CN110143579B - Preparation method of nano crystal - Google Patents
Preparation method of nano crystal Download PDFInfo
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- CN110143579B CN110143579B CN201910450937.1A CN201910450937A CN110143579B CN 110143579 B CN110143579 B CN 110143579B CN 201910450937 A CN201910450937 A CN 201910450937A CN 110143579 B CN110143579 B CN 110143579B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
- C01B25/082—Other phosphides of boron, aluminium, gallium or indium
- C01B25/087—Other phosphides of boron, aluminium, gallium or indium of gallium or indium
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a preparation method of a nanocrystal, which comprises the following steps: 1) dissolving a first precursor material in an organic solvent, wherein the first precursor material contains metal ions required for synthesizing the nano-crystals; 2) and heating to a first temperature, adding a second precursor substance into an organic solvent containing the first precursor substance, wherein the second precursor substance contains non-metallic ions required for synthesizing the nanocrystals, and enabling the first precursor substance and the second precursor substance to be in contact with each other to perform a chemical reaction to generate the nanocrystals with non-uniform particle sizes. The invention prepares the quantum dots with lower performance by a simpler method, is convenient for storage and is easier for large-scale mass production. When the quantum dots are needed to be used, the nano crystals with the uneven particle sizes are prepared to obtain the quantum dots with the even particle sizes and higher performance.
Description
The application is a divisional application with application number of 201610828099.3, entitled preparation method of nanocrystal and application date of 2016, 09 and 19.
The present application claims priority from all of the countries of the prior application (application No. 201610075952.9 entitled method for producing nanocrystals, filed 2016, 03/02/2016).
Technical Field
The invention relates to a preparation method of a nanocrystal.
Background
Quantum dots, also known as nanocrystals or nanocrystals, are materials having a size of a few nanometers, typically in the range of 1-20 nanometers, and having a crystalline structure. The quantum dots can fluoresce under excitation of a suitable light source or voltage. Quantum dots have been extensively studied over the last two decades due to their special properties, such as size-tunable optical properties, high quantum efficiency, relatively narrow half-peak width and resistance to photodegradation.
In the prior art, the preparation of quantum dots often has the following problems that the method with lower preparation cost has poorer performance, and the preparation method with higher product performance has higher preparation cost. For example, the preparation of indium phosphide quantum dots generally comprises three methods: 1) at high temperature, organic alkyl phosphine is used as a phosphorus source to react with an indium fatty acid precursor to obtain indium phosphide quantum dots, and the method has the advantages of complex preparation process, expensive raw materials and higher cost; 2) under high temperature, phosphine gas directly reacts with fatty acid indium to obtain indium phosphide quantum dots, toxic gas is required to be introduced in the method, the operation is complex and dangerous and is difficult to control, the product performance is poor, and the cost is high; 3) simple substance phosphorus is used as a phosphorus source to react with fatty acid indium to obtain the indium phosphide quantum dots, and the method has simple operation but high potential safety hazard.
In addition, the above problems in the preparation of quantum dots also make the production of quantum dots on a large scale difficult.
Therefore, further improvements in quantum dot preparation methods are needed.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: a method for preparing nanocrystals is provided, which can improve the performance of nanocrystals.
The invention provides a preparation method of a nanocrystal, which comprises the following steps: adding nanocrystals having a relatively non-uniform particle size to an organic solvent having a predetermined temperature at which an ionic bond of the nanocrystals can be broken, in which an electron donating-group compound is dissolved, to produce nanocrystals having a relatively uniform particle size.
Preferably, the nanocrystal particle size ranges from 1 to 10 nm.
