CN113831919B - Based on Bi doped Ag 2 Ultra-wideband short-wave infrared LED of Se quantum dot and preparation method and application thereof - Google Patents
Based on Bi doped Ag 2 Ultra-wideband short-wave infrared LED of Se quantum dot and preparation method and application thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
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Abstract
The invention relates to the technical field of photoelectricity, in particular to a Bi-based Ag doped material 2 An ultra-wideband short-wave infrared LED of Se quantum dots and a preparation method and application thereof are as follows: adding selenium powder into the organic phosphine ligand solution to obtain a selenium precursor solution; heating the silver-containing compound, the metal ligand and the non-coordinating solvent to raise the temperature, adding the selenium precursor solution, and reacting to obtain Ag 2 Se quantum dots; dissolving a bismuth-containing compound in a polar solvent, and heating to obtain a Bi precursor solution; mixing Ag with water 2 Heating Se quantum dot and bismuth precursor solution to react to obtain Bi-doped Ag 2 Se quantum dots; doping Bi with Ag 2 And packaging the Se quantum dots to obtain the photoinduced conversion type ultra wide band short wave infrared LED. The invention makes Ag by doping bismuth ions 2 Red shift of Se emission band and strengthening of Ag 2 The Se quantum dots emit light in 1400-1700nm band, so that the light emission of the Se quantum dots in the SWIR full-band ultra-wide band is realized, the ultra-wide band tunable photoinduced conversion type short-wave infrared LED is prepared by combining with the blue light LED chip, and the light-emitting diode has wide application prospect in short-wave infrared spectroscopy.
Description
Technical Field
The invention relates to the technical field of photoelectricity, in particular to a Bi-based Ag doped material 2 An ultra-wideband short-wave infrared LED of Se quantum dots, a preparation method and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The short wave infrared (SWIR, 900-1700 nm) spectrum technology has wide application in food safety analysis, noninvasive health detection, crop and environment detection and other aspects. Biological components such as water, protein, lipid, etc. have strong absorption in SWIR band, and C-H, N-H and O-H bonds present specific in SWIR regionMolecular vibrations, contaminant particles such as dust and smoke, etc. have a high ability to penetrate light in the SWIR band. Taking advantage of these advantages, short-wave infrared light sources enable rapid, sensitive and non-invasive detection of different types of compounds in the above-mentioned applications. The existing SWIR light sources in the market, such as tungsten filament incandescent lamps and halogen lamps, have large volume, are easy to generate heat and have high power consumption, so that the practical application of the SWIR light sources is limited. The light-induced conversion type SWIR light source is a small-sized integrated portable light source obtained by combining a blue light LED or a near ultraviolet LED with a luminescent material with an emission wavelength positioned in the SWIR. The SWIR luminescent materials reported at present mainly include transition metal ion activated materials and rare earth ion doped materials. Cr (chromium) component 3+ 、Mn 4+ 、Ni 2+ The emission peak position of the transition metal ions is usually below 900nm, and the red shift of the emission peak position to above 1000nm is difficult to realize by regulating and controlling the electron energy level. Despite rare earth ions, e.g. Yb 3+ ，Er 3+ ，Nd 3+ And Pr 3+ The emission wavelength of the doped material is above 1000nm, but the emission full width at half maximum of the rare earth ions is generally less than 40nm because the 4f electron layer of the rare earth ions is shielded by 5s and 5p shell electrons. In order to expand the detection range and obtain more compound information in the SWIR spectrum application, a novel ultra-wideband SWIR luminescent material needs to be invented and matched with a blue light chip to prepare a small-sized integrated ultra-wideband short-wave infrared LED light source.
