CN105885846B - The preparation method of CdTe quantum/stratified material composite phosphor - Google Patents
The preparation method of CdTe quantum/stratified material composite phosphor Download PDFInfo
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- CN105885846B CN105885846B CN201510025472.7A CN201510025472A CN105885846B CN 105885846 B CN105885846 B CN 105885846B CN 201510025472 A CN201510025472 A CN 201510025472A CN 105885846 B CN105885846 B CN 105885846B
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Abstract
The present invention relates to a kind of preparation methods of CdTe quantum/stratified material composite phosphor, for raw material, CdTe quantum/stratified material composite phosphor is prepared using the method for electrostatic assembly with CdTe quantum and stratified material (magadiite, montmorillonite, α basic zirconium phosphates) for this method.Prepared CdTe quantum/stratified material composite phosphor fluorescence property is excellent.The invented technology is simple, of low cost, there is good application prospect.
Description
Technical field
The present invention relates to a kind of preparation methods of CdTe quantum/stratified material composite phosphor, belong to nano material system
The field of standby technology.
Background technology
Semiconductor-quantum-point has widely because of it in photoelectric device, the fields such as device for non-linear optical and biomarker
Using and be concerned.Quantum dot can be stabilized in the solution, therefore be typically to be dispersed in organic solvent or water
Colloidal form applied, but after its Precipitation because the unstability on surface easily occur reunite due to lose original quantum
Dimensional effect and optical advantage, and for most of nano-particles, this reunion is irreversible.Quantum dot is applied to solid
The greatest difficulty faced in body integrated device is the stability and dispersibility for ensureing quantum dot in solid matrix.In order to solve this
A problem, people have been working on synthesis quantum dot/polymer nanocomposite and the inorganic nano combined object of quantum dot.Although people
Huge effort is made in the preparation of inorganic nano combined object, but finding more easy prepare has excellent fluorescence property
Quantum dot inorganic nano composite material method be still people endeavour pursue target.
Stratified material is a kind of compound with laminated body structure, such as inorganic silicate, phosphate stratiform chemical combination
Object has the space structure that specific structural unit is formed by corner-sharing, side, face accumulation, and interlayer has moveable oppositely charged
Ion or neutral molecule, to compensate the charge balance of laminate.There are strong covalent bond effects, interlayer in layer then generally to deposit
In the weak interaction such as Van der Waals force or electrostatic force.This structure of lamellar compound imparts its two characteristic：Interlayer from
Son interchangeability, exchange after product have higher stability.This just beats to construct composite material based on lamellar compound
Basis is descended.Using electrostatic assembly method, CdTe quantum is introduced into laminated body, is made using the confinement of laminated body laminate
With being expected to obtain the excellent CdTe quantum of stable fluorescence property/stratified material composite phosphor.
Invention content
The purpose of the present invention is to provide a kind of preparation method of CdTe quantum/stratified material composite phosphor, the party
Method with CdTe quantum and stratified material (montmorillonite, magadiite, alpha zirconium phosphate) for raw material, using the method for electrostatic assembly
Prepare the excellent CdTe quantum of fluorescence property/stratified material composite phosphor.
The preparation method of 1.CdTe quantum dots/stratified material composite phosphor, is as follows：
(1) preparation of tellurium source NaHTe：By NaBH4It is placed in reactor A, adds deionized water dissolving, use N2Purge A
5min, after rapidly join Te powder, make NaBH4Mass ratio with Te powder is 2: 1,80 DEG C of closed stirrings of water bath condition, makes black Te
Powder all dissolves, and eventually becomes colourless transparent solution.
(2) the electronegative CdTe quantum in synthesis in water surface：Using water as solvent, by cadmium salt (including caddy, cadmium nitrate
Or one of their hydrate) be completely dissolved in reactor B and make cadmium salt a concentration of 10-3M, closed stirring, then sulfhydrylation is added dropwise
It closes object (including thioacetic acid, mercaptopropionic acid or dimercaptosuccinic acid) and forms cadmium salt-mercapto-complex, make cadmium salt Cd2+With sulfhydrylation
It is 3: 1 to close object molar ratio, and pH=8~11 are adjusted, then prepared in a dropping step (1) into cadmium salt-mercapto-complex with NaOH
Tellurium source NaHTe solution, make cadmium salt Cd2+It is 10: 1 with NaHTe molar ratios, inert gas N2Protection is returned after agitating and heating boiling
Flow 20min~12h.
(3) the CdTe quantum solution and layer of the electronegative sulfhydryl compound modification in surface step (2) being prepared
Between positively charged stratified material mixed, room temperature magnetic agitation 1-12h.It centrifuges, washs later, 60 DEG C of dry 2h are obtained
Obtain CdTe quantum/stratified material composite phosphor.
Compound CdTe quantum mass fraction is in heretofore described CdTe quantum/stratified material composite phosphor
0.5~5%, the stratified material stratiform material positively charged for the pillared rear interlayer of cetyl trimethylammonium bromide cation
Material, the stratified material raw material include natural montmorillonite, the magadiite of hydrothermal synthesis, the alpha zirconium phosphate of hydrothermal synthesis.