Preferably, the nanocrystals are group iiia-va nanocrystals selected from one of the following compounds: indium phosphide, indium arsenide, gallium nitride, gallium phosphide, gallium arsenide, gallium antimonide, aluminum nitride, aluminum phosphide, aluminum arsenide, aluminum antimonide, indium nitride, indium antimonide, gallium azophoside, gallium antimonide, gallium azophoside, aluminum phosphide, aluminum arsenide azophoside, aluminum gallium antimonide, aluminum gallium arsenphosphate, indium gallium azophoside, indium gallium arsenide, indium gallium antimonide, indium gallium phosphoroarse, indium aluminum nitride, indium aluminum phosphide, indium aluminum arsenide, indium aluminum antimonide.
Preferably, the nanocrystal is indium phosphide and the predetermined temperature is 220 ℃ to 260 ℃.
Preferably, the predetermined temperature is 240 ℃ to 250 ℃.
Preferably, the organic solvent includes a dopant ion selected from at least one of zinc ion, magnesium ion, calcium ion, and aluminum ion.
Preferably, the organic solvent is at least one of long-chain alkane, long-chain alkene, long-chain alcohol, long-chain amine, long-chain ester, long-chain fatty acid and long-chain mercaptan.
Preferably, the long-chain alkane comprises at least one of: comprises 1-octadecane, 1-heptadecane, 1-hexadecane, 1-dodecane, 1-tetradecane, 1-tridecane, 1-pristane, 1-phytane, 1-pentadecane, paraffin, 1-eicosane, 1-octacosane and 1-tetracosane; the long-chain olefin comprises at least one of the following substances: 1-octadecene, 1-dodecene, 1-hexadecene, 1-tetradecene, 1-heptadecene, 1-nonadecene, 1-eicosene, 1-tridecene, 1-pentadecene; the long-chain alkylamine comprises at least one of the following substances: hexadecylamine, octadecylamine, tetradecylamine, decylamine, dodecylamine, undecylamine, tridecylamine, 1, 12-diaminododecane, 1, 18-diaminooctadecane, 1, 16-diaminohexadecane, 1, 14-diaminotetradecylamine, oleylamine; the long-chain alkanol comprises at least one of the following substances: 1-octadecanol, 1-hexadecanol, 1-eicosanol, 1-dodecanol, 1-tridecanol, 1-tetradecanol, 1-docosanol, 1-pentadecanol, 1-heptadecanol, 1-nonadecanol, 1-eicosanol; the long chain alkyl ester comprises at least one of the following substances: stearyl ester, lauryl acetate, cetyl acetate, eicosyl acetate, pentadecyl, heptadecyl acetate; the long-chain alkyl fatty acid comprises at least one of the following substances: capric acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, stearic acid, eicosanoic acid; the long-chain alkyl mercaptan comprises at least one of the following substances: 1-undecanethiol, 1-dodecanethiol, 1-tetradecanethiol, 1-pentadecanethiol, 1-hexadecanethiol, 1-octadecanethiol.
Preferably, the electron-donating group compound includes at least one of trialkylphosphine, trialkylphosphine oxide, alkylamine, enamine, alkylthiol, arylthiol, alkylarylthiol, fatty acid.
Preferably, the alkylamine comprises at least one of mono-substituted alkylamine, di-substituted alkylamine and tri-substituted alkylamine, and the fatty acid comprises at least one of myristic acid, oleic acid and stearic acid.
Preferably, after the nanocrystals having a relatively non-uniform particle size are added to the organic solvent having a predetermined temperature, the temperature of the organic solvent is maintained around the predetermined temperature for 1 second to 1 hour.
Preferably, after the nanocrystals having relatively non-uniform particle sizes are added to an organic solvent having a predetermined temperature and maintained for a certain period of time, a precursor material required for synthesizing the shell of the nanocrystals is added and maintained for a certain period of time to be cooled.
Preferably, the precursor material required for the shell is a zinc sulphide precursor.
Preferably, the nano-crystals with non-uniform particle size are prepared by the following steps: 1) dissolving a first precursor substance in the organic solvent under an inert gas atmosphere or vacuum condition, wherein the first precursor substance contains metal ions required for synthesizing the nano-crystals; 2) and heating to the first temperature, adding a second precursor substance into the mixture, wherein the second precursor substance contains non-metallic ions required for synthesizing the nano-crystals, and enabling the first precursor substance and the second precursor substance to be in contact with each other to perform a chemical reaction to generate the nano-crystals with uneven particle sizes.
