CN106190127A - A kind of preparation method of composite red color fluorescent nano material - Google Patents

A kind of preparation method of composite red color fluorescent nano material Download PDF

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CN106190127A
CN106190127A CN201610512416.0A CN201610512416A CN106190127A CN 106190127 A CN106190127 A CN 106190127A CN 201610512416 A CN201610512416 A CN 201610512416A CN 106190127 A CN106190127 A CN 106190127A
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cadmium
preparation
solution
red color
nano material
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陈建彬
王翔
黄明鹭
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Xiamen Jingjun Technology Co Ltd
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Xiamen Jingjun Technology Co Ltd
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    • 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
    • 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
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The present invention relates to the preparation method of a kind of composite red color fluorescent nano material, described method mainly prepares CdTe nucleus with aqueous-phase reflux method, then leniently generating a silica shell with ammonia-catalyzed teos hydrolysis in pure water phase system, last further heated backflow generates CdS cluster in silica shell.Preparation method of the present invention can obtain the composite fluorescence nano-particle with specific fluorescent emission peak and perfect optics performance, i.e. fluorescence emission peak is positioned at the red nano granule of about 625nm, its structure wraps up the thin layer of silicon dioxide of a doping CdS cluster on the surface of CdTe nucleus, for CdTe@CdS SiO2Shell structurre.The half-peak a width of 35～45nm of gained composite fluorescence nano-particle of the present invention, is expected to be applied to designing and producing of white light LEDs optics.

Description

A kind of preparation method of composite red color fluorescent nano material
Technical field
The present invention relates to nano material, the preparation method of a kind of composite red color fluorescent nano material.
Background technology
Existing White-light LED illumination/display device is normally based on InGaN blue chip and combines YAG:Ce fluorescent material conduct The design solution of light-converting material.Owing to the spectrum of YAG:Ce fluorescent material lacks effective transmitting of red band, this class The white light source that LED component produces is unsatisfactory, there is the deficiencies such as color rendering index is on the low side, colour temperature is colder.Quantum dot (i.e. II-VI Race's semiconductor nanocrystal), particularly emission peak is positioned at red fluorescence quantum dot later for 600nm, due to the optics of its excellence Character is such as with the adjustable fluorescent emission of change in size, the fluorescence emission peak of narrow symmetry, high-fluorescence quantum yield etc., permissible Replace as a kind of novel light-converting material or supplement traditional YAG:Ce fluorescent material, to promote sending out of white light LED part Optical property.
Currently, CdSe, CdSe/ZnS etc. are common high-quality quantum dot is main is to be closed by high temperature organic phase method Become.But, high temperature organic phase method needs harsh reaction condition, and the chemical raw material used is expensive and inflammable, easy Quick-fried, toxicity is relatively strong, is unfavorable for large-scale production.And aqueous phase synthesis method is with water as solvent, needed raw material and reaction condition are the most relative Green, cheap, the large-scale production for quantum dot provides the selection approach that another one is potential.But, aqueous phase synthesis method is subject to Being formed on relatively low reaction temperature (100 DEG C), reaction required time is long, causes the half-peak breadth of quantum dot product to become big, quantum yield Decline.Particularly prepare red fluorescence quantum dot (such as CdTe) with aqueous phase synthesis method, need continuous heating to reflux more than 40 hours, Time and effort consuming.Additionally, often there is photochemical stability and temperature tolerance in the quantum dot of single nucleus (such as CdTe, CdSe) The inherent shortcomings such as difference, bio-toxicity are high, are unfavorable for that it preserves and actual application for a long time.By the superficial growth at quantum dot nucleus Or cladding the second chemical material (such as CdS, ZnS, silicon dioxide etc.), forms composite fluorescence nano-particle, can be effectively Solve the problems referred to above.There is scholar's research Aqueous phase to realize covering the second chemical material, but do not propose composite Nano The fluorescent emission of grain carries out the system synthesis method of controllable adjustment.Especially, their prepared composite nanometer particle is at fluorescence The space promoted further is also had in the optical properties such as quantum yield, fluorescent emission half-peak breadth.
