disc-shaped and the like) and sizes is successfully prepared by different methods4Nanocrystalline material (Ceram Int 2015; 41: s713-s 718). However for how to implement NaYF4The controlled growth of nanocrystals to achieve applications in different fields remains a challenge. Therefore, NaYF can be effectively controlled in the preparation process4The growth of the crystal has important significance in realizing the controllability of the shape and the size of the crystal.
Disclosure of Invention
The invention aims to provide a hexagonal NaYF with adjustable size4The preparation method of the nanocrystalline is basically characterized in that oleic acid is used as an emulsifier, and different Gd is adjusted3+Ion concentration, heating at 190 deg.c for 20 hr to prepare NaYF in different sizes4And (4) nanocrystals. The invention relates to a size-adjustable up-conversion NaYF4The preparation method of the nanocrystalline specifically comprises the following steps:
(1) accurately weighing 0.35 g of sodium hydroxide, and fully dissolving the sodium hydroxide in 10ml of absolute ethyl alcohol to form colorless and transparent sodium hydroxide alcoholic solution for later use;
(2) measuring 8ml of oleic acid, slowly adding the oleic acid into the sodium hydroxide alcohol solution prepared in the step (1), and strongly stirring the solution to react fully to obtain a white viscous solution mixed by the sodium oleate, the oleic acid and the alcohol;
(3) preparing 8ml of NaF (0.5mmol/ml) aqueous solution, slowly adding the aqueous solution into the solution obtained in the step (2), and strongly stirring to obtain a semitransparent mixed solution;
(4) five parts of different Gd are prepared3+Respectively dissolving 1mmol of rare earth nitrate with ion concentration ratio into 2ml of deionized water to obtain five parts of 2ml (0.5mmol/ml) of rare earth nitrate aqueous solution, slowly adding the five parts of the rare earth nitrate aqueous solution into the semitransparent mixed solution obtained in the step (3), and continuously stirring strongly for 30 minutes to obtain emulsion; wherein said Gd3+The molar concentrations of ions are respectively as follows: 5. 10, 20, 30 and 40 mol%;
(5) putting the emulsion obtained in the step (4) into a polytetrafluoroethylene liner of 30ml, placing the polytetrafluoroethylene liner in a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours to obtain a sample;
(6) and (3) alternately cleaning the sample obtained in the step (5) by using absolute ethyl alcohol and deionized water for 3-4 times, collecting the obtained sample by adopting a centrifugal method, and placing the sample in a drying oven to be dried for 24 hours under the environment of 60 ℃.
The preparation method of the invention has the following characteristics and advantages:
(1) NaYF prepared by using method4The nano crystal up-conversion fluorescent material is in a single hexagonal phase structure.
(2) NaYF prepared by using method4The nano crystal up-conversion fluorescent material is rod-shaped and has Gd3+The ion molar concentration is increased to 40 mol%, the average length is reduced from 1239nm to 318nm, and the average diameter is reduced from 194nm to 69 nm.
(3) The method is relatively simple in operation, free of toxic organic matters, and convenient to popularize and apply, and meets the requirement of environmental protection.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention.
FIG. 2 shows NaYGdF prepared in examples 1 to 5 of the present invention4:Yb3+/Er3+/Tm3+X-ray diffraction (XRD) pattern of nanocrystals, all samples were of a single hexagonal phase structure:
wherein (a) is example 1 doped with 5 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Nanocrystalline X-ray diffraction (XRD) data;
(b) example 2 doping with 10 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Nanocrystalline X-ray diffraction (XRD) data;
(c) example 3 doping with 20 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Nanocrystalline X-ray diffraction (XRD) data;
(d) example 4 doping with 30 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Nanocrystalline X-ray diffraction (XRD) data;
(e) example 5 doping with 40 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Nanocrystalline X-ray diffraction (XRD) data.