The invention has the following beneficial effects: the preparation method disclosed by the invention is simple in steps, easy to operate and low in cost; the nano crystal obtained by the preparation method has more uniform particle size and narrower half-peak width. By the method, the quantum dots with lower performance can be prepared by a simpler method, and large-scale mass production is easier. When actual use is needed, a part of quantum dots with lower performance are taken, and the quantum dots with higher performance and more uniform particle size can be quickly and conveniently prepared by the method.
Drawings
FIG. 1 is a diagram of the absorption spectrum and the emission spectrum of the InP quantum dot prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described in detail below with reference to the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
The invention discloses a preparation method of a nanocrystal, which comprises the following steps: and rapidly adding the nanocrystals with the non-uniform particle size into an organic solvent with the electron donating group compound dissolved therein at a predetermined temperature to produce the nanocrystals with the uniform particle size, wherein the predetermined temperature can break ionic bonds of the nanocrystals in the organic solvent.
The predetermined temperature is a temperature range that can break the ionic bonds of the nanocrystals in the organic solvent, but does not completely decompose the nanocrystals into ions at the instant of addition, allowing seeded growth of the nanocrystals. Different nanocrystals correspond to different predetermined temperatures.
The invention causes the ionic bond of partial nanometer crystal to break by contacting the nanometer crystal with high temperature organic solvent to generate the ion of nanometer crystal. Wherein a portion of the nanocrystals having the smallest particle size are completely decomposed into ions constituting the nanocrystals at an instantaneous high temperature, and a portion of the nanocrystals having a larger particle size are only partially decomposed into ions constituting the nanocrystals at an instantaneous high temperature. Since the solubility of inorganic metal ionic compounds in organic solvents is very small, the ions of these newly produced nanocrystals cause supersaturation of ions in organic solvents and tend to deposit and grow on the surface of the nanocrystals, whose ionic bonds have not yet been broken, thereby narrowing the overall particle size distribution of the nanocrystals.
The cleavage of the ionic bonds of the nanocrystals starts first from the outermost layer, generating the corresponding cations and anions into the organic solution. In the heterogeneous organic system of the present invention, the cleavage of the ionic bond of the nanocrystal is a dynamic process. When the tendency of the ions constituting the nanocrystal to deposit and grow on the nanocrystal is greater than the tendency of the ionic bond of the nanocrystal to break at the predetermined temperature, the nanocrystal as a whole is in a growth state.
The source of the nano-crystals with non-uniform particle size in the invention comprises two ways, one is obtained by purchasing and the other is obtained by preparing.
In a preferred embodiment, the preparation method of the present invention comprises the step of preparing nanocrystals with relatively non-uniform particle sizes, specifically as follows: 1) dissolving a first precursor material in an organic solvent, the first precursor material containing metal ions required for synthesizing the nanocrystals; 2) and heating to the first temperature, adding a second precursor substance into the mixture, wherein the second precursor substance contains nonmetallic ions required by the synthesis of the nanocrystals, and enabling the first precursor substance and the second precursor substance to be in contact with each other to perform a chemical reaction to generate the nanocrystals with uneven particle sizes. In order to obtain better nanocrystals, it is preferable that another metal ion is further dissolved in the organic solvent in step 1) to activate the metal ion in the first precursor substance or to fill in the defects of the generated nanocrystals.
In a preferred embodiment, the nanocrystals of the invention have a particle size in the range of 1-10 nm.