2. it is had the following advantages according to preparation method of the present invention：
(1) CdTe quantum/stratified material composite phosphor fluorescence property prepared by is excellent.
(2) invented technology is simple, of low cost, there is good application prospect.
Description of the drawings
The XRD diagram of the CdTe quantum of Fig. 1 embodiments 2/magadiite composite phosphor
Photo under the ultraviolet lamp of the CdTe quantum of Fig. 2 embodiments 2/magadiite composite phosphor
The fluorescence spectra of the CdTe quantum of Fig. 3 embodiments 2/magadiite composite phosphor
The fluorescence spectra of the CdTe quantum of Fig. 4 embodiments 5/montmorillonite Composite fluorescent powder
The fluorescence spectra of the CdTe quantum of Fig. 5 embodiments 6/alpha zirconium phosphate composite phosphor
Specific embodiment
It is further illustrated the present invention below in conjunction with example, embodiment 1-6 is preparating example, which is only used for
It is bright, the practical ranges without limiting the present invention.
Embodiment 1
(1) preparation of tellurium source NaHTe：Weigh 0.12g NaBH4It is placed in reactor A, adds deionized water dissolving, use N2It blows
Sweep reactor A 5min, after rapidly join 0.06g Te powder, 80 DEG C of closed stirrings of water bath condition make black Te powder all dissolve,
Eventually become colourless transparent solution.
(2) the electronegative CdTe quantum in synthesis in water surface：0.23g CdCl are added in into 500mL three-necked flasks2·
2.5H2O, and with 240mL deionized water dissolvings, lead to N220min is stirred, 200 μ L thioacetic acid are injected, with 2mol/L NaOH solutions
PH value of solution=10 in flask are adjusted, continue logical N2And after being vigorously stirred 20min, it is freshly prepared 0.4mL to be drawn with needle tubing rapidly
In NaHTe solution injection flask, make n (Cd2+)∶n(Te2-): n (TGA)=1: 0.1: 3, flow back 20min after agitating and heating boiling,
Obtain the CdTe quantum solution that maximum emission wavelength is 532nm.
(3) pass through SiO2-NaOH-Na2CO3System hydrothermal synthesis magadiite, then to synthesized magadiite
Acidification stripping, further introduce cetyl trimethylammonium bromide carry out it is pillared obtain cetyl trimethylammonium bromide sun from
The pillared magadiite of son.The CdTe quantum solution that step (2) is obtained and cetyl trimethylammonium bromide cation
Magadiite after pillared is mixed by liquid-solid ratio for 50mL/0.5g, room temperature magnetic agitation 5h.It centrifuges, washes later
It washs, 60 DEG C of dry 2h, obtains CdTe quantum/magadiite composite phosphor that CdTe quantum mass fraction is 1%,
Maximum emission wavelength is 532nm.
Embodiment 2
(1) preparation of tellurium source NaHTe such as embodiment 1 (1).
(2) the electronegative CdTe quantum in synthesis in water surface and embodiment 1 (2) the difference lies in：It flows back after boiling
Time is 2h, obtains the CdTe quantum solution that maximum emission wavelength is 550nm.
(3) the preparation such as embodiment 1 (3) of the pillared magadiite of cetyl trimethylammonium bromide cation.Then
The magadiite of CdTe quantum solution that step (2) is obtained and cetyl trimethylammonium bromide cation after pillared by
Liquid-solid ratio is mixed for 50mL/0.5g, room temperature magnetic agitation 5h.It centrifuges, washs later, 60 DEG C of dry 2h are obtained
CdTe quantum mass fraction is 1% CdTe quantum/magadiite composite phosphor, and maximum emission wavelength is
555nm。
Embodiment 3
(1) preparation of tellurium source NaHTe such as embodiment 1 (1).
(2) the electronegative CdTe quantum in synthesis in water surface and embodiment 1 (2) the difference lies in：PH=11, boiling
Return time is 12h afterwards, obtains the CdTe quantum solution that maximum emission wavelength is 578nm.
(3) the preparation such as embodiment 1 (3) of the pillared magadiite of cetyl trimethylammonium bromide cation.Then
The magadiite of CdTe quantum solution that step (2) is obtained and cetyl trimethylammonium bromide cation after pillared by
Liquid-solid ratio is mixed for 50mL/0.5g, room temperature magnetic agitation 5h.It centrifuges, washs later, 60 DEG C of dry 2h are obtained
CdTe quantum mass fraction is 1% CdTe quantum/magadiite composite phosphor, and maximum emission wavelength is
591nm。
Embodiment 4
(1) preparation of tellurium source NaHTe such as embodiment 1 (1).
(2) the electronegative CdTe quantum in synthesis in water surface such as embodiment 2 (2) obtains maximum emission wavelength as 550nm
CdTe quantum solution.
