CN101805605A - Attapulgite clay quantum dot nano-composite fluorescent material and preparation method thereof - Google Patents
Attapulgite clay quantum dot nano-composite fluorescent material and preparation method thereof Download PDFInfo
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- CN101805605A CN101805605A CN 201010145046 CN201010145046A CN101805605A CN 101805605 A CN101805605 A CN 101805605A CN 201010145046 CN201010145046 CN 201010145046 CN 201010145046 A CN201010145046 A CN 201010145046A CN 101805605 A CN101805605 A CN 101805605A
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Abstract
The invention relates to an attapulgite clay quantum dot nano-composite fluorescent material and a preparation method thereof, the material comprises inorganic quantum dots and uniformly dispersed nano-attapulgite clay, the quantum dots are positioned in pore paths of the nano-attapulgite clay, and the inorganic quantum dots are zinc oxide, zinc sulfide or cadmium sulfide. The method comprises the following steps: a) adding the nano-attapulgite clay into water solution of metal ion salt, carrying out magnetic stirring for 1-60h at the temperature of 20-80 DEG C, carrying out centrifugation on solids, cleaning with deionized water, drying and obtaining attapulgite clay/metal ions; and b) taking the attapulgite clay/metal ions, carrying out reaction on the attapulgite clay/metal ions and a negative ion source for 1-60h at the temperature of 20-80 DEG C, carrying out the centrifugation on the solids, washing, drying and obtaining the attapulgite clay quantum dot nano-composite fluorescent material. The prepared attapulgite clay quantum dot composite material is the one-dimensional nano-material with uniform size and integration of the fluorescence property of the quantum dots and the water solubility of the attapulgite clay, fluorescence is derived from the intrinsic luminescence of the quantum dots in the pore paths, and the size of the quantum dots is controllable.
Description
Technical field
The present invention relates to a kind of attapulgite/quantum dot nano-composite fluorescent material, be specifically related to the preparation method of this matrix material.
Background technology
(quantum QDs) is called semiconductor nanocrystal again to quantum dot, has good fluorescence property, and particularly water miscible quantum dot is showing extremely wide application prospect aspect biological chemistry, molecular biology, cytobiology and the medical research.Yet the preparation method of quantum dot is many based on organic synthesis, and what obtain is fat-soluble product, has greatly hindered the application of quantum dot in the biological study field.Fat-soluble quantum dot surface is coated one deck Thiovanic acid, can improve its water-soluble [Science281 (5385), 2016 (1998)]; Adopt water synthetic method, directly obtaining pan coating has the water-soluble quantum dot of Thiovanic acid [J Phys Chem B, 106 (29), 7177 (2002)]; The quantum dot bag also can be improved water-soluble [Science, 298 (5599), 1759 (2002)] in liposome.These methods are because the unstable of Thiovanic acid and liposome makes above-mentioned quantum dot very easily degrade; The quantum dot surface is superscribed SiO
2Layer makes its water-soluble and stable being improved though make nucleocapsid shape structure, and fluorescence intensity obviously descends, thereby has hindered its further Biology Applications [Science, 281 (5385), 2013 (1998)].
Summary of the invention
Technical problem: up to the present, the preparation fluorescence quantum efficiency is higher, photochemical stability good, have the technical barrier that water miscible quantum dot composite material is still existence.Therefore, the invention provides a kind of attapulgite clay quantum dot nano-composite fluorescent material and preparation method thereof, to adapt to its widespread use at biomedical sector.
Technical scheme: attapulgite be a kind of have a layer chain-like structure contain Shuifu County's magnesium alumino metasilicate clay mineral, monodimension nanometer material for natural size homogeneous, hydroxyl that the surface exists and the inner pore passage structure that exists have been given its good colloidality, adsorptivity, ion exchangeable etc., and cheap, successfully be used for many-sided industrial application.
A kind of attapulgite clay quantum dot nano-composite fluorescent material of the present invention, this material comprises inorganic quantum dot and finely dispersed nano-attapulgite, its quantum dot is positioned at the inside, duct of nano-attapulgite, and described inorganic quantum dot is zinc oxide, zinc sulphide or Cadmium Sulfide.
The preparation method of a kind of attapulgite clay quantum dot nano-composite fluorescent material of the present invention may further comprise the steps:
A. add nano-attapulgite in the aqueous solution of metal cation salt, 20-80 ℃ of lower magnetic force stirs 1-60h, with solid centrifugal after, washed with de-ionized water, after the oven dry attapulgite/metal ion,
B. get attapulgite/metal ion, itself and negative ion source are reacted 1-60h down at 20-80 ℃, solid is centrifugal, and washing obtains attapulgite clay quantum dot nano-composite fluorescent material after the oven dry.