In a preferred embodiment, the nanocrystals of the invention are group IIIA-VA nanocrystals. Preferably, the nanocrystal is selected from one of the following compounds: indium phosphide, indium arsenide, gallium nitride, gallium phosphide, gallium arsenide, gallium antimonide, aluminum nitride, aluminum phosphide, aluminum arsenide, aluminum antimonide, indium nitride, indium antimonide, gallium azophoside, gallium antimonide, gallium azophoside, aluminum phosphide, aluminum arsenide azophoside, aluminum gallium antimonide, aluminum gallium arsenphosphate, indium gallium azophoside, indium gallium arsenide, indium gallium antimonide, indium gallium phosphoroarse, indium aluminum nitride, indium aluminum phosphide, indium aluminum arsenide, indium aluminum antimonide.
In a preferred embodiment, the nanocrystal is indium phosphide and the predetermined temperature is 220 ℃ to 260 ℃. More preferably, the nanocrystal is indium phosphide and the predetermined temperature is 240 ℃ to 250 ℃.
In a preferred embodiment, the organic solvent has dopant ions dissolved therein. The doped ions not only can play a role in activation, but also can fill in the defects of the nanocrystals. The doping ion is at least one of zinc ion, magnesium ion, calcium ion and aluminum ion. In a preferred embodiment, the nanocrystals prepared by the present invention comprise a doping element, and the doping element comprises at least one of zinc, magnesium, calcium and aluminum.
The organic solvent is at least one of long-chain alkane, long-chain olefin, long-chain alcohol, long-chain amine, long-chain ester, long-chain fatty acid and long-chain mercaptan. Preferably, the long-chain alkane comprises at least one of 1-octadecane, 1-heptadecane, 1-hexadecane, 1-dodecane, 1-tetradecane, 1-tridecane, 1-pristane, 1-phytane, 1-pentadecane, paraffin, 1-eicosane, 1-octacosane and 1-tetracosane; the long-chain olefin comprises at least one of 1-octadecene, 1-dodecene, 1-hexadecene, 1-tetradecene, 1-heptadecene, 1-nonadecene, 1-eicosene, 1-tridecene and 1-pentadecene; the long-chain alkylamine comprises at least one of hexadecylamine, octadecylamine, tetradecylamine, decylamine, dodecylamine, undecylamine, tridecylamine, 1, 12-diaminododecane, 1, 18-diaminooctadecane, 1, 16-diaminohexadecane, 1, 14-diaminotetradecylamine and oleylamine; the long-chain alkanol comprises at least one of 1-octadecanol, 1-hexadecanol, 1-eicosanol, 1-dodecanol, 1-tridecanol, 1-tetradecanol, 1-docosanol, 1-pentadecanol, 1-heptadecanol, 1-nonadecanol and 1-eicosanol; the long-chain alkyl ester comprises at least one of stearyl ester, lauryl acetate, cetyl acetate, eicosyl acetate, pentadecyl ester and heptadecyl ester; the long-chain alkyl fatty acid comprises at least one of capric acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, stearic acid, and eicosanoic acid; the long-chain alkyl mercaptan comprises at least one of 1-undecane mercaptan, 1-dodecane mercaptan, 1-tetradecane mercaptan, 1-pentadecane mercaptan, 1-hexadecane mercaptan and 1-octadecane mercaptan.
The electron donating group compound of the present invention includes at least one of trialkylphosphine, trialkylphosphine oxide, alkylamine, enamine, alkylthiol, arylthiol, alkylarylthiol, and fatty acid. Preferably, the alkylamine comprises at least one of mono-substituted alkylamine, di-substituted alkylamine and tri-substituted alkylamine, and the fatty acid comprises at least one of myristic acid, oleic acid and stearic acid.
In a preferred embodiment, the organic solvent of the present invention is a mixture comprising a long-chain alkyl acid and octadecene. In another preferred embodiment, the organic solvent of the present invention is a mixture comprising a long-chain alkyl acid, a long-chain alkylamine, and octadecene.
In a preferred embodiment, after the nanocrystals having a relatively non-uniform particle size are added to the organic solvent having a predetermined temperature, the temperature of the organic solvent is maintained around the predetermined temperature for 1 second to 1 hour. The grain size of the prepared nano crystal can be controlled by the difference of the holding time.