The radius of the semiconductor quantum dot is close to or smaller than the exciton Bohr radius (5-20 nm), and as the size is reduced, the energy level is split violently, the forbidden bandwidth is increased, so that the emission wavelength can be regulated and controlled by regulating the size of the quantum dot. In previous studies, ag 2 The emission peak position of the Se quantum dot can be regulated and controlled from 1080nm to 1330nm, the full width at half maximum is usually 200nm, but the SWIR full-wave band is difficult to realize, and particularly, the strong luminescence at 1400-1700nm is realized. The invention makes Ag by doping bismuth ions 2 Red shift of Se emission band and strengthening of Ag 2 The Se quantum dots emit light in 1400-1700nm band to realize the light emission in SWIR full-band ultra-wideband, and the ultra-wideband tunable photoinduced conversion type short-wave infrared LED is prepared by combining with a blue light LED chip, and has wide application prospect in short-wave infrared spectroscopy。
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a Bi-based Ag doping material 2 The preparation method and application of the ultra-wideband photoinduced conversion type short-wave infrared LED of the Se quantum dots can be realized by changing the preparation of Bi doped with Ag 2 The time and the temperature of the Se quantum dots control the LED packaging conditions, the LED short wave infrared SWIR full-wave-band adjustable luminescence is realized, the preparation conditions are mild, the cost is low, and the mass production is facilitated.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in a first aspect of the invention, a Bi-based doped Ag is provided 2 The preparation method of the ultra-wideband short-wave infrared LED of the Se quantum dot comprises the following steps:
(1) Adding selenium powder into the organic phosphine ligand solution to obtain a selenium precursor solution; heating a silver-containing compound, a metal ligand and a non-coordinating solvent, adding a selenium precursor solution, and reacting to obtain Ag 2 Se quantum dots;
(2) Dissolving a bismuth-containing compound in a polar solvent, and heating for reaction to obtain a Bi precursor solution; mixing Ag with water 2 Se quantum dots react with a certain amount of bismuth precursor solution under heating to obtain Bi doped Ag 2 Se quantum dots;
(3) Uniformly mixing epoxy resin and a curing agent to obtain a mixed glue;
(4) Doping the Bi obtained in the step (2) with Ag 2 Uniformly mixing the Se quantum dots with the mixed glue obtained in the step (3) to obtain a powder glue mixture;
(5) And (4) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing.
In a second aspect of the present invention, there is provided a Bi-doped Ag-based alloy of the first aspect 2 Bi-doped Ag-based ultra-wideband short-wave infrared LED prepared by preparation method of Se quantum dot 2 And the Se quantum dot ultra-wideband short-wave infrared LED.
In a third aspect of the present invention, there is provided the Bi-based doped Ag of the second aspect 2 Ultra-wideband short-wave infrared LED (light-emitting diode) with Se quantum dots for food safetyAnalysis, noninvasive health detection, crop and environment detection and the like.
The specific embodiment of the invention has the following beneficial effects:
(1) Compared with the existing light source, the Bi-based doped Ag prepared by the specific embodiment of the invention 2 The ultra-wideband photoinduced conversion type short-wave infrared LED of the Se quantum dot solves the bottleneck that the existing near-infrared LED is only limited to I-region luminescence, and widens the luminescence range of the LED to the full-wave range of short-wave infrared.
Bi-doped Ag-based material prepared by specific embodiment of the invention 2 The ultra-wide band photoinduced conversion type short wave infrared LED of the Se quantum dot can realize tunable short wave infrared adjustable light emission of 900-1700nm ultra-wide band;
(2) The invention adopts the photoluminescence principle to prepare the light-induced conversion type LED, and compared with the traditional electroluminescent LED, the packaging steps are simple and convenient for actual operation;
(3) The photoinduced conversion type LED prepared by the invention has the advantage that the GaN blue light chip directly excites the Bi doped Ag 2 The Se quantum dots emit ultra-wide band short wave infrared fluorescence without doping fluorescent powder, so that the preparation cost of the LED is reduced, and the luminous efficiency of the LED is enhanced.
