CN103965912B - Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED - Google Patents

Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED Download PDF

Info

Publication number
CN103965912B
CN103965912B CN201410216614.3A CN201410216614A CN103965912B CN 103965912 B CN103965912 B CN 103965912B CN 201410216614 A CN201410216614 A CN 201410216614A CN 103965912 B CN103965912 B CN 103965912B
Authority
CN
China
Prior art keywords
self
assembled material
aqueous
add
mol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201410216614.3A
Other languages
Chinese (zh)
Other versions
CN103965912A (en
Inventor
张皓
周鼎
刘敏
林敏�
杨柏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jilin University
Original Assignee
Jilin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jilin University filed Critical Jilin University
Priority to CN201410216614.3A priority Critical patent/CN103965912B/en
Publication of CN103965912A publication Critical patent/CN103965912A/en
Application granted granted Critical
Publication of CN103965912B publication Critical patent/CN103965912B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Luminescent Compositions (AREA)

Abstract

Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED, belong to LED encapsulation material preparing technical field.The method is by regulating the ratio between various reaction raw materials, place through the room temperature short period of time, the one dimension self-assembled material of the spontaneous hyperfluorescenceZeng Yongminggaoyingguang high stability separated from growth media in a large number just can be obtained at container bottom, and the self-assembled material obtained is applied in the packaged material of LED, and then obtains the white LED light source of high-color rendering.Raw materials used in preparation is cadmium salt, mercury salt, ionic tellurium source and/or ionic selenium source or ionic sulphur source, sulfydryl small molecules, sodium borohydride, ammoniac compounds, its mol ratio can regulate arbitrarily within the scope of 1:0-2:0.1-0.8:1.5-2.4:1-10.5:600-1200.Self-assembled material method of preparing in the present invention is applicable to the semi-conductor nano particles that different methods prepares, and has universality.