In a preferred embodiment, the preparation method of the present invention comprises: rapidly adding the nano-crystals with non-uniform particle sizes into an organic solvent with electron-donating group compounds dissolved therein at a preset temperature, keeping the mixture for a period of time, adding precursor substances required for synthesizing shells into the obtained product, keeping the precursor substances at the preset temperature for a period of time, and then cooling. The present embodiment obtains a nanocrystal having a core-shell structure. The shell of the nanocrystal is also a semiconductor material, preferably the shell comprises a semiconductor material comprising a group II/VI compound or a group III/V compound, more preferably the shell comprises a semiconductor material comprising 2 to 20 monolayers of a group II/VI compound or a group III/V compound. In one embodiment, a zinc sulfide shell is synthesized, and a zinc sulfide precursor is added. The zinc sulfide precursor material includes a zinc precursor, a sulfur precursor, or a material containing sulfur and zinc elements. If the original organic solvent already contains a zinc precursor, only a sulfur precursor needs to be added.
In a preferred embodiment, the preparation method of the present invention comprises: quickly adding the nano crystals with uneven particle sizes into an organic solvent with electron-donating group compounds dissolved at a preset temperature, keeping the temperature near the preset temperature for a period of time, then cooling, and separating and purifying the obtained product by means of extraction, centrifugation and the like. And (3) dissolving the finally obtained centrifugal precipitation product in a nonpolar solvent to obtain the purified nanocrystal solution. The organic solvent used for extraction includes but is not limited to one or more of n-hexane, methanol and ethanol.
In a preferred embodiment, the nanocrystal is indium phosphide and the predetermined temperature is 220 ℃ to 260 ℃. Specifically, the preparation method comprises the following steps: 1) dissolving an indium precursor and a zinc precursor in an organic solvent containing a long-chain alkyl acid, wherein the molar ratio of indium element to zinc element is 1:0-1: 5; 2) vacuumizing, heating to 100-140 ℃ under a vacuum condition, and further deoxidizing for 1h to obtain an indium precursor solution; 3) heating the indium precursor solution to 150-200 ℃, introducing phosphine gas into the indium precursor solution until the color is changed into light yellow to brown, and stopping introducing the gas to obtain an indium phosphide nanocrystal solution with uneven particle size; 4) preparing a mixed solution containing zinc ions and long-chain alkyl acid, wherein the molar ratio of the zinc ions to the long-chain alkyl acid is 1:1-1:2.5, and heating to a preset temperature of 220-260 ℃; 5) quickly injecting the indium phosphide nanocrystal solution with relatively non-uniform particle size into a mixed solution with a preset temperature of 220-260 ℃, keeping the mixed solution at 220-260 ℃ for a period of time, and then cooling to obtain an indium phosphide nanocrystal solution with relatively uniform particle size; 6) the separation and purification are carried out by extraction with a nonpolar solvent and centrifugation.
After the nanocrystals with the relatively non-uniform particle size are rapidly added into the mixed solution with the preset temperature, the indium phosphide nanocrystals with the relatively small particle size are rapidly decomposed and combined with the indium phosphide nanocrystals with the relatively large particle size, and finally the indium phosphide nanocrystals with the relatively large particle size and the uniform particle size are formed. After the nano crystals with uniform particle size are formed, the temperature is kept for a period of time, the particle size of the nano crystals becomes more uniform gradually, the defects on the surface are reduced gradually, and finally the indium phosphide nano crystals with uniform particle size and stable performance are obtained. The zinc ions contribute to the activation of the indium ions and reduce defects on the surface of the nanocrystal.
In an embodiment of the above method for producing indium phosphide nanocrystals, the predetermined temperature is preferably 240 ℃ to 250 ℃ and the organic solvent is preferably octadecene. In a preferred embodiment, the mixed solution in step 4) further comprises long-chain amine.