(4) The traditional short-wave infrared spectrometer is generally large in size and not easy to carry, and the problems of large electric power consumption, low spectrum intensity and the like exist in commercial short-wave infrared;
(5) The short-wave infrared quantum dots mostly contain heavy metal elements such as Pb, cd, hg and the like, and have the problem of safe use; the invention selects green low-toxicity Ag 2 Se quantum dots are used as luminescent materials, and are favorable for better application of devices in the field of biomedicine.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 shows the Bi-doped Ag-based material of the present invention 2 Ultra-wideband photoinduced conversion of Se quantum dotsA preparation method and an application device diagram of a short-wave infrared LED,
wherein, FIG. 1a shows Bi-doped Ag according to example 1 of the present invention 2 An ultra-wideband photoinduced conversion type short-wave infrared LED device diagram of Se quantum dots;
FIG. 1b shows the tandem emission of the LED prepared in example 1 of the present invention;
FIG. 1c shows the tandem emission of the LED prepared in example 1 when a 590nm filter is added.
FIG. 2 shows Bi-doped Ag-based alloy prepared in example 1 of the present invention 2 Low power transmission electron microscope photograph of Se quantum dots.
FIG. 3 shows Bi-doped Ag prepared in example 1 of the present invention 2 The X-ray photoelectron spectrum of Se quantum dot,
wherein, FIG. 3a shows Bi doped Ag in example 1 of the present invention 2 X-ray photoelectron spectroscopy of Se quantum dots;
FIG. 3b shows Bi doped Ag in example 1 of the present invention 2 Ag 3d high resolution X-ray photoelectron spectroscopy of Se quantum dots;
FIG. 3c shows Bi doped Ag in example 1 of the present invention 2 Se 3d high resolution X-ray photoelectron spectrum of Se quantum dots;
FIG. 3d shows Bi doped Ag according to example 1 of the present invention 2 Bi 4f high resolution X-ray photoelectron spectrum of Se quantum dots.
FIG. 4 Bi-based doped Ag prepared according to example 1 of the present invention with different Bi-doping ratios 2 Emission spectrum of Se quantum dots.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In one embodiment of the invention, a Bi-based doped Ag is provided 2 The preparation method of the ultra-wideband short-wave infrared LED of the Se quantum dot comprises the following steps:
(1) Adding selenium powder into the organic phosphine ligand solution to obtain a selenium precursor solution; heating a silver-containing compound, a metal ligand and a non-coordinating solvent, adding a selenium precursor solution, and reacting to obtain Ag 2 Se quantum dots;
(2) Dissolving a bismuth-containing compound in a polar solvent, and heating for reaction to obtain a Bi precursor solution; mixing Ag 2 Se quantum dots and a certain amount of bismuth precursor solution are heated to react to obtain Bi doped Ag 2 Se quantum dots;
(3) Uniformly mixing epoxy resin and a curing agent;
(4) Doping the Bi obtained in the step (2) with Ag 2 Uniformly mixing the Se quantum dots with the mixed glue obtained in the step (3) to obtain a powder glue mixture;
(5) And (4) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing.
In a specific embodiment, the organic phosphine ligand solution in the step (1) is one selected from tri-n-octyl phosphine oxide, tributylphosphine, trihexyl phosphine oxide or tetradecyl phosphoric acid;
in a specific embodiment, the silver-containing compound in step (1) is selected from one of silver nitrate, silver acetate or silver diethyldithiocarbamate;
in a specific embodiment, the metal ligand in step (1) is selected from an alkyl thiol or an alkyl dithiol; the metal ligand and the silver ion center form a stable complex, and the ratio of the metal ligand to the metal center influences the structure of the complex;
in a specific embodiment, the non-coordinating solvent in step (1) is one selected from octadecene, oleylamine or liquid paraffin; the non-coordinating solvent is green and safe, and can provide a stable reaction environment;
in a specific embodiment, the bismuth-containing compound in step (2) is one selected from bismuth acetate, bismuth oxide, bismuth oxalate, bismuth nitrate or bismuth chloride;
in a specific embodiment, the selenium powder in the step (1) is added with the organic phosphine ligand solution to react at room temperature, the room temperature reaction time is 0.5-2 h, the heating reaction temperature is 150-200 ℃, and the reaction time is 30-90 min.
