CN106520124A - Preparation method of fluorescent Ag2Te nanocrystals - Google Patents
Preparation method of fluorescent Ag2Te nanocrystals Download PDFInfo
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- CN106520124A CN106520124A CN201610114741.1A CN201610114741A CN106520124A CN 106520124 A CN106520124 A CN 106520124A CN 201610114741 A CN201610114741 A CN 201610114741A CN 106520124 A CN106520124 A CN 106520124A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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Abstract
The invention relates to a preparation method of fluorescent Ag2Te nanocrystals. The Ag2Te nanocrystals have a continuous light-induced near-infrared light-emitting spectrum within the range of 1350-1620 nm. The preparation method of the Ag2Te nanocrystals includes the steps that a silver source and sulfur alcohol are heated to 90-145 DEG C under protection of inert gas, tributyl phosphine tellurium is injected, and a reaction is carried out sufficiently; a mixed reaction system is cooled, then a polar solvent is added, and the Ag2Te nanocrystals are obtained through centrifuging and washing. The Ag2Te nanocrystals are good in dispersity, high in fluorescence intensity and good in stability.
Description
Technical field
The present invention be more particularly directed to one kind prepares fluorescence Ag2Te nanocrystalline method, belongs to material chemistry technical field.
Background technology
Two area's b scopes of near-infrared（1500-1700 nm）Fluorescence be reported in living imaging application the advantage that there is the existing fluorescence such as ultralow scattering, zero background, Centimeter Level penetration depth cannot reach, therefore arouse widespread concern in fields such as biomedicines.Two area b quantum dot nano-particles of near-infrared common at present all contain heavy metal Pb, Hg etc. and have virose element.Ag2Used as a kind of new two area's fluorescent nano material of near-infrared, the report of research is not but many to Te, and it is Ag that existing method is prepared to trace it to its cause2Te does not have fluorescence, or fluorescence is very weak, no using value.The standby Ag of the Pang Daiwen project team systems of Wuhan University2Te quantum dots also only have fluorescence in 1320 nm（SCI, 2015,36,1264-1268）, have no idea for fluorescence to be adjusted to two area's b scopes of near-infrared.
Therefore development favorable repeatability, fluorescence intensity are high, optical property is stable, the Ag of spectrum continuously adjustabe to two area b of near-infrared2Te is nanocrystalline to seem very urgent.
The content of the invention
It is an object of the invention to provide a kind of fluorescence Ag2Te nanocrystalline preparation method, the method adopt solvent-thermal process method, prepare the Ag in the range of 1350-1620 nm with continuous photic near-infrared luminous spectrum2Te is nanocrystalline, so as to overcome deficiency of the prior art.
For achieving the above object, present invention employs following technical scheme：
Fluorescence Ag2Te nanocrystalline preparation method is：Silver-colored source and long chain mercaptans are mixed, 90-145 DEG C is heated under inert gas shielding, tributylphosphine tellurium is injected and fully reaction obtains Ag2Te is nanocrystalline.
Further, the method is comprised the following steps：
Ith, by 2 mmol
Te powder is dissolved in 5mL tributylphosphines, standby；
IIth, silver-colored source and long chain mercaptans are heated to into 90-145 DEG C under inert gas shielding；
IIIth, tributylphosphine tellurium is injected into above-mentioned mixed solution, then the holding 1-280 min under injection temperature;
IVth, after solution is cooled to room temperature, add polar solvent, it is scrubbed and dry after obtain hydrophobicity Ag2Te nanocrystalline powders.
The silver-colored source is at least any one in silver nitrate, silver trifluoroacetate, silver acetate.
The long chain mercaptans are at least any one in lauryl mercaptan, tetradecanylthioalcohol, 16 mercaptan, stearylmercaptan.
The preparation method of the present invention can regulate and control Ag by the temperature of control injection tributylphosphine tellurium, dosage, and response time2The nanocrystalline photoluminescence spectrums of Te so as to photoluminescence spectrum continuously adjustabe in the range of the 1350-1620 nm.The preparation method of the present invention can be carried out in a mild condition, and high-volume repeats to prepare the nano-particle with same emission wavelength.
