WO2014127585A1

WO2014127585A1 - Zinc selenide fluorescent nanoparticles and preparation method thereof

Info

Publication number: WO2014127585A1
Application number: PCT/CN2013/074732
Authority: WO
Inventors: 王春; 秦锋; 王辉; 张一三
Original assignee: 合肥京东方光电科技有限公司; 京东方科技集团股份有限公司
Priority date: 2013-02-22
Filing date: 2013-04-25
Publication date: 2014-08-28
Also published as: CN103130201B; CN103130201A

Abstract

Provided are a method for preparing zinc selenide fluorescent nanoparticles, and the zinc selenide fluorescent nanoparticles prepared by the method, which fall within the technical field of luminescent materials, and can solve the problems of the organic solvent being flammable, explosive, expensive and having a relatively high toxicity, expensive comprehensive costs, and inconvenient operation etc. in the existing preparation method for zinc selenide nanoparticles. The method for preparing the zinc selenide fluorescent nanoparticles comprises the steps of preparing a selenium precursor solution and a zinc precursor solution, and preparing zinc selenide fluorescent nanoparticles that are easy to nucleate, uniformly nucleated, and will not easily agglomerate by selecting a suitable ligand at a relatively low reaction temperature.

Description

Selenization speech fluorescent nano particle and preparation method thereof

The invention particularly relates to a method for preparing a selenized fluorescent nanoparticle and a selenized fluorescent nanoparticle prepared by the method. Background technique

Nanoparticles with a size between 10 and 10 nm, also known as quantum dots, are "artificial molecules" that are combined by 10 ³ - 10 ⁵ atoms. Theoretical analysis shows that when the semiconductor material is gradually reduced from the bulk phase to a certain critical dimension, the feature size of the material is comparable to or smaller than the electron's De Broglie wavelength or electron mean free path in three dimensions. The motion in the material is limited in three dimensions, which means that the energy of the electron is quantized in three dimensions. Nanoparticles have unique quantum size effects and surface effects due to their radius being smaller or closer to the exciton Boer radius, and different sizes and compositions correspond to different fluorescence emission colors. The Chinese Patent Publication No. 102044552A, 102563545A, 101788737A, 102280565A all have a display device or display using fluorescent nanoparticles. At present, most commonly used fluorescent nanoparticles are Cd-containing Cd-containing nanoparticles such as CdSe, CdS, and CdTe, and Cd is a heavy metal, which may cause environmental pollution. The EU also strictly prohibits the presence of cadmium on the display. Therefore, in recent years, Zn-containing nano-particles such as ZnSe and ZnS have attracted more and more attention. The luminescent properties of these nano-particles are similar to those of cadmium-based nanoparticles, and have a modulating emission wavelength in the visible range. The narrow emission half-width and the color of the emitted light are more pure, and the display thus prepared shows a wider color gamut.

The organometallic method is one of the classical methods for preparing selenized nanoparticles. Usually, organic acid compound, selenium powder, etc. are used as raw materials, and trioctylphosphine oxide (TOPO), trioctylphosphine (antimony), tetrabutylphosphoric acid (phosphonium) and the like are solvents/surfactants, and are anhydrous and anaerobic. Selenization of nanoparticles is prepared under high temperature conditions. Although this synthetic circuit can obtain high-quality selenium-labeled nanoparticles with good monodispersity, the organic solvents such as TOPO, TOP, and TBP used in this method are flammable, explosive, expensive, and highly toxic. High cost and harsh conditions (need to be operated in a glove box) are not conducive to mass production. Summary of the invention

The object of the present invention is to solve the problem that the organic solvent is flammable, explosive, expensive, and has high toxicity, high comprehensive cost and inconvenient operation in the preparation method of the prior art deuterated nanoparticle, and provides a preparation of a bismuth nanoparticle. method.