Description

Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED
Technical field
The invention belongs to LED encapsulation material technical field, one dimension self-assembled material be made up of inorganic semiconductor nanoparticle prepared under being specifically related to a kind of room temperature and preparation method thereof, the method is by regulating the ratio between various reaction raw materials, place through the room temperature short period of time, the one dimension self-assembled material of the spontaneous hyperfluorescenceZeng Yongminggaoyingguang high stability separated from growth media in a large number just can be obtained at container bottom, and the self-assembled material obtained is applied in LED encapsulation material, and then obtains the LED light source of high-color rendering.
Background technology
Photodiode (LED), as a kind of emerging artificial light in recent years, because its cost is low, the advantage such as the few and trigger voltage of long service life, high brightness, reduce power consumption, heat production is low, causes the extensive research interest of people.At present, on market, the preparation of commercial LED is mainly divided into two processes: (1) adopts InGaN/GaN material to prepare the LED lamp that electroluminescent is blue light; (2) rare earth material with photoluminescent property is utilized to encapsulate wick.When LED is energized, the fluorescent substance in the blue-light excited packaged material that wick sends, is excited the fluorescence produced and the blue light compound that is not predominantly absorbed, thus produces shades of colour LED light source.Along with updating of manufacture craft, it is found that existing rare earth class packaged material can not meet the increasing requirement of people gradually, as the aspect such as color developing and brightness.Because the peak width at half height of fluorescent substance in conventional encapsulant is very wide, cause and reduce the controllability of luminescent spectrum, thus have impact on the color rendition index of white LED light source, this is also the bottleneck run in current LED light source development process.In order to address this problem, invent a kind of fluorescent material that can be used for packaged LED newly and just seeming particularly important.
Relative to the fluorescent material of rare earth class, semi-conductor nano particles is owing to having quantum size effect, thus unique size-dependent luminosity is demonstrated, and it has the advantages such as half-peak width, fluorescence quantum efficiency is high, good stability, wider absorption band and controllability are strong, becomes a focus in investigation of materials field gradually.Along with the development of nanotechnology, the material of various based semiconductor nanoparticle is constantly developed by people, and this is also for the packaged material of LED opens a kind of new situation.
Summary of the invention
Object of the present invention is just to provide a kind of easy and simple to handle and more energy-conservation one dimension self-assembled material based on aqueous-phase semiconductor nanoparticle, namely direct various reactant is carried out mixing rear room temperature under obtain the self-assembled material of hyperfluorescenceZeng Yongminggaoyingguang, be then applied to prepare in the white LED light source of high-color rendering.
The present invention utilizes colloid chemistry method, in aqueous by directly various reaction raw materials being mixed, then the ratio between all ingredients is regulated, it just can be made at room temperature to obtain a kind of self-assembled material of based semiconductor nanoparticle, this material has very high fluorescence quantum efficiency, adjustable fluorescence color, well stability, and can be applied in the packaged material of LED, as color conversion layer.Meanwhile, by regulating the ratio with the self-assembled material of different fluorescence color added, the white LED light source of high-color rendering, high brightness, adjustable color can be produced.
The raw material that the present invention adopts is all the commercial inorganic salt that can have directly bought, do not need further process, directly mix according to a certain percentage, therefore experimental implementation is easy, dangerous little, and have good experimental repeatability, the self-assembled material obtained has very high fluorescence quantum efficiency simultaneously.The LED light source adopted is the commercial naked paster of blue-ray LED 5050 do not encapsulated.