The product and existing Ag of the present invention2Te quantum dot nano-particles are compared, and luminescent emission wavelength range is wider, can be adjusted to two area's b scopes of near-infrared.
Description of the drawings
Fig. 1 is hydrophobicity Ag in embodiment 12Te nanocrystalline transmission electron microscope photo.
Fig. 2 is hydrophobicity Ag in embodiment 12Te nanocrystalline near-infrared fluorescent spectrogram.
Specific embodiment
The present invention obtains the Ag that hydrophobicity there is near-infrared fluorescent to launch by the method for injecting tributylphosphine tellurium under high temperature using silver-colored source and long chain mercaptans as reactant2Te is nanocrystalline, and wherein long chain mercaptans are used as surface ligand molecule.
From the point of view of specifically, the technique of the present invention is：Mixed using silver-colored source and long chain mercaptans, be placed in an obturator, be heated to suitable temperature injection tributylphosphine tellurium under inert gas shielding and kept for the regular hour so as to nucleating growth；Then its natural cooling, Jing centrifugations, washing is allowed to obtain hydrophobicity Ag2Te is nanocrystalline.
Additionally, the prioritization scheme of above-mentioned technical proposal can also include：
The reaction can be regulating and controlling Ag using different silver-colored sources, different mercaptan, the tributylphosphine tellurium of various dose, different injection temperatures, different response time2Te nanocrystalline size, such as rise high-temperature or extend the response time can make it is nanocrystalline become large-sized, while there is red shift in fluorescence spectrum.
Below by way of two specific embodiments, the preparation process of the present invention is discussed in detail：
Embodiment 1
The silver acetate of 0.1 mmol and the mixing of 10 g lauryl mercaptans are placed in there-necked flask, in N2110 DEG C are warming up in atmosphere, the tributylphosphine tellurium of 0.125 mL is injected, and then react 5 min at 110 DEG C, finally after solution naturally cools to room temperature, 50 mL acetone, Jing centrifugations, washing is added, it is dispersed in hexamethylene, the sample of gained is uniform monodispersed Ag2Te is nanocrystalline（As shown in Figure 1）, with near-infrared fluorescent emission spectrum as shown in Figure 2 well.
Embodiment 2
The silver nitrate of 0.1 mmol and the mixing of 18 g stearylmercaptans are placed in flask, 100 DEG C are warming up in an ar atmosphere, are injected the tributylphosphine tellurium of 0.08 mL, then 4.5 h are reacted at 100 DEG C, finally after solution naturally cools to room temperature, add 50 mL ethanol, Jing centrifugations, washing, are dried to obtain Ag2Te nanocrystalline powders.
Embodiment 3
The silver trifluoroacetate of 0.1 mmol and the mixing of 12 g, 16 mercaptan are placed in flask, in N2145 DEG C are warming up in atmosphere, the tributylphosphine tellurium of 0.15 mL is injected, then 1 min is reacted at 145 DEG C, finally after solution naturally cools to room temperature, 50 mL ethanol is added, and then Jing centrifugations, washing are dried to obtain Ag2Te nanocrystalline powders.
The above is only and have much representational embodiment in numerous concrete application examples of the invention, protection scope of the present invention is not limited in any way.All employing equivalents or equivalence replacement and the technical scheme that formed, all fall within rights protection scope of the present invention.
Claims (4)
1. a kind of fluorescence Ag2Te nanocrystalline preparation method, is characterised by, the method is：Silver-colored source and long chain mercaptans are mixed, 90-145 DEG C is heated under inert gas shielding, tributylphosphine tellurium is injected and fully reaction obtains Ag2Te is nanocrystalline.