In order to solve the above technical problems, an aspect of the present invention provides a method for preparing a selenization word nanoparticle, comprising the following steps:

Step 1): Preparation of ruthenium precursor liquid

Dissolving the litmus in a mixture of the first fatty acid and the oleylamine to prepare a selenium precursor solution;

Step 2): Preparation of the precursor liquid

Dissolving the compound in a mixture of the second fatty acid, the 18-mer, and the benzophenone to obtain a precursor liquid;

Step 3): Preparation of selenized fluorescent nanoparticles

The selenium precursor solution obtained in the step 1) is mixed with the precursor liquid obtained in the step 2) to obtain a fluorinated nanoparticle.

In a preferred embodiment, the step of preparing the ruthenium precursor liquid comprises:

Selenium is dissolved in a mixture of the first fatty acid and the oleylamine at a temperature of 220 ° C to 250 ° C, wherein the volume ratio of the first fatty acid to the oleylamine is 1: 1/3 to 1:3, selenium and The foregoing mixture of the first fatty acid and the oleylamine has a mass ratio of 1:1 to 1:3, and then is cooled to 5 ° C to 40 ° C to obtain a litmus precursor solution.

In a preferred embodiment, the step of preparing the precursor liquid comprises: dissolving the compound in the inert gas at a temperature of 230 ° C to 250 ° C in an inert atmosphere, the 18th women, the benzophenone In the mixture of ketones, the ratio of the amounts of the four substances is 1: (0.25-5): (5-10): (2-10), and the temperature is maintained to obtain the precursor liquid.

In a preferred embodiment, the step of preparing the fluorinated fluorescent nanoparticles is as follows: the mass ratio of the selenium precursor obtained in the step 1) to the precursor liquid obtained in the step 2) is 1: 1/3 to 1: 3 mixing, reacting at a temperature of 200 ° C - 220 ° C, 0.5-30 min, to obtain selenized fluorescent nanoparticles.

In a preferred embodiment, the first fatty acid and the second fatty acid may be the same or different monovalent fatty acids having 10 to 20 carbon atoms.

Further preferably, the first fatty acid and the second fatty acid may be the same or different one-way linear fatty acids having 10-20 carbon atoms, for example, a linear saturated or unsaturated one having a carbon number of 10-20. fatty acid. In a preferred embodiment, the first fatty acid and the second fatty acid may be the same or different ones of oleic acid, citric acid, eicosanoic acid, and palmitic acid.

In a particularly preferred embodiment, the first fatty acid and the second fatty acid are the same. In a preferred embodiment, the lexical compound is an organic grammatical compound or an inorganic grammatical compound. In a preferred embodiment, the organic character is a diethyl or chlorinated methyl group.

In a preferred embodiment, the inorganic compound is an oxidized or chlorinated word. In a preferred embodiment, the method further comprises the step of purifying the prepared selenized fluorescent fluorescent nanoparticles, comprising: centrifuging the deuterated fluorescent nanoparticles with a mixed solvent composed of a deuterated solvent and an impurity solvent, wherein The mass ratio of the selenization solvent to the impurity solvent is 1: 1/3 to 1:

3.

In a preferred embodiment, the selenization solvent is any one or more of methanol, ethanol, propanol and butanol, and the impurity solvent is toluene or n-hexane.

Another aspect of the present invention also provides a selenium fluorescing nanoparticle prepared by the above-described method for preparing a fluorinated fluorescent nanoparticle.

The preparation method of the bismuth-modified nanoparticle provided by the invention has the advantages of simple operation, good repeatability, low cost, mild condition, low toxicity and suitable for industrial production.

The selenized fluorescent nanoparticles prepared by the method of the invention have the advantages of narrow half-peak width of the fluorescence emission peak, uniform particle dispersion, and easier control of the particle size.

The selenized fluorescent nanoparticle prepared by the invention does not contain heavy metals, has good fluorescence emission characteristics, and can be used as an excellent luminescent material for illumination, display and the like. DRAWINGS

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a graph showing the fluorescence emission spectral emission intensity of a series of selenized fluorescent nanoparticles prepared in accordance with the present invention.

Figure 2 shows the fluorescence emission spectra of selenization nanoparticles prepared on behalf of the inventive examples 1-5 (line labeled 220 ° C) and comparative examples 1-5 (line labeled 280 ° C), respectively. The result of the emission peak scan. detailed description

The object of the present invention is to solve the problem that the organic solvent is flammable in the preparation method of the prior art deuterated nanoparticle. It is explosive, expensive and toxic, and has a high comprehensive cost and inconvenient operation, and provides a preparation method of the nanoparticle.