FIG. 3 shows NaYGdF prepared by the embodiments 1 to 5 of the present invention4:Yb3+/Er3+/Tm3+Scanning Electron Microscope (SEM) pictures of nanocrystals:
wherein (a) is example 1 doped with 5 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Scanning Electron Microscope (SEM) pictures of nanocrystals;
(b) example 2 doping with 10 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Scanning Electron Microscope (SEM) pictures of nanocrystals;
(c) example 3 doping with 20 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Scanning Electron Microscope (SEM) pictures of nanocrystals;
(d) example 4 doping with 30 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Scanning Electron Microscope (SEM) pictures of nanocrystals;
(e) example 5 doping with 40 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Scanning Electron Microscope (SEM) images of the nanocrystals.
FIG. 4 shows the hexagonal phase NaYGdF prepared in examples 1 to 5 of the present invention4:Yb3+/Er3+/Tm3+Upconversion fluorescence spectrogram of nanocrystalline excited by 980nm semiconductor laser:
wherein (a) is example 1 doped with 5 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Upconversion fluorescence spectra of nanocrystals;
(b) example 2 doping with 10 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Upconversion fluorescence spectra of nanocrystals;
(c) example 3 doping with 20 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Upconversion fluorescence spectra of nanocrystals;
(d) example 4 doping with 30 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Upconversion fluorescence spectra of nanocrystals;
(e) example 5 doping with 40 mmol% Gd3+Ion prepared NaYGdF4:Yb3+/Er3+/Tm3+Upconversion fluorescence spectra of nanocrystals.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1:
(1) 0.35 g of sodium hydroxide was accurately weighed and sufficiently dissolved in 10ml of anhydrous ethanol to form a colorless transparent alcoholic solution of sodium hydroxide. Measuring 8ml of oleic acid, slowly adding the oleic acid into the sodium hydroxide alcohol solution, and strongly stirring the solution for full reaction to obtain a white viscous solution mixed by the sodium oleate, the oleic acid and the alcohol.
(2) Preparing 8ml of NaF (0.5mmol/ml) aqueous solution, adding the aqueous solution into the solution obtained in the step (1), and stirring strongly to obtain a semitransparent mixed solution;
(3) weighing 1mmol of rare earth nitrate (wherein the molar percentages of Y, Gd, Yb, Er and Tm are 78.875%, 5%, 15%, 0.125% and 1%); dissolving the rare earth nitrate into 2ml of deionized water to obtain 2ml (0.5mmol/ml) of rare earth nitrate aqueous solution, slowly adding the rare earth nitrate aqueous solution into the semitransparent mixed solution obtained in the step (3), and continuously stirring strongly for 30 minutes to obtain emulsion;
(4) and (4) filling the emulsion obtained in the step (3) into a polytetrafluoroethylene liner of 30ml, placing the polytetrafluoroethylene liner into a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours. Naturally cooling to room temperature, alternately cleaning the sample with anhydrous ethanol and deionized water for 3-4 times, collecting the obtained sample by centrifugation, and drying in a drying oven at 60 deg.C for 24 hr.
As shown in FIG. 2 and FIG. 3- (a), the sample has a single hexagonal phase structure, and exhibits a rod-like morphology with an average diameter of about 194nm and an average length of about 1239 nm.
Example 2:
(1) 0.35 g of sodium hydroxide was accurately weighed and sufficiently dissolved in 10ml of anhydrous ethanol to form a colorless transparent alcoholic solution of sodium hydroxide. Measuring 8ml of oleic acid, slowly adding the oleic acid into a sodium hydroxide alcohol solution, and strongly stirring the solution for full reaction to obtain a viscous white solution mixed by the sodium oleate, the oleic acid and the alcohol;
(2) preparing 8ml of NaF (0.5mmol/ml) aqueous solution, adding the aqueous solution into the solution obtained in the step (1), and stirring strongly to obtain a semitransparent mixed solution;
(3) weighing 1mmol of rare earth nitrate (wherein the molar percentages of Y, Gd, Yb, Er and Tm are 73.875%, 10%, 15%, 0.125% and 1%); dissolving the rare earth nitrate into 2ml of deionized water to obtain 2ml (0.5mmol/ml) of rare earth nitrate aqueous solution, slowly adding the rare earth nitrate aqueous solution into the semitransparent mixed solution obtained in the step (3), and continuously stirring strongly for 30 minutes to obtain emulsion;
(4) and (4) filling the emulsion obtained in the step (3) into a polytetrafluoroethylene liner of 30ml, placing the polytetrafluoroethylene liner into a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours. Naturally cooling to room temperature, alternately cleaning the sample with anhydrous ethanol and deionized water for 3-4 times, collecting the obtained sample by centrifugation, and drying in a drying oven at 60 deg.C for 24 hr;
as shown in FIG. 2 and FIG. 3- (b), the sample was a single hexagonal phase structure, exhibiting a rod-like morphology with an average diameter of about 132nm and an average length of about 1100 nm.