Above-mentioned water-soluble II-VI group nanoparticle synthesis is raw materials used is cadmium salt, mercury salt, tellurium source, selenium source or sulphur source, sulfydryl small molecules, sodium hydroxide, sodium borohydride, ammoniac compounds.Cadmium salt can be CdCl 2, Cd (ClO 4) 2deng; Mercury salt can be HgCl 2, Hg (NO 3) 2deng; Tellurium source is Te powder, Na 2teO 3deng; Selenium source is Se powder, Na 2seO 3deng; Sulphur source is Na 2s; Sulfydryl small molecules can be thiohydracrylic acid, Thiovanic acid; Ammoniac compounds is N 2h 4h 2o.In packaged LED process, need the prepolymer adopting polydimethylsiloxane.
Specifically, the one dimension self-assembled material based on aqueous-phase semiconductor nanoparticle of the present invention, it is preparation one of by the following method:
First method, at room temperature opens wide in system and adds cadmium salt, by water dissolution, then add sulfydryl small molecules, ionic tellurium source (Na 2teO 3) or ionic selenium source (Na 2seO 3), then add NaBH 4, after ambient temperatare puts 48 ~ 60 hours, namely obtain nucleation aqueous phase CdTe nanoparticle precursor solution completely; Finally add the ammoniac compounds solution that concentration is 80wt% ~ 99wt% again, after ambient temperatare puts 15 ~ 20 hours, the self-assembled material based on CdTe semi-conductor nano particles can be obtained at container bottom.In reaction system, the concentration of cadmium salt is 1.0 × 10 -3~ 1.5 × 10 -2mol/L, cadmium salt, ionic tellurium source or ionic selenium source, sulfydryl small molecules, NaBH 4, ammoniac compounds mol ratio be 1:0.1 ~ 0.8:1.5 ~ 2.4:1 ~ 10.5:600 ~ 1200.
Second method, at room temperature opens wide in system and adds cadmium salt and mercury salt, by water dissolution, then add sulfydryl small molecules, and be 9 ~ 10 with NaOH regulator solution pH, then add NaHTe (by Te powder and NaBH 4reaction is obtained), NaHSe is (by Se powder and NaBH 4reaction is obtained), Na 2s or NaHSe xte 1-x(by mixture and the NaBH of Te powder and Se powder 4reaction is obtained, wherein 0<x<1), after ambient temperatare puts 8 ~ 15 hours, namely obtain nucleation aqueous phase CdTe, CdSe, CdS, CdSe completely xte 1-x, CdHgTe, CdHgSe, CdHgS or CdHgSe xte 1-xnanoparticle precursor solution, obtains finally by controlling heat-up time CdTe, CdSe, CdS, CdSe of launching different fluorescence color xte 1-x, CdHgTe, CdHgSe, CdHgS or CdHgSe xte 1-xnanoparticle; The concentration of cadmium salt is 1.0 × 10 -3~ 1.5 × 10 -2mol/L; Cadmium salt, mercury salt, NaHTe, NaHSe, Na 2s or NaHSe xte 1-x, the mol ratio of sulfydryl small molecules four kinds of materials is 1:0 ~ 2:0.1 ~ 0.8:1.5 ~ 2.4;
Cadmium salt is added in another unlimited system, then water dissolution is used, add the ammoniac compounds solution that sulfydryl small molecules and concentration are 80wt% ~ 99wt% again, after 2 ~ 3 hours, add the semi-conductor nano particles that above-mentioned steps prepares, after 30 ~ 45 minutes, the self-assembled material based on aqueous-phase semiconductor nanoparticle can be obtained at container bottom; The concentration of cadmium salt is 1.0 × 10 -3~ 1.5 × 10 -2mol/L, the mol ratio of cadmium salt, sulfydryl small molecules, ammoniac compounds, semi-conductor nano particles is 1:1 ~ 1.7:600 ~ 1200:0.5 ~ 0.01.
After the self-assembled material that reactor bottom obtains based on various semi-conductor nano particles, through centrifugal, collect the self-assembled material bottom centrifuge tube, at 60 ~ 80 DEG C after drying, be ground into powder, and blended with the prepolymer of polydimethylsiloxane, then be coated on the LED that do not encapsulate, be positioned in 80 ~ 95 DEG C of baking ovens again, after 3 ~ 5 hours, namely obtain packaged LED light source.In reaction system, the prepolymer of polydimethylsiloxane and the mass ratio of self-assembled material are 18:1 ~ 2.
Accompanying drawing explanation
Fig. 1: the fluorescent microscopy images (a) with the self-assembled material of green fluorescence prepared by the CdTe nanoparticle utilizing thiohydracrylic acid stable, utilize the LED light source (b) that the self-assembled material with green fluorescence is green glow as luminescence prepared by packaged material, CIE coordinate (c) of LED light source, its CIE coordinate is (0.22,0.69), illustrate and utilize this self-assembled material can obtain the LED light source that utilizing emitted light is green glow;