In a specific embodiment, the ratio of Ag: the molar ratio of Se is 3:1 to 5:1.
in a specific embodiment, the molar content of Bi in the step (2) is 0.15-15% of the molar content of Ag.
In a specific embodiment, the heating reaction temperature in the step (2) is 20-40 ℃, and the reaction time is 20-60 min.
In a specific embodiment, the heating reaction in step (1) and step (2) is completed and further comprises the steps of washing and drying;
preferably, the washing is carried out by acetone, and the drying temperature is 60 ℃;
in a particular embodiment, both step (1) and step (2) should be carried out in a strictly oxygen-free and water-free inert gas atmosphere,
preferably, the inert gas atmosphere is one of a nitrogen atmosphere and an argon atmosphere;
in a specific embodiment, the mass ratio of the epoxy resin to the curing agent in the step (3) is 2;
preferably, the curing agent is a curing type organic silicon rubber material, and has good cohesiveness, ultraviolet resistance and high temperature resistance;
in a specific embodiment, in the step (4), bi is doped with Ag 2 The mass ratio of the Se quantum dots to the mixed glue is 1;
preferably, the mixed glue can be replaced by polymethyl methacrylate (PMMA) and Bi is doped with Ag 2 The mass ratio of the Se quantum dots to the PMMA is 1.
In a specific embodiment, after the step (2) and the step (3) are uniformly mixed, the method further comprises the step of vacuumizing to remove bubbles.
In a specific embodiment, the chip in the step (5) is positioned at the center of the LED chip;
preferably, the size of the LED chip is 7.3mm multiplied by 7.3mm;
preferably, the LED chip is a purple light chip or a blue light chip, and the peak wavelength is 395nm or 460nm respectively.
In a specific embodiment, the drying and curing temperature of the LED in the step (5) is 80-180 ℃;
in one embodiment of the present invention, there is provided a method for preparing the Bi-based doped Ag 2 And the Se quantum dot ultra-wideband short-wave infrared LED.
In one embodiment of the present invention, there is provided a method for preparing the Bi-based doped Ag 2 The application of the ultra-wideband short-wave infrared LED of the Se quantum dot in food safety analysis, noninvasive health detection, crop and environment detection and the like.
The invention will be further explained and illustrated with reference to specific examples.
Example 1
Firstly, 0.005mol of selenium powder is added into 5ml of trioctylphosphates, and the solution is clarified at room temperature to obtain selenium precursor solution. Adding 0.002mol of silver acetate, 20ml of dodecyl mercaptan and 10ml of octadecene into a three-necked flask, heating to 185 ℃, simultaneously adding 0.3ml of selenium precursor solution, and reacting for 60min to obtain Ag 2 Se quantum dots; dissolving 0.3mmol of bismuth acetate in 20ml of methanol, and heating for reaction for a period of time to obtain a Bi precursor solution; adding 0.04mmol of Ag 2 Se quantum dots are dissolved in 30ml of toluene, a ml of bismuth precursor solution is added, and the mixture reacts for 1h at the temperature of 20 ℃ to obtain Bi doped Ag 2 Se quantum dots; according to the formula of the ring illumination oxygen resin: curing agent =1:1, uniformly mixing in proportion; according to Ag 2 Se quantum dots: mixed glue =1:3, uniformly mixing to obtain a powder-glue mixture; and (3) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing at 100 ℃.
Wherein, a ml of bismuth precursor solution is added,
(1) The molar content of Bi is 0 percent of the molar content of Ag, and corresponds to a =0;
(2) The molar content of Bi accounts for 1.0 percent of the molar content of Ag, and corresponds to a =0.53ml;
(3) The molar content of Bi is 2.5 percent of the molar content of Ag, which corresponds to a =1.33ml;
(4) The molar content of Bi accounts for 5.0 percent of the molar content of Ag, and corresponds to a =2.67ml;
(5) The molar content of Bi was 10.0% of the molar content of Ag, corresponding to a =5.33ml.