2. a kind of fluorescence Ag according to claim 12Te nanocrystalline preparation method, it is characterised in that comprise the following steps：
Ith, silver-colored source and long chain mercaptans are heated to into 90-145 DEG C under inert gas shielding；
IIth, tributylphosphine tellurium is injected into above-mentioned mixed solution, then the holding 1-280 min under injection temperature;
IIIth, after solution is cooled to room temperature, add polar solvent, it is scrubbed and dry after obtain Ag2Te nanocrystalline powders.
3. a kind of fluorescence Ag according to claim 22Te nanocrystalline preparation method, it is characterised in that in step I, the silver-colored source are at least any one in silver nitrate, silver trifluoroacetate, silver acetate.
4. a kind of fluorescence Ag according to claim 22Te nanocrystalline preparation method, it is characterised in that in step I, the long chain mercaptans are at least any one in lauryl mercaptan, tetradecanylthioalcohol, 16 mercaptan, stearylmercaptan.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610114741.1A CN106520124A (en) | 2016-03-02 | 2016-03-02 | Preparation method of fluorescent Ag2Te nanocrystals |
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| CN201610114741.1A CN106520124A (en) | 2016-03-02 | 2016-03-02 | Preparation method of fluorescent Ag2Te nanocrystals |
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| CN201610114741.1A Pending CN106520124A (en) | 2016-03-02 | 2016-03-02 | Preparation method of fluorescent Ag2Te nanocrystals |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021029389A1 (en) * | 2019-08-15 | 2021-02-18 | Ｎｓマテリアルズ株式会社 | Quantum dots and production method therefor |
| WO2021070858A1 (en) * | 2019-10-09 | 2021-04-15 | Ｎｓマテリアルズ株式会社 | Quantum dot and method for producing same |
| WO2024024298A1 (en) * | 2022-07-29 | 2024-02-01 | 昭栄化学工業株式会社 | Infrared-absorbing quantum dot, and method for producing infrared-absorbing quantum dot |
| TWI838568B (en) | 2019-08-15 | 2024-04-11 | 日商Ｎｓ材料股份有限公司 | Quantum dots and methods for making the same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103842562A (en) * | 2011-08-02 | 2014-06-04 | 意大利理工学院 | Ordered superstructures of octapod-shaped nanocrystals, their process of fabrication and use thereof |
| CN104302572A (en) * | 2012-03-19 | 2015-01-21 | 奈科斯多特股份公司 | Light-emitting device containing flattened anisotropic colloidal semiconductor nanocrystals and processes for manufacturing such devices |
-
2016
- 2016-03-02 CN CN201610114741.1A patent/CN106520124A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103842562A (en) * | 2011-08-02 | 2014-06-04 | 意大利理工学院 | Ordered superstructures of octapod-shaped nanocrystals, their process of fabrication and use thereof |
| CN104302572A (en) * | 2012-03-19 | 2015-01-21 | 奈科斯多特股份公司 | Light-emitting device containing flattened anisotropic colloidal semiconductor nanocrystals and processes for manufacturing such devices |
Non-Patent Citations (2)
| Title |
|---|
| JEFFREY J. URBAN等: "Synergismin binary nanocrystal superlattices leads to enhanced p-type conductivity in self-assembled PbTe/Ag2Te thin films", 《NATURE MATERIALS》 * |
| YU-WEN LIU等: "Near-Infrared Absorption of Monodisperse Silver Telluride (Ag2Te) Nanocrystals and Photoconductive Response of Their Self-Assembled Superlattices", 《CHEM. MATER.》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021029389A1 (en) * | 2019-08-15 | 2021-02-18 | Ｎｓマテリアルズ株式会社 | Quantum dots and production method therefor |
| TWI838568B (en) | 2019-08-15 | 2024-04-11 | 日商Ｎｓ材料股份有限公司 | Quantum dots and methods for making the same |
| WO2021070858A1 (en) * | 2019-10-09 | 2021-04-15 | Ｎｓマテリアルズ株式会社 | Quantum dot and method for producing same |
| WO2024024298A1 (en) * | 2022-07-29 | 2024-02-01 | 昭栄化学工業株式会社 | Infrared-absorbing quantum dot, and method for producing infrared-absorbing quantum dot |
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