Fig. 2: the fluorescent microscopy images (a) with the self-assembled material of orange-yellow fluorescence prepared by the CdTe nanoparticle utilizing thiohydracrylic acid stable, utilize the LED light source (b) that the self-assembled material with orange-yellow fluorescence is gold-tinted as luminescence prepared by packaged material, CIE coordinate (c) of LED light source, its CIE coordinate is (0.54,0.44), illustrate and utilize this self-assembled material can obtain the LED light source that utilizing emitted light is gold-tinted;
Fig. 3: the fluorescent microscopy images (a) with the self-assembled material of red fluorescence prepared by the CdTe nanoparticle utilizing thiohydracrylic acid stable, utilize the LED light source (b) that the self-assembled material with red fluorescence is gold-tinted as luminescence prepared by packaged material, CIE coordinate (c) of LED light source, its CIE coordinate is (0.53,0.29), illustrate and utilize this self-assembled material can obtain the LED light source that utilizing emitted light is ruddiness;
Fig. 4: the fluorescent microscopy images (a) with the self-assembled material of yellow fluorescence prepared by the CdTe nanoparticle utilizing thiohydracrylic acid stable, utilize the LED light source (b) that the self-assembled material with yellow fluorescence is white light as luminescence prepared by packaged material, CIE coordinate (c) of LED light source, its CIE coordinate is (0.31,0.31), illustrate and utilize this self-assembled material can obtain the LED light source that utilizing emitted light is white light;
Fig. 5: the fluorescent microscopy images (a) with the self-assembled material of fluorescent orange prepared by the CdS nanoparticle utilizing thiohydracrylic acid stable, fluorescence spectrum (b) corresponding thereto and EDS power spectrum (c), fluorescence spectrum shows that self-assembled material maintains the luminosity of particle, and EDS power spectrum then proves in self-assembled material containing CdS nanoparticle;
Fig. 6: the fluorescent microscopy images (a) with the self-assembled material of yellow fluorescence prepared by the CdSe nanoparticle utilizing thiohydracrylic acid stable, fluorescence spectrum (b) corresponding thereto and EDS power spectrum (c), fluorescence spectrum shows that self-assembled material maintains the luminosity of particle, and EDS power spectrum then proves in self-assembled material containing CdSe nanoparticle;
Fig. 7: utilize the CdSe that thiohydracrylic acid is stable 0.25te 0.75the fluorescent microscopy images (a) of prepared by nanoparticle the have self-assembled material of red fluorescence, fluorescence spectrum (b) corresponding thereto and EDS power spectrum (c), fluorescence spectrum shows that self-assembled material maintains the luminosity of particle, and EDS power spectrum then proves in self-assembled material containing CdSe 0.25te 0.75nanoparticle;
Fig. 8: utilize the Cd that thiohydracrylic acid is stable 0.75hg 0.25the optical microscope photograph (a) of self-assembled material prepared by Te nanoparticle, fluorescence spectrum (b) corresponding thereto and EDS power spectrum (c), fluorescence spectrum shows that self-assembled material maintains the luminosity of particle, and EDS power spectrum then proves in self-assembled material containing Cd 0.75hg 0.25te nanoparticle;
Fig. 9: the optical microscope photograph (a) of self-assembled material prepared by the CdTe nanoparticle utilizing Thiovanic acid stable and fluorescent microscopy images (b);
Figure 10: utilize the LED light source (a) that the self-assembled material with various fluorescence color is white light as luminescence prepared by packaged material, the luminescent spectrum (b) of LED light source and its CIE coordinate (c), its CIE coordinate is (0.31,0.31), illustrate that the self-assembled material by mixing various fluorescence color can obtain the LED light source that utilizing emitted light is white light.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated, instead of will limit the invention with this.
Embodiment 1