Chinese invention patent CN 103773358 B discloses the preparation side of a kind of CdTe/CdS/ZnS/SiO2 quantum dot Method, first in aqueous phase, is synthesized monokaryon CdTe quantum by cadmium acetate, mercaptopropionic acid and sodium hydrogen telluride；Then, will be cooled to room The reactant liquor of the CdTe quantum of temperature is transferred to the precursor liquid of the pH9.0-10.0 containing cadmium acetate, zinc sulfate and mercaptopropionic acid In, it is uniformly mixed, adds sodium sulfide solution, back flow reaction, synthesis bivalve CdTe/CdS/ZnS quantum dot；Finally, directly In the reactant liquor of CdTe/CdS/ZnS quantum dot, add tetraethyl orthosilicate, back flow reaction, synthesize CdTe/CdS/ZnS/ SiO2Quantum dot, resulting materials is four-layer structure, is followed successively by CdTe, CdS, ZnS, SiO from inside to outside2, structure is the most numerous and diverse, relates to And component is many, it is difficult to carry out controllable adjustment.
Summary of the invention
Problem to be solved by this invention is the deficiency overcoming prior art to exist, it is provided that a kind of based on water-soluble CdTe amount Cheap, the preparation method easily of the composite fluorescence nano-particle of son point, described method is mainly prepared with aqueous-phase reflux method CdTe nucleus, then leniently generates a silica shell with ammonia-catalyzed teos hydrolysis in pure water phase system Layer, last further heated backflow generates CdS cluster in silica shell.
In preparation method of the present invention, material concentration and response time are the important changes affecting end-product photoluminescent property Amount, needs to be in optimized selection by substantial amounts of orthogonal experiment.Specifically, the concentration of cadmium ion in the first reaction system, the The concentration of the concentration of CdTe nucleus, cadmium ion and TGA and adding of ratio, ammonia and tetraethyl orthosilicate in two reaction systems Enter amount, and the time of two step back flow reaction, the equal photoluminescent property that can affect the composite nanometer particle finally given, wherein, the In one reaction system, contained cadmium ion, sodium hydrogen telluride, the mol ratio of TGA are 1:0.2～0.5:1.1～2 the most suitable.
More particularly, the molar ratio of cadmium ion, sodium hydrogen telluride and TGA is being kept not in the first reaction system On the premise of becoming (1:0.3:1.3), the appropriate concentration range of contained cadmium ion is 2～20mmol/L, continues to improve material concentration The drastically decline of CdTe product luminescent properties can be caused, and too low material concentration can strengthen product and concentrate the difficulty purified.The In two reaction systems, along with the carrying out of back flow reaction, CdS cluster is gradually raw in the silica shell of CdTe nucleating surface Become, thus cause the red shift of whole composite nanometer particle fluorescence emission peak.Each material in our system thinking reaction system The concentration impact on this red shift speed (i.e. unit return time causes the degree of product fluorescent emission red shift), such as Fig. 1 and Shown in Fig. 2, result shows: the increase of CdTe nucleus concentration can cause the reduction of red shift speed, the increase of ammonia concn to cause The increase of red shift speed, and the concentration change of ethyl orthosilicate is little on the impact of red shift speed.Being found by research, second is anti- Answering in system, the mass concentration of contained cadmium telluride nucleus is corresponding after being equivalent to step 1 gained cadmium telluride solution is diluted 2-10 times Mass concentration time, product property is more stable.
After determining the optimal material concentration of two-step reaction system, it is necessary to adjust the return time of two-step reaction, By going forward one by one, the compound mode of addition, finally determine that suitable reaction condition is, in the second reaction system, contained cadmium telluride is brilliant The mass concentration that the mass concentration of core is corresponding after being equivalent to step 1 gained cadmium telluride solution is diluted 2-10 times, contained cadmium ion Being 1:3 with the mol ratio of TGA, the concentration of contained ammonia is 0.1-0.5mol/L, the molar concentration of contained tetraethyl orthosilicate For 0.01-0.03mol/L, can obtain under the conditions of being somebody's turn to do and there is specific fluorescent transmitting and the red composite quantum of excellent fluorescence property Point.
Concrete scheme is as follows:
The preparation method of a kind of composite red color fluorescent nano material, comprises the following steps:
(1) chloride hydrate cadmium is dissolved in water, adds TGA and sodium hydroxide, regulate pH to 11.4, before obtaining cadmium Liquid solution；In the cadmium precursor solution of gained, add sodium hydrogen telluride solution obtain the first reaction system, will heat back under its normal pressure Flow 8-14 hour, obtain cadmium telluride nucleus solution；
(2) adding isopropanol in the cadmium telluride nucleus solution of gained, the centrifugal rear solid obtained again is dispersed in and contains Have in the aqueous solution of cadmium ion and TGA molecule, regulate pH to 10.5, be subsequently adding ammonia and tetraethyl orthosilicate, obtain the Two reaction systems, are stirred at room temperature 2-4 hour, obtain surface parcel doping cadmium ion and the silicon dioxide of TGA The cadmium telluride quantum dot solution of shell；
(3) by surface parcel doping cadmium ion and the cadmium telluride quantum dot solution normal pressure of the silica shell of TGA Under be heated to reflux 1-3 hour, cooling reaction system afterwards, add isopropanol make product separate out, by centrifugation, washing acquisition in telluride The material C dTe@CdS-SiO of the silica shell of cadmium surfaces parcel doped cadmium sulfide cluster2, obtain described composite red color Fluorescent nano material.