Example 3:
(1) 0.35 g of sodium hydroxide was accurately weighed and sufficiently dissolved in 10ml of anhydrous ethanol to form a colorless transparent alcoholic solution of sodium hydroxide. Measuring 8ml of oleic acid, slowly adding the oleic acid into a sodium hydroxide alcohol solution, and strongly stirring the solution for full reaction to obtain a viscous white solution mixed by the sodium oleate, the oleic acid and the alcohol;
(2) preparing 8ml of NaF (0.5mmol/ml) aqueous solution, adding the aqueous solution into the solution obtained in the step (1), and stirring strongly to obtain a semitransparent mixed solution;
(3) weighing 1mmol of rare earth nitrate (wherein the molar percentages of Y, Gd, Yb, Er and Tm are 63.875%, 20%, 15%, 0.125% and 1%); dissolving the rare earth nitrate into 2ml of deionized water to obtain 2ml (0.5mmol/ml) of rare earth nitrate aqueous solution, slowly adding the rare earth nitrate aqueous solution into the semitransparent mixed solution obtained in the step (3), and continuously stirring strongly for 30 minutes to obtain emulsion;
(4) and (4) filling the emulsion obtained in the step (3) into a polytetrafluoroethylene liner of 30ml, placing the polytetrafluoroethylene liner into a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours. Naturally cooling to room temperature, alternately cleaning the sample with anhydrous ethanol and deionized water for 3-4 times, collecting the obtained sample by centrifugation, and drying in a drying oven at 60 deg.C for 24 hr.
As shown in FIG. 2 and FIG. 3- (c), the sample has a single hexagonal phase structure, and exhibits a rod-like morphology with an average diameter of about 102nm and an average length of about 807 nm.
Example 4:
(1) 0.35 g of sodium hydroxide was accurately weighed and sufficiently dissolved in 10ml of anhydrous ethanol to form a colorless transparent alcoholic solution of sodium hydroxide. Measuring 8ml of oleic acid, slowly adding the oleic acid into a sodium hydroxide alcohol solution, and strongly stirring the solution for full reaction to obtain a viscous white solution mixed by the sodium oleate, the oleic acid and the alcohol;
(2) preparing 8ml of NaF (0.5mmol/ml) aqueous solution, adding the aqueous solution into the solution obtained in the step (1), and stirring strongly to obtain a semitransparent mixed solution;
(3) weighing 1mmol of rare earth nitrate (wherein the molar percentages of Y, Gd, Yb, Er and Tm are 53.875%, 30%, 15%, 0.125% and 1%); dissolving the rare earth nitrate into 2ml of deionized water to obtain 2ml (0.5mmol/ml) of rare earth nitrate aqueous solution, slowly adding the rare earth nitrate aqueous solution into the semitransparent mixed solution obtained in the step (3), and continuously stirring strongly for 30 minutes to obtain emulsion;
(4) and (4) filling the emulsion obtained in the step (3) into a polytetrafluoroethylene liner of 30ml, placing the polytetrafluoroethylene liner into a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours. Naturally cooling to room temperature, alternately cleaning the sample with anhydrous ethanol and deionized water for 3-4 times, collecting the obtained sample by centrifugation, and drying in a drying oven at 60 deg.C for 24 hr.