FIG. 1a shows the Bi-based doped Ag prepared in this example 2 The light-induced conversion type ultra-wideband short-wave infrared LED device diagram of the Se quantum dots has the advantages that the size of an LED is 7.3mm multiplied by 7.3mm, the size is small, the carrying is convenient, and the practical application is facilitated; fig. 1b shows that when the serial LED prepared in this embodiment is powered by 6.48V, the LED chip emits blue fluorescence; FIG. 1b shows the light emission of the series LED (with a 590nm filter applied) prepared in this embodiment when a working voltage of 6.48V is applied, the applied filter can filter blue fluorescence, and red fluorescence is the short-wave infrared emission of the LED.
FIG. 2 shows the Bi-doped Ag prepared in this example 2 The Se quantum dots are spherical in low-power transmission electron microscope photos, good in dispersity and uniform in size.
FIG. 3 shows the Bi-doped Ag prepared in this example 2 The X-ray diffraction pattern of Se quantum dots does not obviously change Ag after Bi ions are doped 2 Se lattice structure.
FIG. 4 shows different concentrations of Bi-doped Ag prepared in this example 2 The fluorescence emission spectrum of the Se quantum dots is red-shifted in emission peak position after doping Bi ions, and the full width at half maximum is widened.
Example 2
Firstly, 0.005mol of selenium powder is added into 5ml of trioctylphosphate, and the solution is clarified at room temperature to obtain selenium precursor solution. Adding 0.002mol of silver acetate, 20ml of dodecyl mercaptan and 10ml of octadecene into a three-necked flask, heating to 185 ℃, simultaneously adding 0.3ml of selenium precursor solution, and reacting for 60min to obtain Ag 2 Amount of SeSub-points; dissolving 0.3mmol of bismuth acetate in 20ml of methanol, and heating for reaction for a period of time to obtain a Bi precursor solution; adding 0.04mmol of Ag 2 Se quantum dots are dissolved in 30ml of toluene, 1.33ml of bismuth precursor solution is added, and the mixture is heated to b ℃ for reaction for 60min to obtain Bi-doped Ag 2 Se quantum dots; according to the formula of the ring illumination oxygen resin: curing agent =1:1, mixing uniformly; according to Ag 2 Se quantum dots: mixed glue =1:3, uniformly mixing to obtain a powder-gel mixture; and (3) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing at 100 ℃.
Wherein the reaction temperature is b ℃ when doping Bi element,
(1) The reaction temperature was 20 ℃, corresponding to b =20 ℃;
(2) The reaction temperature was 30 ℃, corresponding to b =30 ℃;
(3) The reaction temperature was 40 ℃, corresponding to b =40 ℃.
Example 3
Firstly, 0.005mol of selenium powder is added into 5ml of trioctylphosphate, and the solution is clarified at room temperature to obtain selenium precursor solution. Adding 0.002mol of silver acetate, 20ml of dodecyl mercaptan and 10ml of octadecene into a three-necked flask, heating to 185 ℃, simultaneously adding 0.3ml of selenium precursor solution, and reacting for 60min to obtain Ag 2 Se quantum dots; dissolving 0.3mmol of bismuth acetate in 20ml of methanol, and heating for reaction for a period of time to obtain a Bi precursor solution; adding 0.04mmol of Ag 2 Se quantum dots are dissolved in 30ml of toluene, 1.33ml of bismuth precursor solution is added, the mixture is heated to 20 ℃ to react for c min, and Bi doped Ag is obtained 2 Se quantum dots; according to the formula of epoxy resin: curing agent =1:1, mixing uniformly; according to Ag 2 Se quantum dots: mixed glue =1:3, uniformly mixing to obtain a powder-glue mixture; and (3) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing at 100 ℃.
Wherein the reaction time is c min when doping Bi element,
(1) Reaction time was 20min, corresponding to c =20;
(2) Reaction time was 40min, corresponding to c =40;
(3) The reaction time was 60min, corresponding to c =60.