Further, in described step (1), sodium hydrogen telluride solution is by tellurium powder, sodium borohydride mixing, protects at nitrogen Lower addition ultra-pure water, obtains in 40 DEG C of reacting by heating 60min.
Further, in described step (1) in cadmium precursor solution, the concentration of contained cadmium ion is 2～20mmol/L.
Further, in described step (1) in the first reaction system, contained cadmium ion, sodium hydrogen telluride, TGA Mol ratio is 1:0.2～0.5:1.1～2.
Further, the temperature being heated to reflux in described step (1) is 95-100 DEG C.
Further, described step (2) adds 2-4 times that volume is cadmium telluride nucleus liquor capacity of isopropanol.
Further, in described step (2) in the second reaction system, the mass concentration of contained cadmium telluride nucleus is equivalent to Mass concentration corresponding after step 1 gained cadmium telluride solution is diluted 2-10 times, contained cadmium ion and the mol ratio of TGA For 1:3, the concentration of contained ammonia is 0.1-0.5mol/L, and the molar concentration of contained tetraethyl orthosilicate is 0.01-0.03mol/L.
Further, described step (3) adds 2-4 times that volume is reaction system volume of isopropanol.
Further, the temperature being heated to reflux in described step (3) is 95-100 DEG C.
Preparation method of the present invention can obtain having the compound glimmering of specific fluorescent emission peak and perfect optics performance Light nano-particle, i.e. fluorescence emission peak are positioned at the red nano granule of about 625nm, and its structure is wrapped up on the surface of CdTe nucleus The thin layer of silicon dioxide of one doping CdS cluster, for shell structurre.The half-peak of gained composite fluorescence nano-particle of the present invention is a width of 35～45nm, it is expected to be applied to designing and producing of white light LEDs optics.
Accompanying drawing explanation
Fig. 1 is in the second reaction system, under different CdTe nucleus concentration, and the fluorescent emission of generated composite nanometer particle Peak position is with the red shift curve of return time；
Fig. 2 is in the second reaction system, under different ammonia and ethyl orthosilicate concentration, generated composite nanometer particle Fluorescent emission peak position is with the red shift curve of return time；
Fig. 3 is CdTe and the CdTe@CdS-SiO that the embodiment of the present invention 1 provides2The fluorescent emission of composite fluorescence nano material Spectrum；
Fig. 4 is that CdTe and the CdTe@CdS-SiO2 composite fluorescence nano material of the embodiment of the present invention 1 offer is 60 DEG C of heating Under fluorescence decay curve；
Fig. 5 is the CdTe@CdS-SiO that the embodiment of the present invention 1 provides2The solid fluorescence exciting light of composite fluorescence nano material Spectrum and emission spectrum (365nm excites).
Detailed description of the invention
Below in conjunction with embodiment, technical solution of the present invention is further elaborated.Unreceipted concrete technology or bar in embodiment Part person, according to the technology described by the document in this area or condition or is carried out according to product description.Agents useful for same or instrument Device unreceipted production firm person, be can by city available from conventional products.
Embodiment 1
(1) CdTe nucleus is prepared
A. 100.0mg tellurium powder and 67.0mg sodium borohydride are proceeded in 25mL twoport flask, after sealing a bottle with turned welt plug Vacuumizing is also filled with nitrogen protection, is then injected into 10mL ultra-pure water, in 40 DEG C of reacting by heating 60min, obtains sodium hydrogen telluride molten Liquid.
B. by 0.5960g CdCl2·2.5H2O proceeds to flask, adds 200mL water dissolution, and stirring is lower adds 235.0 μ L sulfydryls Acetic acid (is called for short TGA), is then added dropwise over 1MNaOH solution regulation pH to 11.4, obtains cadmium precursor solution.
C. whole sodium hydrogen telluride solution of aspiration step (A) gained, are being stirred vigorously and implantation step under nitrogen air-flow protection (B), in the cadmium precursor solution of gained, cadmium telluride precursor solution is obtained.