Step 1): Preparation of ruthenium precursor liquid

Step 2): Preparation of the precursor liquid

Dissolving the compound in a mixture of the second fatty acid, octadecene and benzophenone to obtain a precursor liquid;

Step 3): Preparation of selenized fluorescent nanoparticles

In a preferred embodiment, the step of preparing the ruthenium precursor liquid comprises: dissolving selenium in a mixture of the first fatty acid and the oleylamine at a temperature of 220 ° C to 250 ° C, wherein the first fatty acid The volume ratio of oleylamine to oleylamine is 1: 1/3 to 1:3, and the mass ratio of selenium to the mixture of the first fatty acid and oleylamine is 1:1 to 1:3, and then cooled to 5 ° C to 40 °. C, the production of Shixi precursor fluid.

In the step 1), the selenium as a raw material is preferably in the form of a powder.

It will be understood by those skilled in the art that the steps of the step 1) of preparing the lithographic precursor liquid in the present invention and the step 2) of preparing the precursor liquid can be reversed. In a specific case, these two steps can also be performed simultaneously. That is, "Step 1" and "Step 2" used in this article do not force these two steps to be performed in order.

In a preferred embodiment, the step of preparing the fluorinated fluorescent nanoparticles is as follows: the mass ratio of the selenium precursor obtained in the step 1) to the precursor liquid obtained in the step 2) is 1: 1/3 to 1: 3. For example, 1: (0.8~3) mixing, at a temperature of 200 ° C - 220 ° C, the reaction is 0.5-30 min, to obtain selenized fluorescent nanoparticles.

Advantageously, in step 3), the selenium precursor solution obtained in step 1) and the precursor liquid obtained in step 2) The mixing proceeds quickly because rapid mixing promotes nucleation and growth of the crystal.

The invention adopts the common fatty acid as the reaction solvent of selenium, that is, the first fatty acid, so that the reaction is more convenient and the cost is lower. Secondly, using a lower reaction temperature (200 ° C - 220 ° C), the fluorescence emission peak of the nanoparticles obtained at a lower reaction temperature is red-shifted slowly during the same reaction time, indicating that the obtained nano-particle size is obtained. The increase is slower, meaning that the nanoparticle size is easier to control, while the lower reaction temperature favors the obtaining of smaller particle size uniform size nanoparticles. Again, lower reaction temperatures also help to reduce production costs.

Further preferably, the first fatty acid and the second fatty acid may be the same or different one-way linear fatty acids having 10-20 carbon atoms, for example, a linear saturated or unsaturated one having a carbon number of 10-20. fatty acid.

In a preferred embodiment, the first fatty acid and the second fatty acid may be the same or different ones of oleic acid, citric acid, eicosanoic acid, and palmitic acid.

In a particularly preferred embodiment, the first fatty acid and the second fatty acid are the same. In a preferred embodiment, the lexical compound is an organic grammatical compound or an inorganic grammatical compound. In a preferred embodiment, the organic chemical is a diethyl or chlorinated methyl group. In a preferred embodiment, the inorganic compound is an oxidized or chlorinated word.

In a further preferred embodiment, the method further comprises the step of purifying the prepared selenized fluorescent nanoparticles, comprising using the selenized fluorescent nanoparticles with a selenization solvent (ie, a solvent for dissolving selenium) and A mixed solvent composed of an impurity solvent (i.e., a solvent for dissolving impurities) is subjected to centrifugation, and the mass ratio of the selenization solvent to the impurity solvent is 1: 1/3 to 1:3.

It should be understood that the selenization nanoparticles prepared according to the present method are in the form of selenium nanoparticles dispersed in a solvent. That is, the final product obtained after the mixing step or the refining step according to the present method is a solution in which the deuterated nanoparticles are dissolved, wherein the solvent depends on the solvent used in the preparation. Unless otherwise stated, the product "selenization" as described herein actually refers to selenization nanoparticles dissolved in a solvent.