Example 4
Firstly, 0.005mol of selenium powder is added into 5ml of trioctylphosphate, and the solution is clarified at room temperature to obtain selenium precursor solution. Adding 0.002mol of silver acetate, 20ml of dodecyl mercaptan and 10ml of octadecene into a three-necked flask, heating to 185 ℃, simultaneously adding 0.3ml of selenium precursor solution, and reacting for 60min to obtain Ag 2 Se quantum dots; dissolving 0.3mmol of bismuth acetate in 20ml of methanol, and heating for reaction for a period of time to obtain a Bi precursor solution; adding 0.04mmol of Ag 2 Se quantum dots are dissolved in 30ml of toluene, 1.33ml of bismuth precursor solution is added, and the mixture is heated to 20 ℃ to react for 40min to obtain Bi doped Ag 2 And (4) Se quantum dots. According to the formula of epoxy resin: curing agent = m: n is mixed evenly; according to Ag 2 Se quantum dots: mixed glue =1:3, uniformly mixing to obtain a powder-gel mixture; and (4) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing at 100 ℃.
Wherein, the epoxy resin: the proportion of the curing agent is m to n,
(1) Epoxy resin: curing agent =2: n =2 for m: 1;
(2) Epoxy resin: curing agent =1:1, corresponding to m: n =1:1;
(3) Epoxy resin: curing agent =1:2, corresponding to m: n =1:2.
example 5
Firstly, adding 0.005mol of selenium powder into 5ml of trioctylphosphates, and clarifying the solution at room temperature to obtain a selenium precursor solution; adding 0.002mol of silver acetate, 20ml of dodecyl mercaptan and 10ml of octadecene into a three-necked flask, heating to 185 ℃, simultaneously adding 0.3ml of selenium precursor solution, and reacting for 60min to obtain Ag 2 Se quantum dots; dissolving 0.3mmol of bismuth acetate in 20ml of methanol, and heating for reaction for a period of time to obtain a Bi precursor solution; adding 0.04mmol of Ag 2 Se quantum dots are dissolved in 30ml of toluene, 1.33ml of bismuth precursor solution is added, and the mixture is heated to 20 ℃ to react for 40min to obtain Bi doped Ag 2 Se quantum dots; according to the formula of epoxy resin: curing agent =1:1, mixing uniformly; doping Ag according to Bi 2 Se quantum dots: mixed glue = s: t, uniformly mixing to obtain a powder-rubber mixture; dropping the powder-glue mixture on the chipAnd sealing the LED, and drying and curing at 100 ℃.
Wherein, the epoxy resin: the proportion of the curing agent is s to t,
(1)Ag 2 se quantum dots: mixed glue =1:3, corresponding to s: t =1:3;
(2)Ag 2 se quantum dots: mixed glue =1: t =1 for s: 4;
(3)Ag 2 se quantum dots: mixed glue =1: t =1 for s: 5;
(4)Ag 2 se quantum dots: mixed glue =1: t =1 for s: 6.
example 6
Firstly, adding 0.005mol of selenium powder into 5ml of trioctylphosphate, and clarifying the solution at room temperature to obtain a selenium precursor solution; adding 0.002mol of silver acetate, 20ml of dodecyl mercaptan and 10ml of octadecene into a three-necked flask, heating to 185 ℃, simultaneously adding 0.3ml of selenium precursor solution, and reacting for 60min to obtain Ag 2 Se quantum dots; dissolving 0.3mmol of bismuth acetate in 20ml of methanol, and heating for reaction for a period of time to obtain a Bi precursor solution; adding 0.04mmol of Ag 2 Se quantum dots are dissolved in 30ml of toluene, 1.33ml of bismuth precursor solution is added, and the mixture is heated to 20 ℃ to react for 40min to obtain Bi-doped Ag 2 Se quantum dots; doping Ag according to Bi 2 Se quantum dots: PMMA = x: y, uniformly mixing to obtain a powder-gel mixture; and (4) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing at 100 ℃.