(3) this step and embodiment 2 (3) the difference lies in：By CdTe quantum solution and cetyl trimethyl bromine
Magadiite after change ammonium cation is pillared is mixed by liquid-solid ratio for 75mL/0.5g, room temperature magnetic agitation 5h.Later from
The heart detaches, washing, 60 DEG C of dry 2h, and it is multiple to obtain CdTe quantum/magadiite that CdTe quantum mass fraction is 1.5%
Close fluorescent powder, maximum emission wavelength 558nm.
Embodiment 5
(1) preparation of tellurium source NaHTe such as embodiment 1 (1).
(2) the electronegative CdTe quantum in synthesis in water surface such as embodiment 2 (2) obtains maximum emission wavelength as 550nm
CdTe quantum solution.
(3) it is pillared to natural montmorillonite progress using cetyl trimethylammonium bromide, then step (2) is obtained
Montmorillonite after CdTe quantum solution and cetyl trimethylammonium bromide cation are pillared by liquid-solid ratio for 25mL/0.5g into
Row mixing, room temperature magnetic agitation 5h.It centrifuges, washs, 60 DEG C of dry 2h, obtaining CdTe quantum mass fraction is later
0.5% CdTe quantum/montmorillonite Composite fluorescent powder, maximum emission wavelength 555nm.
Embodiment 6
(1) preparation of tellurium source NaHTe such as embodiment 1 (1).
(2) the electronegative CdTe quantum in synthesis in water surface and embodiment 1 (2) the difference lies in：It flows back after boiling
Time is 6h, obtains the CdTe quantum solution that maximum emission wavelength is 560nm.
(3) with ZrOCl2·8H2O、H3PO4For raw material hydrothermal synthesis alpha zirconium phosphate, then synthesized alpha zirconium phosphate is shelled
From further introducing cetyl trimethylammonium bromide and carry out that pillared to obtain cetyl trimethylammonium bromide cation pillared
Alpha zirconium phosphate.After CdTe quantum solution that step (2) is obtained and cetyl trimethylammonium bromide cation are pillared
Alpha zirconium phosphate is mixed by liquid-solid ratio for 25mL/0.5g, room temperature magnetic agitation 5h.It centrifuges, washs, 60 DEG C of dryings later
2h obtains CdTe quantum/alpha zirconium phosphate composite phosphor that CdTe quantum mass fraction is 0.5%, emission maximum wave
A length of 567nm.
Claims (3)
- A kind of 1. preparation method of CdTe quantum/stratified material composite phosphor, which is characterized in that the CdTe quantum Point/stratified material composite phosphor is that electrostatic occurs by the CdTe quantum of the electrically charged stratified material of interlayer and oppositely charged Assembling obtains；The layered material stratified material positively charged for the pillared rear interlayer of cetyl trimethylammonium bromide cation, it is used Stratified material raw material is the magadiite of hydrothermal synthesis.
- 2. the preparation method of CdTe quantum according to claim 1/stratified material composite phosphor, which is characterized in that Compound CdTe quantum mass fraction is 0.5~5% in the CdTe quantum/stratified material composite phosphor.
- 3. the preparation method of CdTe quantum according to claim 1/stratified material composite phosphor, which is characterized in that It is as follows：(1) preparation of tellurium source NaHTe：By NaBH4It is placed in reactor A, adds deionized water dissolving, use N2Purge A5min, after rapidly join Te powder, make NaBH4Mass ratio with Te powder is 2: 1,80 DEG C of closed stirrings of water bath condition, makes black Te Powder all dissolves, and eventually becomes colourless transparent solution；(2) the electronegative CdTe quantum in synthesis in water surface：Using water as solvent, by caddy, cadmium nitrate or their hydration One of object, which is completely dissolved in reactor B, makes cadmium salt a concentration of 10-3M, closed stirring, then be added dropwise thioacetic acid, mercaptopropionic acid or Dimercaptosuccinic acid forms cadmium salt-mercapto-complex, makes cadmium salt Cd2+It is 3: 1 with sulfhydryl compound molar ratio, pH=is adjusted with NaOH 8~11, then the tellurium source NaHTe solution prepared in a dropping step (1) into cadmium salt-mercapto-complex, make cadmium salt Cd2+With NaHTe molar ratios are 10: 1, inert gas N2It protects, flow back 20min~12h after ebuillition of heated；(3) the CdTe quantum solution and interlayer band of the electronegative sulfhydryl compound modification in surface step (2) being prepared The stratified material of positive electricity is mixed, 1~12h of room temperature magnetic agitation；It centrifuges, washs, 60 DEG C of dry 2h later, obtain CdTe quantum/stratified material composite phosphor.
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| CN106959289B (en) * | 2017-03-22 | 2019-07-12 | 东南大学 | A kind of electrogenerated chemiluminescence material, preparation method and application |
| CN109679645A (en) * | 2018-12-23 | 2019-04-26 | 天津纳美纳米科技有限公司 | A kind of preparation method of high stability perovskite quantum dot |
| CN113049839B (en) * | 2019-12-27 | 2022-11-29 | 桂林英美特生物技术研究所 | Stable liver function composite quality control product |
| CN111334280B (en) * | 2020-01-17 | 2021-07-02 | 华中科技大学 | Fluorescent powder quantum dot composite particle and preparation method and application thereof |
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