As used herein, "inert atmosphere" means an ambient atmosphere that has no effect on the progress of the reaction, such as A rare gas such as argon or a nitrogen atmosphere can be used.

The technical problem to be solved by the present invention further comprises providing a deuterated fluorescent nanoparticle, which is prepared by the above-mentioned preparation method of the deuterated fluorescent nanoparticle.

The selenized fluorescent nanoparticle prepared by the invention does not contain heavy metals, has good fluorescence emission characteristics, and can be used as an excellent luminescent material for illumination, display and the like. Example

The technical solutions of the embodiments of the present invention will be clearly and completely described in the following with reference to the accompanying drawings of the embodiments of the invention. It is apparent that the described embodiments are part of the embodiments of the invention, rather than all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the described embodiments of the present invention without departing from the scope of the invention are within the scope of the invention.

Example 1

In this embodiment, the deuterated fluorescent nanoparticles are prepared by the following steps:

Step 1): Preparation of ruthenium precursor liquid

The oleic acid and oleylamine are mixed in a volume ratio of 1:1, and the selenium powder is added to the above mixture, wherein the mass ratio of the selenium powder to the mixed liquid is 1:3, and the mixture is stirred at a temperature of 220 °C. The selenium powder was dissolved, kept for 10 minutes, and cooled to 25 ° C to obtain a selenium precursor solution.

Step 2): Preparation of the precursor liquid

Dissolving oleic acid, 18 women and benzophenone into a mixed solution, heating the mixture to 250 ° C under an argon atmosphere, and dissolving diethyl ether in the above mixture under stirring Among them, the ratio of the amount of the substance of diethyl oleic acid, oleic acid, octadecene and benzophenone is 1: 0.25 : 5 : 2, and the precursor liquid is obtained by heat preservation. Step 3): Preparation of selenized fluorescent nanoparticles

The selenium precursor solution obtained in the first step is rapidly added to the precursor liquid obtained in the step 2 at a mass ratio of 1 : 1/3, and reacted at 220 ° C for 0.5 min to obtain selenized fluorescent nanoparticles.

In the reaction system, oleic acid acts as a solvent and as a main ligand, and benzophenone acts as a secondary ligand to stabilize the reaction system; oleylamine has a protective effect on the generated nanoparticles to prevent agglomeration; The precursor liquid is quickly added to the precursor liquid, which causes the temperature of the precursor liquid to drop, which is beneficial to the nucleation of the nanoparticles and the formation of uniform particles of nanoparticles in the high temperature reaction medium octadecene.

Further, the above-mentioned prepared selenization fluorescent nanoparticles are refined, and the specific steps are as follows: the selenium compound nanoparticle mixture obtained above is added to a mixed solution of toluene and methanol, wherein the volume of toluene and methanol The ratio is 1:1/3, toluene dissolves selenium into nanoparticles, and methanol removes unreacted organic matter. After centrifugation, the supernatant was removed twice, and a precipitate was obtained, which was dissolved in toluene to obtain a clear selenium-labeled nanoparticle transparent solution. Example 2

Step 1): Preparation of ruthenium precursor liquid

The tannic acid and oleylamine are mixed in a volume ratio of 1:3, and the selenium powder is added to the above mixture, wherein the mass ratio of the selenium powder to the mixed liquid is 1:1, and the mixture is stirred at 250 ° C. The selenium powder was dissolved, kept for 5 minutes, and cooled to 2 ° C to obtain a selenium precursor solution.

Step 2): Preparation of the precursor liquid

The tantalum, the 18 women, the benzophenone are arranged in a mixed solution, wherein the ratio of the three substances is 1: 2: 2, and the mixture is heated to 230 ° C under the protection of an argon atmosphere. The chlorinated methyl group is dissolved in the above mixture under stirring, wherein the ratio of the amount of the substance of the methyl chloride, decanoic acid, octadecene, and benzophenone is 1: 5 : 10 : 10, Insulation preparation to get the pre-drive liquid.

Step 3): Preparation of selenized fluorescent nanoparticles

The selenium precursor solution obtained in the first step is rapidly added to the pre-discovering liquid obtained in the step 2 by mass ratio of 1:1, and reacted at 200 ° C for 2 min to obtain selenized fluorescent nanoparticles.