Wherein Bi is doped with Ag 2 Se quantum dots: PMMA = x: y is the number y of,
(1) Bi doped Ag 2 Se quantum dots: PMMA =1:0.5, corresponding to p: q =1:0.5;
(2) Bi doped Ag 2 Se quantum dots: PMMA =1: q =1, for p: 1;
(3) Bi doped Ag 2 Se quantum dots: PMMA =1: q =1, corresponding to p: 2.
example 7
Firstly, adding 0.005mol of selenium powder into 5ml of trioctylphosphates, and clarifying the solution at room temperature to obtain a selenium precursor solution; 0.002mol of silver acetate, 20ml of dodecyl mercaptan and 10ml of octadecene were addedHeating to 185 deg.C in a three-neck flask, adding 0.3ml selenium precursor solution, and reacting for 60min to obtain Ag 2 Se quantum dots; dissolving 0.3mmol of bismuth acetate in 20ml of methanol, and heating for reaction for a period of time to obtain a Bi precursor solution. Adding 0.04mmol of Ag 2 Se quantum dots are dissolved in 30ml of toluene, 1.33ml of bismuth precursor solution is added, and the mixture is heated to 20 ℃ to react for 40min to obtain Bi doped Ag 2 And (4) Se quantum dots. According to the formula of epoxy resin: curing agent =1:1, mixing uniformly; doping Ag according to Bi 2 Se quantum dots: mixed glue =1:3, uniformly mixing to obtain a powder-glue mixture; and (4) dispensing the powder glue mixture on the chip, sealing the LED, and drying and curing at the temperature of z ℃.
Wherein the curing temperature after sealing the LED is z ℃,
(1) The curing temperature after sealing the LED was z ℃, corresponding to z =105;
(2) The curing temperature after sealing the LED was z ℃, corresponding to z =125;
(3) The curing temperature after sealing the LED is z ℃, corresponding to z =135;
(4) The post cure temperature for the encapsulated LED was z ℃, corresponding to z =145.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (21)
1. Bi-based doped Ag 2 The preparation method of the ultra-wideband short-wave infrared LED of the Se quantum dot is characterized by comprising the following steps:
(1) Adding selenium powder into the organic phosphine ligand solution to obtain a selenium precursor solution; heating a silver-containing compound, a metal ligand and a non-coordinating solvent, adding a selenium precursor solution, and reacting to obtain Ag 2 Se quantum dots;
(2) Dissolving a bismuth-containing compound in a polar solvent, and heating for reaction to obtain a Bi precursor solution; mixing Ag with water 2 Se quantum dot and a certain amount of bismuth precursor solutionThermal reaction to obtain Bi doped Ag 2 Se quantum dots;
(3) Uniformly mixing epoxy resin and a curing agent to obtain a mixed glue;
(4) Doping the Bi obtained in the step (2) with Ag 2 Uniformly mixing the Se quantum dots with the mixed glue obtained in the step (3) to obtain a powder glue mixture;
(5) Dispensing the powder glue mixture on a chip, sealing the LED, and drying and curing; the chip is a purple light chip or a blue light chip, and the peak wavelength is 395nm or 460nm respectively.
2. The method according to claim 1, wherein the organophosphine ligand solution in step (1) is one selected from the group consisting of trioctylphosphine ester, tri-n-octylphosphine oxide, tributylphosphine, trihexylphosphine, and tetradecylphosphoric acid.
3. The method of claim 1, wherein the silver-containing compound in step (1) is one selected from the group consisting of silver nitrate, silver acetate, and silver diethyldithiocarbamate.
4. The method of claim 1, wherein the metal ligand of step (1) is selected from the group consisting of an alkylthiol and an alkyldithiol.
5. The method according to claim 1, wherein the non-coordinating solvent in step (1) is one selected from octadecene, oleylamine and liquid paraffin.
6. The method according to claim 1, wherein the bismuth-containing compound in the step (2) is one selected from the group consisting of bismuth acetate, bismuth oxide, bismuth oxalate, bismuth nitrate and bismuth chloride.
7. The preparation method according to claim 1, wherein the selenium powder in the step (1) is added into the organic phosphine ligand solution to react at room temperature, and the reaction time at room temperature is 0.5 h-2 h.