In the above embodiment of the method for preparing indium phosphide nanocrystals, the final nanocrystal particle size can be influenced by controlling the time for introducing the phosphine gas in step 3). The grain size of the nano crystal can be roughly judged by changing the color of the solution in the step 3). As the amount of phosphine gas was increased, the time for introducing the phosphine gas was increased, and the color of the indium precursor solution was changed from light yellow to brown. Light yellow indicates smaller nanocrystal particle size and brown indicates larger nanocrystal particle size.
In the present invention, the particle size of the nanocrystal can also be adjusted by controlling the holding time. The temperature range during the holding period is a predetermined temperature range, and the particle size of the nanocrystal increases with increasing holding time.
Example 1
Preparing indium phosphide nanocrystals with uniform particle size: 1) mixing indium acetate, zinc acetate, octadecanoic acid and octadecylamine, wherein the molar ratio of the indium acetate to the zinc acetate is 1:2, adding the indium acetate to a small amount of octadecene solvent, and uniformly stirring to form a mixture; 2) heating the mixture to 120 ℃ under a vacuum condition, and deoxidizing for 1h to obtain a precursor mixed solution of indium acetate and zinc acetate; 3) heating the mixed solution to 180 ℃, introducing phosphine gas into the mixed solution until the mixed solution becomes light yellow, and stopping introducing the gas to obtain indium phosphide nanocrystal dispersion liquid with uneven particle size; 4) adding zinc acetate and long-chain alkyl acid into a certain amount of octadecene at a molar ratio of 1:1, uniformly stirring, and heating to 245 ℃ to obtain an organic solution at a preset temperature; 5) adding the obtained indium phosphide nanocrystal dispersion liquid with uneven particle size into the organic solution at the temperature of 245 ℃, preserving the heat for 5 seconds, and then cooling; 6) and adding the cooled dispersion liquid into a mixed solution of normal hexane and ethanol, carrying out high-speed centrifugation, dissolving the obtained centrifugal precipitate with the normal hexane, adding methanol to form turbid liquid, carrying out high-speed centrifugal separation again, and dissolving the centrifugal precipitate in the normal hexane to obtain the purified indium phosphide nanocrystal with uniform particle size.
Example 2
Preparing zinc sulfide coated indium phosphide nanocrystals with uniform particle size: the same as in example 1, except that step 5) was: adding the indium phosphide nanocrystal dispersion liquid with uneven particle size into the organic solution at 245 ℃, preserving the heat for 5 seconds, dropwise adding a sulfur source dissolved in octadecene, continuously preserving the heat for 5min, and then cooling.
Example 3
Preparing zinc sulfide coated indium phosphide nanocrystals with uniform particle size: the same as in example 1, except that step 5) was: adding the indium phosphide nanocrystal dispersion liquid with uneven particle size into the organic solution with 245 ℃, preserving the heat for 20 seconds, dripping a sulfur source dissolved in octadecene into the dispersion liquid, continuously preserving the heat for 20 seconds, and then cooling.
Example 4
Preparing indium phosphide nanocrystals with uniform particle size: the same as in example 1, except that step 3) is: and heating the mixed solution to 180 ℃, introducing hydrogen phosphide gas into the mixed solution until the mixed solution turns brown, and stopping introducing the gas to obtain the indium phosphide nanocrystal dispersion liquid with uneven particle size.
The nanocrystals prepared in examples 1 to 4 demonstrate that they can be prepared simply and rapidly by the preparation method of the present invention. Because the requirement on the particle size is not high, the required nanocrystals with uneven particle size can be obtained in large quantities by a simple method, and the storage is convenient. When high-quality nanocrystals with uniform particle sizes need to be prepared, the nanocrystals can be directly used for preparation, the conversion method from the nanocrystals with the uniform particle sizes to the nanocrystals with the uniform particle sizes is very simple, and the preparation cost can be greatly reduced.