In the reaction system, citric acid acts as a solvent and serves as a main ligand, and benzophenone acts as a secondary ligand to stabilize the reaction system; oleylamine has a protective effect on the generated nanoparticles to prevent agglomeration; The precursor fluid is quickly added to the pre-displacement fluid, which causes the temperature of the precursor liquid to drop, which is beneficial to The rice particles nucleate and form uniform particles of nanoparticles in the high temperature reaction medium octadecene.

Further, the selenium fluorescein nanoparticles prepared above are refined, and the specific steps are as follows: The selenium sulphate nanoparticle mixture obtained above is added to a mixed solution of n-hexane and butanol, wherein n-hexane and The volume ratio of butanol is 1:1, n-hexane dissolves the selenization of the nanoparticles, and butanol removes the unreacted organic matter. After centrifugation, the supernatant was removed twice, and a precipitate was obtained, which was dissolved in n-hexane to obtain a clear selenium-containing nanoparticle transparent solution. Example 3

Step 1): Preparation of Selenium Precursor

The eicosanoid and oleylamine are mixed in a volume ratio of 1:0.8, and the selenium powder is added to the above mixture, wherein the mass ratio of the selenium powder to the mixed liquid is 1:3, at 230 ° C The selenium powder was dissolved by stirring, kept for 7 min, and cooled to 30 ° C to obtain a selenium precursor solution.

Step 2): Preparation of the precursor liquid

Dissolving the eicosanic acid, octadecene, and benzophenone into a mixed solution, and heating the mixture to 240 ° C under an argon atmosphere to dissolve the oxidized solution in the above mixture under stirring Among them, the ratio of the amount of the substances of oxidized, eicosanoid, octadecene and benzophenone is 1:3:8:5, and the precursor liquid is obtained by heat preservation.

Step 3): Preparation of selenized fluorescent nanoparticles

The selenium precursor solution obtained in the first step was quickly added to the pre-expressed liquid obtained in the step 2 at a mass ratio of 1:3, and reacted at 210 ° C for 5 minutes to obtain selenized fluorescent nanoparticles.

In the reaction system, eicosanic acid is used as a solvent and as a main ligand, and benzophenone acts as a secondary ligand to stabilize the reaction system; oleylamine has a protective effect on the generated nanoparticles to prevent agglomeration. The selenium precursor solution is quickly added to the pre-displacement fluid, which causes the temperature of the precursor liquid to drop, which is beneficial to the nucleation of the nanoparticles, and forms the nanoparticles of the particles in the high-temperature reaction medium.

Further, the above-mentioned prepared selenized fluorescent nanoparticles are refined, and the specific steps are as follows: The selenium compound nanoparticle mixture obtained above is added to a mixed solution of n-hexane and ethanol, wherein n-hexane and ethanol The volume ratio is 1:3, n-hexane dissolves selenium nanoparticles, and ethanol removes unreacted organic matter. After centrifugation, the supernatant was removed twice, and a precipitate was obtained, which was dissolved in n-hexane to obtain a clear selenium-labeled nanoparticle transparent solution. Example 4

In this embodiment, selenization fluorescent nanoparticles are prepared in the following steps:

Step 1): Preparation of ruthenium precursor liquid

The palmitic acid and oleylamine are mixed in a volume ratio of 1: 1/3, and the selenium powder is added to the above mixture, wherein the mass ratio of the selenium powder to the mixed liquid is 1:1.5, at 240 ° C The selenium powder was dissolved by stirring, kept for 8 minutes, and cooled to 40 ° C to obtain a selenium precursor solution.

Step 2): Preparation of the precursor liquid

Disposing palmitic acid, octadecene, and benzophenone into a mixed solution, and heating the mixture to 245 ° C under an argon atmosphere, and dissolving the chloride in the above mixture under stirring, wherein The ratio of the amount of the substances of oxidized words, palmitic acid, octadecene and benzophenone is 1:4:7:6, and the precursor liquid is obtained by heat preservation.