8 × 10 are added in 80mL reaction system -4the CdCl of mol 2, 1.2 × 10 -3mol thiohydracrylic acid, 8 × 10 -5the Na of mol 2teO 3, 0.03g NaBH 4, after rocking a little and at room temperature place 48 hours, the concentration adding 30mL is the N of 80wt% 2h 4h 2o solution, after 15 hours, as shown in Fig. 1 (a), the fluorescence color under reactor bottom obtains self-separation is green one dimension self-assembled material.
Through centrifugal, collect the self-assembled material bottom centrifuge tube, pulverize after drying, get the self-assembled material that 11mg is ground, blended with the prepolymer of 100mg polydimethylsiloxane, be then coated on the LED that do not encapsulate, then be positioned in 80 DEG C of baking ovens, after 5 hours, namely obtain LED light source that packaged luminescence is green glow (Fig. 1 b and c).
Embodiment 2
8 × 10 are added in 80mL reaction system -4the CdCl of mol 2, 1.6 × 10 -3mol thiohydracrylic acid, 1.6 × 10 -4the Na of mol 2teO 3, 0.1g NaBH 4, after ambient temperatare puts 48 hours, the concentration adding 50mL is the N of 80wt% 2h 4h 2o solution, after room temperature places 20 hours, as shown in Fig. 2 (a), the fluorescence color under reactor bottom obtains self-separation is orange-yellow one dimension self-assembled material.Through centrifugal, collect the self-assembled material bottom centrifuge tube, pulverize after drying, get the self-assembled material that 6mg is ground, blended with the prepolymer of 100mg polydimethylsiloxane, be then coated on the LED that do not encapsulate, then be positioned in 80 DEG C of baking ovens, after 3 hours, namely obtain the LED light source (Fig. 2 b and Fig. 2 c) that packaged luminescence is gold-tinted.
Embodiment 3
8 × 10 are added in 80mL reaction system -4the CdCl of mol 2, 1.9 × 10 -3mol thiohydracrylic acid, 6.4 × 10 -4the Na of mol 2teO 3, 0.3g NaBH 4, after ambient temperatare puts 60 hours, the concentration adding 70mL is the N of 80wt% 2h 4h 2o solution, after room temperature places 20 hours, as shown in Fig. 3 (a), the fluorescence color under reactor bottom obtains self-separation is red one dimension self-assembled material.Through centrifugal, collect the self-assembled material bottom centrifuge tube, pulverize after drying, get the self-assembled material that 9mg is ground, blended with the prepolymer of 100mg polydimethylsiloxane, be then coated on the LED that do not encapsulate, then be positioned in 80 DEG C of baking ovens, after 5 hours, namely obtain the LED light source (Fig. 3 b and Fig. 3 c) that packaged luminescence is ruddiness.
Embodiment 4
8 × 10 are added in 80mL reaction system -4the CdCl of mol 2, 1.6 × 10 -3mol thiohydracrylic acid, 1.6 × 10 -4the Na of mol 2teO 3, 0.1g NaBH 4, after ambient temperatare puts 48 hours, the concentration adding 40mL is the N of 99wt% 2h 4h 2o solution, after room temperature places 15 hours, as shown in Fig. 4 (a), the fluorescence color under reactor bottom obtains self-separation is yellow one dimension self-assembled material.Through centrifugal, collect the self-assembled material bottom centrifuge tube, pulverize after drying, get the self-assembled material that 8mg is ground, blended with the prepolymer of 100mg polydimethylsiloxane, be then coated on the LED that do not encapsulate, then be positioned in 80 DEG C of baking ovens, after 3 hours, namely obtain the LED light source (Fig. 4 b and Fig. 4 c) that packaged luminescence is white light.
Embodiment 5
8 × 10 are added in 80mL reaction system -4the CdCl of mol 2, 1.2 × 10 -3mol thiohydracrylic acid, and be 9 ~ 10 with the NaOH regulation system pH of 1mol/L, then add 8 × 10 -5the Na of mol 2s, then carries out reflux to it, after two hours, obtains the CdS nanoparticle prepared.1 × 10 is added in another 20mL reaction system -4the CdCl of mol 2, 1 × 10 -4the concentration of mol thiohydracrylic acid, 4mL is the N of 80wt% 2h 4h 2o solution, after lucifuge under room temperature condition places 2 hours, adds the CdS nanoparticle that 2mL prepares.After 35 minutes, as shown in Fig. 5 (a-c), the fluorescence color under reactor bottom obtains self-separation is orange-yellow one dimension self-assembled material.
Embodiment 6
0.32g Se, 0.32g NaBH is added in 6mL reaction system 4, after 5 hours, sealed reaction system, obtains NaHSe solution.
Then in 80mL reaction system, 8 × 10 are added -4the CdCl of mol 2, 1.9 × 10 -3mol thiohydracrylic acid, and be 9 ~ 10 with the NaOH regulation system pH of 1mol/L, then add 6.4 × 10 -4the NaHSe of mol, then carries out reflux to it, after two hours, obtains the CdSe nanoparticle prepared.