The described metal cation salt of described step a is zinc acetate, zinc chloride or Cadmium chloride fine powder.
The described negative ion source of described step b is sodium hydroxide, sodium sulphite, hydrogen sulfide or thiocarbamide.
Beneficial effect: utilize attapulgite clay quantum dot matrix material that the present invention makes monodimension nanometer material for the size homogeneous, have the water-soluble of the fluorescence property of quantum dot and attapulgite concurrently, it is luminous that its fluorescence derives from the intrinsic of the inner quantum dot in duct, the quantum dot controllable size.
The preparation method has easy, easy row, low-cost and pollution-less and safe advantage can be by regulating the rod-like nano particle that other raw material obtains different emission wavelengths.
Description of drawings
Fig. 1 is the fluorescence spectrum figure of the embodiment of the invention 1 gained,
Fig. 2 is the fluorescence spectrum figure of the embodiment of the invention 2 gained.
Embodiment
Attapulgite clay quantum dot nano-composite fluorescent material of the present invention comprises inorganic quantum dot and finely dispersed nano-attapulgite, and its quantum dot is positioned at the inside, duct of nano-attapulgite.
Inorganic quantum dot is zinc oxide, zinc sulphide or Cadmium Sulfide.
The preparation method of attapulgite clay quantum dot nano-composite fluorescent material of the present invention may further comprise the steps:
A. add nano-attapulgite in the aqueous solution of metal cation salt, 20-80 ℃ of lower magnetic force stirs 1-60h, with solid centrifugal after, washed with de-ionized water, after the oven dry attapulgite/metal ion,
B. get attapulgite/metal ion, itself and negative ion source are reacted 1-60h down at 20-80 ℃, solid is centrifugal, and washing obtains attapulgite clay quantum dot nano-composite fluorescent material after the oven dry.
The described metal cation salt of step a is zinc acetate, zinc chloride or Cadmium chloride fine powder.
The described negative ion source of step b is sodium hydroxide, sodium sulphite, hydrogen sulfide or thiocarbamide.
Embodiment 1: add the 0.15g nano-attapulgite in reaction vessel, 30ml concentration is the Zn (CH of 0.1M
3COO)
2Solution, 30 ℃ of lower magnetic forces stir 8h, with solid centrifugal after, washed with de-ionized water, after the oven dry attapulgite/Zn
2+Get an amount of attapulgite/Zn
2+, adding 40ml concentration and be in the ethanolic soln of NaOH of 0.25M, 65 ℃ of lower magnetic forces stir 12h.Solid is centrifugal, use washing with alcohol, obtain attapulgite/ZnO composite nano materials after the oven dry.
Embodiment 2: add the 0.13g nano-attapulgite in reaction vessel, 30ml concentration is the CdCl of 0.1M
2Solution, room temperature lower magnetic force stir 24h, with solid centrifugal after, washed with de-ionized water, after the oven dry attapulgite/Cd
2+To an amount of attapulgite/Cd
2+Middle adding 40ml concentration is the Na of 0.25M
2The ethanolic soln of S, the room temperature lower magnetic force stirs 24h.After reaction finishes the solid eccentric cleaning is neutral to pH, obtains attapulgite/CdS composite nano materials after the oven dry.
Embodiment 3: add the 0.13g attapulgite in reaction vessel, 30ml concentration is the CdCl of 0.1M
2Solution, room temperature lower magnetic force stir 24h, with solid centrifugal after, washed with de-ionized water, after the oven dry attapulgite/Cd
2+With attapulgite/Cd
2+Solid feeds H behind 110 ℃ of vacuum-drying 2h
2S gas obtains attapulgite/CdS composite nano materials behind the reaction 12h.
Embodiment 4: add the 0.13g attapulgite in reaction vessel, 30ml concentration is the CdCl of 0.1M
2Solution, the room temperature lower magnetic force stirs 24h, with the centrifugal back of solid washed with de-ionized water, gets attapulgite/Cd after the oven dry
2+To attapulgite/Cd
2+Adding 15ml concentration in the solid is the NaOH solution of 0.8M, and magnetic agitation is even, is heated to 90 ℃, adds the thiourea solution that an amount of concentration is 0.1M again, reaction 8h.With the solid eccentric cleaning, obtain attapulgite/CdS composite nano materials after the oven dry.
Claims (4)
1. attapulgite clay quantum dot nano-composite fluorescent material, it is characterized in that this material comprises inorganic quantum dot and finely dispersed nano-attapulgite, its quantum dot is positioned at the inside, duct of nano-attapulgite, and described inorganic quantum dot is zinc oxide, zinc sulphide or Cadmium Sulfide.