D. above cadmium telluride precursor solution is heated to reflux 12 hours at ambient pressure, obtains cadmium telluride nucleus solution.
(2) at CdTe nucleating surface parcel doping Cd2+Silica shell with TGA
A. adding isopropanol with the volume ratio of 1:3 in CdTe nucleus solution obtained as above makes product separate out, then with The rotating speed of 8000rpm is centrifuged 10 minutes, removes supernatant solution, and remaining solid product is dispersed in 20mL pure water again, obtains dilute CdTe nucleus solution after releasing, reacts for next step.
B. by 0.1508g CdCl2·2.5H2O proceeds to flask, adds 200mL water dissolution, and stirring is lower adds 138.5 μ L sulfydryls Acetic acid.Then it is added dropwise over 1MNaOH solution elder generation regulation system pH to about 9.5, adds more than 5mL CdTe nucleus concentrated solution, so The rear dropping NaOH solution that continues is to pH=10.5.
C., after continuing to add 10mL 6.25wt% ammonia spirit in above system, the positive silicic acid of 1mL under stirring, it is slowly added to Ethyl ester, the most at room temperature gentle agitation is reacted 3 hours, can generate doping Cd at CdTe nucleating surface2+Titanium dioxide with TGA Silicon shell.
(3) silica shell of doping CdS cluster is generated at CdTe nucleating surface
A. above reaction system is transferred in electric heating device, is heated to reflux under normal pressure 2 hours, can be at CdTe nucleus table Face generates the silica shell of doping CdS cluster.
B. reaction system is cooled to room temperature, adds isopropanol with the volume ratio of 1:3 and makes product separate out, then with 8000rpm Rotating speed be centrifuged 10 minutes, remove supernatant solution, solid precipitation is dispersed in 20mL pure water again.It is repeated twice centrifugal-washing Operation, to remove the Cd of nano grain surface absorption2+With other excess reactant, obtain CdS doping silicon dioxide packing CdTe (CdTe@CdS-SiO2) composite red color fluorescent nano particle.
By the CdTe nucleus prepared in embodiment 1 and end-product CdTe@CdS-SiO2Carry out fluorescence emission spectrum test, knot Fruit is such as Fig. 3.
From figure 3, it can be seen that the transmitting wavelength of CdTe nucleus is positioned at 580nm, CdTe CdS-SiO2Transmitting wavelength be positioned at 629nm, red shift 49nm, wherein CdTe@CdS-SiO2Half-peak a width of 35～45nm, peak shape is narrow and symmetrical, shows its quality Preferably.
By the CdTe nucleus prepared in embodiment 1 and end-product CdTe@CdS-SiO2Carry out the light under 60 DEG C of heating conditions Stability test, result such as Fig. 4.
From fig. 4, it can be seen that core-shell type composite nano particles has preferable light stability compared to single CdTe nucleus, The silica shell of doping CdS cluster can improve the thermostability of quantum dot kernel.
To the CdTe@CdS-SiO prepared in embodiment 12Composite fluorescence nano material carries out Solid fluorescene spectrum sign, its Excitation spectrum and emission spectrum are shown in Fig. 5.
From fig. 5, it can be seen that gained composite nano materials of the present invention has wide absorption, the fluorescent characteristic of narrow transmitting, favorably In being applied to LED illumination/display device.
Embodiment 2
(1) CdTe nucleus is prepared
A. 100.0mg tellurium powder and 67.0mg sodium borohydride are proceeded in 25mL twoport flask, after sealing a bottle with turned welt plug Vacuumizing is also filled with nitrogen protection, is then injected into 10mL ultra-pure water, in 40 DEG C of reacting by heating 60min, obtains sodium hydrogen telluride molten Liquid.
B. by 0.5960g CdCl2·2.5H2O proceeds to flask, adds 200mL water dissolution, and stirring is lower adds 235.0 μ L sulfydryls Acetic acid (is called for short TGA), is then added dropwise over 1MNaOH solution regulation pH to 11.4, obtains cadmium precursor solution.
C. whole sodium hydrogen telluride solution of aspiration step (A) gained, are being stirred vigorously and implantation step under nitrogen air-flow protection (B), in the cadmium precursor solution of gained, cadmium telluride precursor solution is obtained.
D., above cadmium telluride precursor solution is heated to 95 DEG C-100 DEG C at ambient pressure reflux 8 hours, obtains cadmium telluride brilliant Core solution.