8. The preparation method according to claim 1, wherein the heating reaction in the step (1) is carried out at a temperature of 150 ℃ to 200 ℃ for a reaction time of 30min to 90min.
9. The method according to claim 1, wherein the ratio of Ag: the molar ratio of Se is 3:1 to 5:1.
10. the method of claim 1, wherein the Bi to Ag content in step (2) is 0.15 mol% to 15 mol%.
11. The preparation method according to claim 1, wherein the heating reaction temperature in the step (2) is 20 ℃ to 40 ℃ and the reaction time is 20min to 60min.
12. The method according to claim 1, wherein the heating reaction in the steps (1) and (2) is completed and then the steps of washing and drying are further included; the washing is carried out by adopting acetone, and the drying temperature is 60 ℃.
13. The method according to claim 1, wherein both of the step (1) and the step (2) are performed in an oxygen-free and water-free inert gas atmosphere, which is one of a nitrogen atmosphere and an argon atmosphere.
14. The preparation method according to claim 1, wherein in the step (3), the mass ratio of the epoxy resin to the curing agent is 2; the curing agent is a curing type organic silicon rubber material.
15. The method of claim 1, wherein in step (4) Bi is doped with Ag 2 The mass ratio of the Se quantum dots to the mixed glue is 1 to 4-1.
16. The method of claim 15, whereinCharacterized in that the mixed glue can be replaced by polymethyl methacrylate material PMMA, and Bi is doped with Ag 2 The mass ratio of the Se quantum dots to the PMMA is 1.
17. The method of claim 1, wherein the step of removing bubbles by vacuum after mixing in step (3) and step (4) is further included.
18. The method of claim 1, wherein the drying and curing temperature in the step (5) is 80 ℃ to 180 ℃.
19. The method of claim 1, wherein the size of the chip in step (5) is 7.3mm by 7.3 mm.
20. The Bi-doped Ag-based material as claimed in any one of claims 1 to 19 2 Bi-based doped Ag prepared by Se quantum dot preparation method 2 And the Se quantum dot ultra-wideband short-wave infrared LED.
21. The Bi-doped Ag-based alloy of claim 20 2 The application of the ultra-wideband short-wave infrared LED of the Se quantum dot in food safety analysis, noninvasive health detection, crop and environment detection.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712490A (en) * | 2009-11-20 | 2010-05-26 | 云南大学 | Method for preparing polysiloxane by catalyzing polymeric silane with sulfureted bismuth silver and nanometer noble metals |
| CN104327847A (en) * | 2014-09-30 | 2015-02-04 | 东南大学 | Preparation method of pure yellow fluorescence water-soluble doped zinc selenide quantum dots |
| CN106867532A (en) * | 2017-03-16 | 2017-06-20 | 武汉理工大学 | Lanthanide rare ytterbium doping silver sulfide quantum dot and its preparation method and application |
| CN107954467A (en) * | 2017-11-03 | 2018-04-24 | 畅的新材料科技（上海）有限公司 | A kind of silver, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712490A (en) * | 2009-11-20 | 2010-05-26 | 云南大学 | Method for preparing polysiloxane by catalyzing polymeric silane with sulfureted bismuth silver and nanometer noble metals |
| CN104327847A (en) * | 2014-09-30 | 2015-02-04 | 东南大学 | Preparation method of pure yellow fluorescence water-soluble doped zinc selenide quantum dots |
| CN106867532A (en) * | 2017-03-16 | 2017-06-20 | 武汉理工大学 | Lanthanide rare ytterbium doping silver sulfide quantum dot and its preparation method and application |
| CN107954467A (en) * | 2017-11-03 | 2018-04-24 | 畅的新材料科技（上海）有限公司 | A kind of silver, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology |
Non-Patent Citations (1)
| Title |
|---|
| The effect of doping process on the structural and optical properties of Ag2Se thin films;Rana Gamal Mazban 等;《AIP Conference Proceedings》;20201215;第2307卷;第020034页 * |
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