Step 3): Preparation of selenized fluorescent nanoparticles

The selenium precursor solution obtained in the first step was quickly added to the pre-discovering liquid obtained in the step 2 at a mass ratio of 1:0.8, and reacted at 215 ° C for 10 min to obtain selenized fluorescent nanoparticles.

In the reaction system, palmitic acid acts as a solvent and as a main ligand, and benzophenone acts as a secondary ligand to stabilize the reaction system; oleylamine has a protective effect on the generated nanoparticles to prevent agglomeration; The precursor fluid is quickly added to the pre-displacement fluid, which causes the temperature of the precursor liquid to drop, which is beneficial to the nucleation of the nanoparticles, and the formation of uniform particles of nanoparticles in the high temperature reaction medium.

Further, the above-mentioned prepared selenized fluorescent nanoparticles are refined, and the specific steps are as follows: the selenium compound nanoparticle mixture obtained above is added to a mixed solution of toluene and propanol, wherein toluene and propanol The volume ratio is 1:0.8, the toluene dissolves the selenium nanoparticles, and the propanol removes the unreacted organic matter. After centrifugation, the supernatant was removed twice, and a precipitate was obtained, which was dissolved in toluene to obtain a clear selenium-labeled nanoparticle transparent solution. Example 5

Step 1): Preparation of ruthenium precursor liquid

The oleic acid and the oleylamine are mixed in a volume ratio of 1:1, and the selenium powder is added to the above mixture, wherein the mass ratio of the selenium powder to the mixed liquid is 1:3, and the mixture is stirred at 220 ° C. The selenium powder was dissolved, kept for 10 minutes, and cooled to 25 ° C to obtain a selenium precursor solution. Step 2): Preparation of the precursor liquid

Dissolving oleic acid, 18 women and benzophenone into a mixed solution, heating the mixture to 250 ° C under an argon atmosphere, and dissolving diethyl ether in the above mixture under stirring Among them, the ratio of the amount of the substances of diethyl oleic acid, oleic acid, 18 women and benzophenone is 1:3:10:5, and the precursor liquid is obtained by heat preservation.

Step 3): Preparation of selenized fluorescent nanoparticles

The selenium precursor solution obtained in the first step is rapidly added to the precursor liquid obtained in the step 2 by mass ratio of 1: 1/3, and reacted at 220 ° C for 30 minutes to obtain selenized fluorescent nanoparticles.

Further, the above-mentioned prepared selenization fluorescent nanoparticles are refined, and the specific steps are as follows: the selenium compound nanoparticle mixture obtained above is added to a mixed solution of toluene and methanol, wherein the volume of toluene and methanol The ratio is 1:3, toluene dissolves selenium nanoparticles, and methanol removes unreacted organic matter. After centrifugation, the supernatant was removed twice, and a precipitate was obtained, which was dissolved in toluene to obtain a clear selenium-labeled nanoparticle transparent solution. Example 6-9

The preparation of the selenized fluorescent nanoparticles in Examples 6-9 was similar to the preparation of the selenized fluorescent nanoparticles in Example 1, except that the reaction time in the third step was 2 min (Example 6), 5 min ( Example 7), lOmin (Example 8), 30 min (Example 9). The fluorescence emission spectrum emission intensity scan results of the bismuth-modified nanoparticles prepared in Example 1 and Examples 6-9 are shown in Fig. 1. It can be seen from Fig. 1 that with the prolongation of the reaction time, the fluorescence emission peak of the bismuth ruthenium nanoparticles is less red-shifted, the size of the nano-particles is not changed much, and the size of the prepared nanoparticles is relatively uniform. Comparative example 1-5

The preparation of the selenized fluorescent nanoparticles in Comparative Examples 1-5 was similar to the preparation of the selenized fluorescent nanoparticles in Examples 1-5, respectively, except that the reaction temperature in the third step was 280 °C. Figure 2 shows the fluorescence emission of selenization nanoparticles prepared on behalf of the inventive examples 1-5 (marked at 220 ° C) and comparative examples 1-5 (marked at 280 ° C). The result of the speech emission peak scan.