Fig. 1 is an absorption spectrum and an emission spectrum of the quantum dot of example 1 of the present invention. As can be seen from the figure, the half-peak width of the nanocrystals prepared by the present invention is narrow, which indicates that the particle size of the nanocrystals is relatively uniform.
In conclusion, the invention provides a novel preparation method of the nano-crystal, which is simple and easy to operate and can obtain the nano-crystal with more uniform particle size.
Although the invention has been described and illustrated in greater detail by the inventors, it should be understood that modifications and/or alterations to the above-described embodiments, or equivalent alterations thereto, will become apparent to those skilled in the art without departing from the spirit of the invention, and that no limitation to the invention is intended by the terms of the present invention as set forth herein is intended to be exhaustive or to be construed as limiting the invention.
Claims (7)
1. A method for producing nanocrystals, comprising the steps of:
1) dissolving a first precursor substance in an organic solvent, wherein the first precursor substance contains metal ions required for synthesizing indium phosphide nanocrystals;
2) heating to a first temperature, adding a second precursor substance into an organic solvent containing the first precursor substance, wherein the second precursor substance contains non-metallic ions required for synthesizing the indium phosphide nanocrystal, and enabling the first precursor substance and the second precursor substance to mutually contact to carry out a chemical reaction to generate the indium phosphide nanocrystal with uneven grain size;
3) And adding the indium phosphide nanocrystals with the relatively non-uniform particle size into an organic solvent with electron donating group compounds dissolved therein and with a predetermined temperature of 220-260 ℃ to produce indium phosphide nanocrystals with the relatively uniform particle size, wherein the predetermined temperature can break ionic bonds of the indium phosphide nanocrystals in the organic solvent.
2. The method of claim 1, wherein: the organic solvent comprises doping ions, and the doping ions are at least one selected from zinc ions, magnesium ions, calcium ions and aluminum ions.
3. The method of claim 1, wherein: the organic solvent is at least one of long-chain alkane, long-chain olefin, long-chain alcohol, long-chain amine, long-chain ester, long-chain fatty acid and long-chain mercaptan.
4. The method of claim 1, wherein: the electron donating group compound includes at least one of trialkyl phosphine, trialkyl phosphine oxide, alkyl amine, enamine, alkyl thiol, aryl thiol, alkyl aryl thiol, and fatty acid.
5. The method of claim 1, wherein: after the nanocrystals having a relatively non-uniform particle size are added to an organic solvent having a predetermined temperature, the temperature of the organic solvent is maintained around the predetermined temperature for 1 second to 1 hour.
6. The method of claim 1, wherein: after the nano crystal with uneven grain size is added into organic solvent with preset temperature and maintained for some time, precursor material for synthesizing the shell of nano crystal is added and maintained for some time to lower the temperature.
7. The method of claim 1, wherein: adding the nano crystals with uneven particle sizes into an organic solvent with a preset temperature, keeping the temperature for a period of time, cooling, and separating and purifying.
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| KR20180052170A (en) * | 2016-11-09 | 2018-05-18 | 시노코 유한회사 | Synthesis method of quantum dot with minimized lattice boundary defect by continuous crystal growth and quantum dot at the same |
| CN107754801B (en) * | 2017-10-18 | 2019-12-20 | 成都理工大学 | Preparation method of Fe @ Ni nanocrystal with octahedral structure |
| CN107737950B (en) * | 2017-10-25 | 2019-05-10 | 成都理工大学 | The preparation method for being uniformly distributed formula FeNi nanocrystal of octahedral structure |
| CN110655913A (en) * | 2018-06-28 | 2020-01-07 | 深圳市晟诚世纪科技有限公司 | Preparation method of nano crystal |
| CN111908436B (en) * | 2019-05-10 | 2022-12-02 | 苏州星烁纳米科技有限公司 | Preparation method of indium phosphide nanocrystalline and product prepared by same |
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| CN106435739A (en) | 2017-02-22 |
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