1 × 10 is added in another 20mL reaction system -4the CdCl of mol 2, 1.7 × 10 -4the concentration of mol thiohydracrylic acid, 8mL is the N of 80wt% 2h 4h 2o solution, after lucifuge under room temperature condition places 2 hours, adds the CdSe nanoparticle that 0.1mL prepares.After 30 minutes, as shown in Fig. 6 (a-c), the fluorescence color under reactor bottom obtains self-separation is yellowish green one dimension self-assembled material.
Embodiment 7
0.08g Se, 0.38g Te, 0.34g NaBH is added in 6mL reaction system 4, after 5 hours, sealed reaction system, obtains NaHSe 0.25te 0.75solution.Then in 80mL reaction system, 8 × 10 are added -4the CdCl of mol 2, 1.6 × 10 -3mol thiohydracrylic acid, and be 9 ~ 10 with the NaOH regulation system pH of 1mol/L, then add 1.6 × 10 -4the NaHSe of mol 0.25te 0.75, then reflux is carried out to it, after two hours, obtains the CdSe prepared 0.25te 0.75nanoparticle.
1 × 10 is added in another 20mL reaction system -4the CdCl of mol 2, 1 × 10 -4the concentration of mol thiohydracrylic acid, 8mL is the N of 80wt% 2h 4h 2o solution, after lucifuge under room temperature condition places 3 hours, adds the CdSe that 1mL prepares 0.25te 0.75nanoparticle.After 45 minutes, as shown in Fig. 7 (a-c), the fluorescence color under reactor bottom obtains self-separation is red one dimension self-assembled material.
Embodiment 8
0.51g Te, 0.34g NaBH is added in 6mL reaction system 4, after 5 hours, sealed reaction system, obtains NaHTe solution.Then in 80mL reaction system, 6 × 10 are added -4the CdCl of mol 2, 2 × 10 -4the HgCl of mol 2, 1.6 × 10 -3mol thiohydracrylic acid, and be 9 ~ 10 with the NaOH regulation system pH of 1mol/L, then add 1.6 × 10 -4the NaHTe of mol, then carries out reflux to it, after two hours, obtains the Cd prepared 0.75hg 0.25te nanoparticle.
1 × 10 is added in another 20mL reaction system -4the CdCl of mol 2, 1.5 × 10 -4the concentration of mol thiohydracrylic acid, 6mL is the N of 80wt% 2h 4h 2o solution, after lucifuge under room temperature condition places 2 hours, adds the Cd that 1mL prepares 0.75hg 0.25te nanoparticle.After 30 minutes, as shown in Fig. 8 (a-c), the one dimension self-assembled material under reactor bottom obtains self-separation.
Embodiment 9
0.51g Te, 0.34g NaBH is added in 6mL reaction system 4, after 5 hours, sealed reaction system, obtains NaHTe solution.Then in 80mL reaction system, 8 × 10 are added -4the CdCl of mol 2, 1.6 × 10 -3mol Thiovanic acid, and be 9 ~ 10 with the NaOH regulation system pH of 1mol/L, then add 1.6 × 10 -4the NaHTe of mol, then carries out reflux to it, after 1 hour, and the CdTe nanoparticle that the Thiovanic acid obtaining preparing is coated.
1 × 10 is added in another 20mL reaction system -4the CdCl of mol 2, 1 × 10 -4the concentration of mol Thiovanic acid, 8mL is the N of 80wt% 2h 4h 2o solution, after lucifuge under room temperature condition places 2 hours, adds the CdTe nanoparticle that Thiovanic acid that 1mL prepares is coated.After 30 minutes, as Fig. 8 (a and b) shown in, the fluorescence color under reactor bottom obtains self-separation is yellow one dimension self-assembled material.
Embodiment 10
8 × 10 are added in 80mL reaction system -4the CdCl of mol 2, 1.6 × 10 -3mol thiohydracrylic acid, 1.6 × 10 -4the Na of mol 2teO 3, 0.1g NaBH 4, after ambient temperatare puts 60 hours, the concentration adding 20mL is the N of 80wt% 2h 4h 2o solution, after 15 hours, the fluorescence color under reactor bottom obtains self-separation is green one dimension self-assembled material.When being the N of 80wt% the concentration of 20mL 2h 4h 2o solution changes into 40,50,60,80, the concentration of 100mL is the N of 80wt% 2h 4h 2during O solution, can obtain that fluorescence color is respectively yellow, orange, reddish orange, redness, wine-colored one dimension self-assembled material.
Then through centrifugal, collect the self-assembled material bottom centrifuge tube, pulverize after drying.Next the self-assembled material of various fluorescence color is carried out blended, get 11mg mixing material, blended with the prepolymer of 100mg polydimethylsiloxane, then be coated on the LED that do not encapsulate, be positioned in 80 DEG C of baking ovens again, after 5 hours, namely obtain the high-color rendering LED light source (Figure 10 a-c) that packaged luminescence is white light.In mixing material, the mass ratio of green, yellow, orange, reddish orange, redness, wine-colored one dimension self-assembled material is 3:1:0.8:0.5:0.5:0.5.