It can be seen from Fig. 2 that the nanoparticles obtained by using the lower reaction temperature (200 ° C - 220 ° C) relative to the higher reaction temperature (280 ° C), the lower reaction temperature in the same reaction time The fluorescence emission peak is red-shifted more slowly, and the particle size increase is slower, so the nanoparticle size is easier to control, and the lower reaction temperature is favorable for obtaining smaller-sized uniform-sized nanoparticles. In addition, lower reaction temperatures also contribute to lower production costs. It is to be understood that the above embodiments are merely illustrative embodiments employed to illustrate the principles of the invention, but the invention is not limited thereto. Various modifications and improvements can be made by those skilled in the art without departing from the spirit and scope of the invention. These modifications and improvements are also considered to be within the scope of the invention.

Claims

Claim

A method for preparing a selenized fluorescent nanoparticle, comprising the steps of:

Step 1): Preparation of ruthenium precursor liquid

Dissolving hydrazine in a mixture of the first fatty acid and oleylamine to prepare a selenium precursor solution;

Step 2): Preparation of the precursor liquid

Step 3): Preparation of selenized fluorescent nanoparticles

The selenium precursor solution obtained in the step 1) is mixed with the precursor liquid obtained in the step 2) to obtain a selenium-emitting fluorescent nanoparticle.

2 . The method for preparing a selenium fluorescein nanoparticle according to claim 1 , wherein the step of preparing a selenium precursor solution comprises: dissolving selenium in a first temperature at a temperature of 220° C. to 250° C. In a mixture of a fatty acid and an oleylamine, wherein the volume ratio of the first fatty acid to the oleylamine is 1: 1/3 to 1:3, and the mass ratio of the selenium to the mixture of the first fatty acid and the oleylamine is 1: 1 to 1:3, then cooled to 5 °C -40 °C to prepare a selenium precursor solution.

3. The method for preparing a selenium fluorescing nanoparticle according to claim 1, wherein the step of preparing the precursor liquid comprises: at a temperature of 230 ° C to 250 ° C, the compound is in an inert atmosphere. Dissolved in a mixture of a second fatty acid, octadecene, and benzophenone, wherein the ratio of the amounts of the four substances is 1: (0.25-5): (5-10): (2-10) And keep warm, and get the pre-drive liquid.

4. The method for preparing a selenized fluorescent nanoparticle according to claim 1, wherein the step of preparing a selenized fluorescent nanoparticle comprises:

The selenium precursor liquid obtained in the step 1) and the precursor liquid obtained in the step 2) are mixed at a mass ratio of 1: 1/3 to 1:3, and reacted at a temperature of 200 ° C to 220 ° C for 0.5-30 min to obtain Selenization of fluorescent nanoparticles.

The method for preparing a selenized fluorescent fluorescent particle according to any one of claims 1 to 4, wherein the first fatty acid and the second fat are the same or different, and the first fatty acid and the second The fatty acid is a monobasic fatty acid having 10 to 20 carbon atoms, and is preferably a monohydric straight chain fatty acid having 10 to 20 carbon atoms.

The method for preparing a selenized fluorescent nanoparticle according to any one of claims 1 to 4, wherein The first fatty acid and the second fatty acid may be the same or different and are a monohydric linear saturated or unsaturated fatty acid having 10-20 carbon atoms, preferably oleic acid, citric acid, eicosanoic acid, palmitic acid. Any of them.

The method for producing a selenized fluorescent fluorescent particle according to any one of claims 1 to 4, wherein the chemical substance is an organic chemical or an inorganic chemical.

The method for producing a selenized fluorescent nanoparticle according to claim 7, wherein the organic character is diethyl or chloromethyl.

The method for producing a selenized fluorescent nanoparticle according to claim 7, wherein the inorganic chemical is an oxidized or chlorinated word.

The method for preparing a selenized fluorescent nanoparticle according to any one of claims 1 to 4, further comprising the step of refining the prepared selenized fluorescent nanoparticle, comprising using the selenized fluorescent nanoparticle. The mixed solvent consisting of a solvent and an impurity solvent is subjected to centrifugation, and the mass ratio of the hydrazine solvent to the impurity solvent is 1: 1/3 to 1:3.