(2) at CdTe nucleating surface parcel doping Cd2+Silica shell with TGA
A. adding isopropanol with the volume ratio of 1:3 in CdTe nucleus solution obtained as above makes product separate out, then with The rotating speed of 8000rpm is centrifuged 10 minutes, removes supernatant solution, and remaining solid product is dispersed in 20mL pure water again, obtains dilute CdTe nucleus solution after releasing, reacts for next step.
B. by 0.1508g CdCl2·2.5H2O proceeds to flask, adds 200mL water dissolution, and stirring is lower adds 138.5 μ L sulfydryls Acetic acid.Then it is added dropwise over 1MNaOH solution elder generation regulation system pH to about 9.5, adds more than 5mL CdTe nucleus concentrated solution, so The rear dropping NaOH solution that continues is to pH=10.5.
C., after continuing to add 10mL 6.25wt% ammonia spirit in above system, the positive silicic acid of 1mL under stirring, it is slowly added to Ethyl ester, the most at room temperature gentle agitation is reacted 2 hours, can generate doping Cd at CdTe nucleating surface2+Titanium dioxide with TGA Silicon shell.
(3) silica shell of doping CdS cluster is generated at CdTe nucleating surface
A. above reaction system is transferred in electric heating device, is heated to 95 DEG C-100 DEG C under normal pressure and refluxes 1 hour, The silica shell of doping CdS cluster is generated at CdTe nucleating surface.
B. reaction system is cooled to room temperature, adds isopropanol with the volume ratio of 1:3 and makes product separate out, then with 8000rpm Rotating speed be centrifuged 10 minutes, remove supernatant solution, solid precipitation is dispersed in 20mL pure water again.It is repeated twice centrifugal-washing Operation, to remove the Cd of nano grain surface absorption2+With other excess reactant, obtain CdS doping silicon dioxide packing CdTe (CdTe@CdS-SiO2) composite red color fluorescent nano particle.
The half-peak a width of 35～45nm of this composite fluorescence nano-particle, fluorescence quantum yield are about 40%, and material property is excellent Different.
Embodiment 3
(1) CdTe nucleus is prepared
A. 100.0mg tellurium powder and 67.0mg sodium borohydride are proceeded in 25mL twoport flask, after sealing a bottle with turned welt plug Vacuumizing is also filled with nitrogen protection, is then injected into 10mL ultra-pure water, in 40 DEG C of reacting by heating 60min, obtains sodium hydrogen telluride molten Liquid.
B. by 0.5960g CdCl2·2.5H2O proceeds to flask, adds 200mL water dissolution, and stirring is lower adds 235.0 μ L sulfydryls Acetic acid (is called for short TGA), is then added dropwise over 1MNaOH solution regulation pH to 11.4, obtains cadmium precursor solution.
C. whole sodium hydrogen telluride solution of aspiration step (A) gained, are being stirred vigorously and implantation step under nitrogen air-flow protection (B), in the cadmium precursor solution of gained, cadmium telluride precursor solution is obtained.
D., above cadmium telluride precursor solution is heated to 95 DEG C-100 DEG C at ambient pressure reflux 14 hours, obtains cadmium telluride brilliant Core solution.
(2) at CdTe nucleating surface parcel doping Cd2+Silica shell with TGA
A. adding isopropanol with the volume ratio of 1:3 in CdTe nucleus solution obtained as above makes product separate out, then with The rotating speed of 8000rpm is centrifuged 10 minutes, removes supernatant solution, and remaining solid product is dispersed in 20mL pure water again, obtains dilute CdTe nucleus solution after releasing, reacts for next step.
B. by 0.1508g CdCl2·2.5H2O proceeds to flask, adds 200mL water dissolution, and stirring is lower adds 138.5 μ L sulfydryls Acetic acid.Then it is added dropwise over 1MNaOH solution elder generation regulation system pH to about 9.5, adds more than 5mL CdTe nucleus concentrated solution, so The rear dropping NaOH solution that continues is to pH=10.5.
C., after continuing to add 10mL 6.25wt% ammonia spirit in above system, the positive silicic acid of 1mL under stirring, it is slowly added to Ethyl ester, the most at room temperature gentle agitation is reacted 4 hours, can generate doping Cd at CdTe nucleating surface2+Titanium dioxide with TGA Silicon shell.
(3) silica shell of doping CdS cluster is generated at CdTe nucleating surface
A. above reaction system is transferred in electric heating device, is heated to 95 DEG C-100 DEG C under normal pressure and refluxes 3 hours, The silica shell of doping CdS cluster is generated at CdTe nucleating surface.