2. the preparation method of an attapulgite clay quantum dot nano-composite fluorescent material is characterized in that this method may further comprise the steps:
A. add nano-attapulgite in the aqueous solution of metal cation salt, 20-80 ℃ of lower magnetic force stirs 1-60h, with solid centrifugal after, washed with de-ionized water, after the oven dry attapulgite/metal ion,
B. get attapulgite/metal ion, itself and negative ion source are reacted 1-60h down at 20-80 ℃, solid is centrifugal, and washing obtains attapulgite clay quantum dot nano-composite fluorescent material after the oven dry.
3. the preparation method of a kind of attapulgite clay quantum dot nano-composite fluorescent material according to claim 2 is characterized in that the described metal cation salt of step a is zinc acetate, zinc chloride or Cadmium chloride fine powder.
4. the preparation method of a kind of attapulgite clay quantum dot nano-composite fluorescent material according to claim 2 is characterized in that the described negative ion source of step b is sodium hydroxide, sodium sulphite, hydrogen sulfide or thiocarbamide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350365A (en) * | 2011-08-16 | 2012-02-15 | 淮阴师范学院 | Synthesis method of CdS-attapulgite photoelectric composite material |
| CN107090289A (en) * | 2017-04-25 | 2017-08-25 | 安徽博硕科技有限公司 | A kind of preparation method of attapulgite loaded artificial schellite and Zinc Tungstate co-precipitated materials |
| CN109880613A (en) * | 2019-02-28 | 2019-06-14 | 苏州星烁纳米科技有限公司 | Quantum dot compound and preparation method thereof, quantum dot LED light source |
| CN109957391A (en) * | 2017-12-26 | 2019-07-02 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method |
| CN110394183A (en) * | 2019-07-29 | 2019-11-01 | 常州大学 | A kind of ATP/Zn0.5Cd0.5The preparation method of S composite visible light catalyst |
| CN111545190A (en) * | 2020-05-27 | 2020-08-18 | 常州大学 | Preparation method of non-stoichiometric molybdenum oxide/modified attapulgite composite material and application of non-stoichiometric molybdenum oxide/modified attapulgite composite material in photocatalytic denitration |
| CN113959994A (en) * | 2020-07-20 | 2022-01-21 | Tcl科技集团股份有限公司 | Method for detecting residual metal ions in quantum dots |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101000809A (en) * | 2006-12-31 | 2007-07-18 | 江苏工业学院 | Preparation method of nano-conducting attapulgite material |
| CN101352677A (en) * | 2008-09-11 | 2009-01-28 | 北京理工大学 | Sepiolite supported nano zinc oxide photocatalysis material and preparation method thereof |
| KR20090066096A (en) * | 2007-12-18 | 2009-06-23 | 한국화학연구원 | Nano fluorescent material for targeting cell |
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2010
- 2010-04-12 CN CN 201010145046 patent/CN101805605A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101000809A (en) * | 2006-12-31 | 2007-07-18 | 江苏工业学院 | Preparation method of nano-conducting attapulgite material |
| KR20090066096A (en) * | 2007-12-18 | 2009-06-23 | 한국화학연구원 | Nano fluorescent material for targeting cell |
| CN101352677A (en) * | 2008-09-11 | 2009-01-28 | 北京理工大学 | Sepiolite supported nano zinc oxide photocatalysis material and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350365A (en) * | 2011-08-16 | 2012-02-15 | 淮阴师范学院 | Synthesis method of CdS-attapulgite photoelectric composite material |
| CN107090289A (en) * | 2017-04-25 | 2017-08-25 | 安徽博硕科技有限公司 | A kind of preparation method of attapulgite loaded artificial schellite and Zinc Tungstate co-precipitated materials |
| CN109957391A (en) * | 2017-12-26 | 2019-07-02 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method |
| CN109880613A (en) * | 2019-02-28 | 2019-06-14 | 苏州星烁纳米科技有限公司 | Quantum dot compound and preparation method thereof, quantum dot LED light source |
| CN110394183A (en) * | 2019-07-29 | 2019-11-01 | 常州大学 | A kind of ATP/Zn0.5Cd0.5The preparation method of S composite visible light catalyst |
| CN111545190A (en) * | 2020-05-27 | 2020-08-18 | 常州大学 | Preparation method of non-stoichiometric molybdenum oxide/modified attapulgite composite material and application of non-stoichiometric molybdenum oxide/modified attapulgite composite material in photocatalytic denitration |
| CN111545190B (en) * | 2020-05-27 | 2023-03-24 | 常州大学 | Preparation method of non-stoichiometric molybdenum oxide/modified attapulgite composite material and application of non-stoichiometric molybdenum oxide/modified attapulgite composite material in photocatalytic denitration |
| CN113959994A (en) * | 2020-07-20 | 2022-01-21 | Tcl科技集团股份有限公司 | Method for detecting residual metal ions in quantum dots |
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Application publication date: 20100818 |