Claims (5)

1. based on a preparation method for the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, it is characterized in that: at room temperature open wide in system and add cadmium salt, by water dissolution, then add sulfydryl small molecules, ionic tellurium source, then add NaBH 4, after ambient temperatare puts 48 ~ 60 hours, namely obtain nucleation aqueous phase CdTe nanoparticle precursor solution completely; Finally add the ammoniac compounds solution that concentration is 80wt% ~ 99wt% again, after ambient temperatare puts 15 ~ 20 hours, the self-assembled material based on CdTe semi-conductor nano particles can be obtained at container bottom; In above-mentioned reaction system, the concentration of cadmium salt is 1.0 × 10 -3~ 1.5 × 10 -2mol/L, cadmium salt, ionic tellurium source, sulfydryl small molecules, NaBH 4, ammoniac compounds mol ratio be 1:0.1 ~ 0.8:1.5 ~ 2.4:1 ~ 10.5:600 ~ 1200.
2., based on a preparation method for the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, its step is as follows:
(1) at room temperature open wide in system and add cadmium salt and mercury salt, by water dissolution, then add sulfydryl small molecules, and be 9 ~ 10 with NaOH regulator solution pH, then add NaHTe, NaHSe, Na 2s or NaHSe xte 1-x, wherein 0<x<1, after ambient temperatare puts 8 ~ 15 hours, namely obtains nucleation aqueous phase CdTe, CdSe, CdS, CdSe completely xte 1-x, CdHgTe, CdHgSe, CdHgS or CdHgSe xte 1-xnanoparticle precursor solution, obtains finally by controlling heat-up time CdTe, CdSe, CdS, CdSe of launching different fluorescence color xte 1-x, CdHgTe, CdHgSe, CdHgS or CdHgSe xte 1-xnanoparticle; The concentration of cadmium salt is 1.0 × 10 -3~ 1.5 × 10 -2mol/L; Cadmium salt, mercury salt, NaHTe, NaHSe, Na 2s or NaHSe xte 1-x, the mol ratio of sulfydryl small molecules four kinds of materials is 1:0 ~ 2:0.1 ~ 0.8:1.5 ~ 2.4;
(2) in another unlimited system, cadmium salt is added, then water dissolution is used, add the ammoniac compounds solution that sulfydryl small molecules and concentration are 80wt% ~ 99wt% again, after 2 ~ 3 hours, add the semi-conductor nano particles that above-mentioned steps prepares, after 30 ~ 45 minutes, the self-assembled material based on aqueous-phase semiconductor nanoparticle can be obtained at container bottom; The concentration of cadmium salt is 1.0 × 10 -3~ 1.5 × 10 -2mol/L, the mol ratio of cadmium salt, sulfydryl small molecules, ammoniac compounds, semi-conductor nano particles is 1:1 ~ 1.7:600 ~ 1200:0.5 ~ 0.01.
3. the preparation method of a kind of one dimension self-assembled material based on aqueous-phase semiconductor nanoparticle as claimed in claim 1 or 2, is characterized in that: cadmium salt is CdCl 2or Cd (ClO 4) 2; Mercury salt is HgCl 2or Hg (NO 3) 2; Ionic tellurium source is Na 2teO 3; Ionic selenium source is Na 2seO 3; Sulphur source is Na 2s; Sulfydryl small molecules is thiohydracrylic acid or Thiovanic acid; Ammoniac compounds is N 2h 4h 2o.
4. based on an one dimension self-assembled material for aqueous-phase semiconductor nanoparticle, it is characterized in that: prepared by the method for claim 1 or 2.
5. the application of one dimension self-assembled material in LED based on aqueous-phase semiconductor nanoparticle according to claim 4.
CN201410216614.3A 2014-05-21 2014-05-21 Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED Expired - Fee Related CN103965912B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410216614.3A CN103965912B (en) 2014-05-21 2014-05-21 Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410216614.3A CN103965912B (en) 2014-05-21 2014-05-21 Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED

Publications (2)

Publication Number Publication Date
CN103965912A CN103965912A (en) 2014-08-06
CN103965912B true CN103965912B (en) 2015-09-09

Family

ID=51235926

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410216614.3A Expired - Fee Related CN103965912B (en) 2014-05-21 2014-05-21 Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED

Country Status (1)

Country Link
CN (1) CN103965912B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105131807B (en) * 2015-10-13 2017-10-20 厦门大学 A kind of hydrophobic aqueous fluorescent polyurethane coating and preparation method thereof
CN105131806B (en) * 2015-10-13 2018-06-26 厦门大学 Aqueous fluorescent polyurethane coating and its prepolymer blend method preparation method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649484A (en) * 2009-09-09 2010-02-17 吉林大学 Method for preparing aqueous-phase semiconductor nanocrystalline by using ammonia compound for catalysis
CN102694110A (en) * 2012-06-08 2012-09-26 北京理工大学 Non-rare earth nanocrystalline fluorescent powder-containing packaging material, preparation method and application
CN103194237A (en) * 2013-04-22 2013-07-10 吉林大学 Self-separating method of aqueous-phase semiconductor nanocrystalline under room temperature

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649484A (en) * 2009-09-09 2010-02-17 吉林大学 Method for preparing aqueous-phase semiconductor nanocrystalline by using ammonia compound for catalysis
CN102694110A (en) * 2012-06-08 2012-09-26 北京理工大学 Non-rare earth nanocrystalline fluorescent powder-containing packaging material, preparation method and application
CN103194237A (en) * 2013-04-22 2013-07-10 吉林大学 Self-separating method of aqueous-phase semiconductor nanocrystalline under room temperature

Also Published As

Publication number Publication date
CN103965912A (en) 2014-08-06

Similar Documents

Publication Publication Date Title
Guan et al. Room temperature synthesis of stable single silica-coated CsPbBr3 quantum dots combining tunable red emission of Ag–In–Zn–S for High-CRI white light-emitting diodes
CN106025042B (en) Stable white light LED and preparation method based on coated with silica perovskite quantum dot
Otto et al. Colloidal nanocrystals embedded in macrocrystals: Robustness, photostability, and color purity
Ziegler et al. Silica-coated InP/ZnS nanocrystals as converter material in white LEDs
JP4366502B2 (en) Semiconductor ultrafine particle phosphor and light emitting device
KR100819337B1 (en) White LED structure using quantum dots and the manufacturing method thereof
CN103597622A (en) Semiconductor nanoparticle-based materials for use in light emitting diodes, optoelectronic displays and the like
US20190330527A1 (en) Light converting luminescent composite material
CN103773364B (en) Preparation method of bicolor fluorescent semiconductor nanomaterial based on Mn-doped CuInS2/ZnS
WO2007034877A1 (en) Semiconductor nanoparticles dispersed glass fine particles and process for preparing the same
Chang et al. A water–ethanol phase assisted co-precipitation approach toward high quality quantum dot–inorganic salt composites and their application for WLEDs
CN101580628A (en) Quantum dot luminescence transparent casting glue composite material
CN104310784A (en) Quantum dot LED light emitting glass and preparation method thereof
CN104830324B (en) A kind of preparation method of pair of light emission doped transition metal ions semiconductor-quantum-point
CN113072928B (en) Preparation method of zero-dimensional manganese-based metal halide ultra-fast self-assembly
CN105733575A (en) Tetravalent manganese ion doped ammonium salt red light material and preparation method thereof
CN110129055A (en) The preparation of CdSeZnS/ZnS/ZnS core shell/shell quantum dot
CN107394014B (en) A kind of preparation method of LED quantum dot coating fluid
JP3755033B2 (en) Silica-based glass particle material and device containing ultrafine semiconductor particles
CN103965912B (en) Based on the one dimension self-assembled material of aqueous-phase semiconductor nanoparticle, preparation method and the application in LED
CN114181104B (en) N-acetyl ethylenediamine metal halide low-dimensional perovskite single crystal material, preparation method and application thereof
CN105226146A (en) Liquid quantum dot LED and preparation method thereof
Zhang et al. High luminescent aqueous CdZnTe QDs incorporated in CaCO3 for excellent color-rendering WLEDs
CN105674144A (en) Full spectrum LED (Light Emitting Diode) ecological light source with 660 nanometer red light character emission
CN110093159B (en) Preparation of single-component CsPb (Cl/Br)3 white-light quantum dot with zero-dimensional Mn-doped core-shell structure

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20150909

Termination date: 20180521

CF01 Termination of patent right due to non-payment of annual fee