As shown in FIG. 2 and FIG. 3- (d), the sample was a single hexagonal phase structure, exhibiting a rod-like morphology with an average diameter of about 74nm and an average length of about 430 nm.
Example 5:
(1) 0.35 g of sodium hydroxide was accurately weighed and sufficiently dissolved in 10ml of anhydrous ethanol to form a colorless transparent alcoholic solution of sodium hydroxide. Measuring 8ml of oleic acid, slowly adding the oleic acid into a sodium hydroxide alcohol solution, and strongly stirring the solution for full reaction to obtain a viscous white solution mixed by the sodium oleate, the oleic acid and the alcohol;
(2) preparing 8ml of NaF (0.5mmol/ml) aqueous solution, adding the aqueous solution into the solution obtained in the step (1), and stirring strongly to obtain a semitransparent mixed solution;
(3) weighing 1mmol of rare earth nitrate (wherein the molar percentages of Y, Gd, Yb, Er and Tm are 43.875%, 40%, 15%, 0.125% and 1%); dissolving the rare earth nitrate into 2ml of deionized water to obtain 2ml (0.5mmol/ml) of rare earth nitrate aqueous solution, slowly adding the rare earth nitrate aqueous solution into the semitransparent mixed solution obtained in the step (3), and continuously stirring strongly for 30 minutes to obtain emulsion;
(4) and (4) filling the emulsion obtained in the step (3) into a polytetrafluoroethylene liner of 30ml, placing the polytetrafluoroethylene liner into a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours. Naturally cooling to room temperature, alternately cleaning the sample with anhydrous ethanol and deionized water for 3-4 times, collecting the obtained sample by centrifugation, and drying in a drying oven at 60 deg.C for 24 hr.
As shown in FIG. 2 and FIG. 3- (e), the sample has a single hexagonal phase structure, and exhibits a rod-like morphology with an average diameter of about 69nm and an average length of about 318 nm.
Claims (2)
1. Size-adjustable up-conversion NaYF4The preparation method of the nanocrystalline is characterized by comprising the following steps: the method comprises the following steps:
(1) accurately weighing 0.35 g of sodium hydroxide, and fully dissolving the sodium hydroxide in 10ml of absolute ethyl alcohol to form colorless and transparent sodium hydroxide alcoholic solution for later use;
(2) measuring 8ml of oleic acid, slowly adding the oleic acid into the sodium hydroxide alcohol solution prepared in the step (1), and strongly stirring the solution to react fully to obtain a viscous white solution mixed by the sodium oleate, the oleic acid and the alcohol;
(3) preparing 8ml of NaF0.5mmol/ml aqueous solution, slowly adding the aqueous solution into the solution obtained in the step (2), and strongly stirring to obtain a semitransparent mixed solution;
(4) preparation of Gd3+Dissolving 1mmol of ionic rare earth nitrate into 2ml of deionized water to obtain a rare earth nitrate aqueous solution, slowly adding the rare earth nitrate aqueous solution into the semitransparent mixed solution obtained in the step (3), and continuously stirring strongly for 30 minutes to obtain an emulsion; the Gd3+The ion concentration is between 5 and 40mol percent;
(5) putting the emulsion obtained in the step (4) into a polytetrafluoroethylene liner of 30ml, placing the polytetrafluoroethylene liner in a high-pressure reaction kettle, and keeping the temperature environment at 190 ℃ for 20 hours to obtain a sample;
(6) the sample is washed by using absolute ethyl alcohol and deionized water for 3-4 times alternately, and the obtained sample is collected by a centrifugal method and is placed in a drying oven to be dried for 24 hours under the condition of keeping the temperature at 60 ℃.
2. The method of claim 1, wherein: the hydrothermal synthesis method adopts oleic acid as milkAgents by doping with different concentrations of Gd3+The ions enable the preparation of nanocrystalline samples of different sizes.
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