B. reaction system is cooled to room temperature, adds isopropanol with the volume ratio of 1:3 and makes product separate out, then with 8000rpm Rotating speed be centrifuged 10 minutes, remove supernatant solution, solid precipitation is dispersed in 20mL pure water again.It is repeated twice centrifugal-washing Operation, to remove the Cd of nano grain surface absorption2+With other excess reactant, obtain CdS doping silicon dioxide packing CdTe (CdTe@CdS-SiO2) composite red color fluorescent nano particle.
The half-peak a width of 35～45nm of this composite fluorescence nano-particle, fluorescence quantum yield are about 40%, and material property is excellent Different.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is example Property, it is impossible to be interpreted as limitation of the present invention, those of ordinary skill in the art is without departing from the principle of the present invention and objective In the case of above-described embodiment can be changed within the scope of the invention, revise, replace and modification.

Claims (9)

1. the preparation method of a composite red color fluorescent nano material, it is characterised in that: comprise the following steps:
(1) chloride hydrate cadmium is dissolved in water, adds TGA and sodium hydroxide, regulate pH to 11.4, obtain cadmium precursor molten Liquid；In the cadmium precursor solution of gained, add sodium hydrogen telluride solution obtain the first reaction system, 8-will be heated to reflux under its normal pressure 14 hours, obtain cadmium telluride nucleus solution；
(2) adding isopropanol in the cadmium telluride nucleus solution of gained, the centrifugal rear solid obtained is dispersed in again containing cadmium In the aqueous solution of ion and TGA molecule, regulate pH to 10.5, be subsequently adding ammonia and tetraethyl orthosilicate, obtain second anti- Answer system, be stirred at room temperature 2-4 hour, obtain surface parcel doping cadmium ion and the silica shell of TGA Cadmium telluride quantum dot solution；
(3) will add under the cadmium telluride quantum dot solution normal pressure of surface parcel doping cadmium ion and the silica shell of TGA Hot reflux 1-3 hour, afterwards cooling reaction system, add isopropanol and make product separate out, and by centrifugation, washs acquisition at cadmium telluride table Bread wraps up in the material C dTe@CdS-SiO of the silica shell of doped cadmium sulfide cluster2, obtain described composite red color fluorescence Nano material.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (1) in, sodium hydrogen telluride solution is by tellurium powder, sodium borohydride mixing, adds ultra-pure water under nitrogen protection, in 40 DEG C of reacting by heating 60min obtains.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (1), in cadmium precursor solution, the concentration of contained cadmium ion is 2～20mmol/L.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (1), in the first reaction system, contained cadmium ion, sodium hydrogen telluride, the mol ratio of TGA are 1:0.2～0.5:1.1～2.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (1) temperature being heated to reflux in is 95-100 DEG C.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (2) 2-4 times that volume is cadmium telluride nucleus liquor capacity of isopropanol is added in.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (2), in the second reaction system, the mass concentration of contained cadmium telluride nucleus is equivalent to step 1 gained cadmium telluride solution is diluted 2- Mass concentration corresponding after 10 times, the mol ratio of contained cadmium ion and TGA is 1:3, and the concentration of contained ammonia is 0.1- 0.5mol/L, the molar concentration of contained tetraethyl orthosilicate is 0.01-0.03mol/L.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (3) 2-4 times that volume is reaction system volume of isopropanol is added in.
The preparation method of composite red color fluorescent nano material the most according to claim 1, it is characterised in that: described step (3) temperature being heated to reflux in is 95-100 DEG C.
CN201610512416.0A 2016-07-01 2016-07-01 A kind of preparation method of composite red color fluorescent nano material Pending CN106190127A (en)

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Cited By (1)

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CN113072839A (en) * 2021-03-11 2021-07-06 龙南鑫坤无机新材料有限公司 Bright scarlet coating pigment for ceramic ink-jet printing and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
MURASE: "Anomalous Photoluminescence in Silica-Coated Semiconductor Nanocrystals After Heat Treatment", 《SMALL》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113072839A (en) * 2021-03-11 2021-07-06 龙南鑫坤无机新材料有限公司 Bright scarlet coating pigment for ceramic ink-jet printing and preparation method thereof
CN113072839B (en) * 2021-03-11 2023-01-03 龙南鑫坤无机新材料有限公司 Bright bright scarlet coating pigment for ceramic ink-jet printing and preparation method thereof

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