CN110635012A - Preparation of high-stability perovskite quantum dot white light-emitting diode based on manganese ion doped lead-cesium chloride embedded in zeolite - Google Patents
Preparation of high-stability perovskite quantum dot white light-emitting diode based on manganese ion doped lead-cesium chloride embedded in zeolite Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-stability perovskite quantum dot white light-emitting diode based on manganese ion doped lead cesium chloride embedded in zeolite+Ion-exchanging the ions into the zeolite and then reacting it with PbCl dissolved in an organic solvent2Reaction, using two separate steps, prevents rejection of cations, thereby allowing Cs to react+And Pb2+Taken together, the pure Mn embedded in the zeolite is finally obtained: CsPbCl3The white perovskite quantum dot photoluminescent device is prepared by coating the perovskite quantum dot composite material on a bluish-purple luminescent bead in combination with green fluorescent powder. The invention greatly improves the stability of the perovskite quantum dot, reduces the loss of the device, and passes through Mn2+For Pb2+Is gotAnd the use of toxic element lead is reduced, the photoluminescence efficiency is improved, and the perovskite quantum dots are better developed towards the green and environment-friendly direction.
Description
Technical Field
The invention relates to the technical field of perovskite quantum dot photoelectric materials, in particular to a preparation method of a high-stability perovskite quantum dot white light-emitting diode based on manganese ion doped chlorine lead cesium embedded in zeolite.
Background
In recent years, all-inorganic perovskites (CsPbX)3X ═ Cl, Br, I) Quantum Dots (QDs) have attracted much attention due to their excellent optoelectronic properties, and this field is rapidly developing. The all-inorganic perovskite quantum dot has high photoluminescence quantum yield and adjustable narrow-band emission in the whole visible spectrum range, so that the all-inorganic perovskite quantum dot is widely applied to the fields of quantum dot white light emitting diodes (WQLEDs), lasers and the like. Although at present, CsPbX is used domestically and abroad3The research of quantum dots as color conversion fluorescent powder is greatly advanced, and the WQLED with better performance is obtained, but the poor stability of the WQLED is still the main defect of the WQLED, which seriously restricts the practical application of devices, especially for the WQLED containing I-The red quantum dots of (2) have very poor resistance to high temperature and moisture.
Therefore, in recent research, efforts have been made to prepare more stable perovskite quantum dots by various methods. On one hand, researchers can isolate oxygen and moisture in the air by embedding perovskite quantum dots into an organic/inorganic matrix or coating the perovskite quantum dots with polymer/silicon dioxide; on the other hand, numerous studies have shown that Zn2+、Cd2+、Sr2+、Ni2+、 Sn2+And Mn2+The chemical composition, the energy band structure and the photoelectric property of the semiconductor nanocrystal can be adjusted by ion doping. And Mn in inorganic perovskite2+The doping can not only improve the photoluminescence yield of the perovskite quantum dots and reduce the use of toxic element lead in the cesium lead perovskite, but also can greatly improve the stability of the quantum dots in the environment. And, Mn in perovskite quantum dots2The orange red emitting light can effectively substitute I-group red fluorescent powder. However, in the two methods, the coating with the polymer/inorganic substance can not even reduce the optical properties such as the luminous efficiency of the perovskite quantum dot, such as oxygen and moisture isolation; and Mn2+The plasma doped perovskite quantum dots can lead Mn to be generated with time2+Plasma is precipitated from the perovskite, thereby reducing its stability. Therefore, we provide a method for combining the two to synthesize perovskite quantum dots with high stability and high luminous efficiency, and apply the perovskite quantum dots to a photoluminescence device.
Disclosure of Invention
The invention aims to solve the problems that: provides a preparation method of a high-stability perovskite quantum dot white light-emitting diode based on manganese ion doped lead cesium chloride embedded in zeolite, in CsPbCl3Mn doping2+On the basis of improving the stability of the perovskite, the Mn: CsPbCl3Synthesized in zeolite, the perovskite material is isolated from oxygen and water in air environment, and the double effects of improving the luminous efficiency and enhancing the stability of the material are achieved. Finally, the obtained material is applied to a photoluminescence device, so that the loss of the device is reduced, and a wider path is provided for material selection for manufacturing a quantum dot white light-emitting device, thereby further realizing the commercial application value of the perovskite quantum dot photoluminescence diode.
The technical scheme provided by the invention for solving the problems is as follows: a preparation method of a high-stability perovskite quantum dot white light-emitting diode based on manganese ion doped lead cesium chloride embedded in zeolite comprises the following steps,
(1) firstly, 2.337g to 9.348g of NaAlO are mixed2Adding the solution into 8-36 mL of 1.25mol/L NaOH solution, and stirring for 1h at the rotation speed of 200-800rpm by using a magnetic stirrer to prepare a first solution;
(2) 9.845g to 39.38g of silica sol (HS-4015) is dissolved in 3.62mL to 14.48mL of distilled water, and a magnetic stirrer is used for stirring for 1h at the rotating speed of 200 and 800rpm to prepare a second solution;
(3) after the first solution and the second solution are stirred for 1 hour, slowly dripping the first solution into the second solution at the speed of 10 mL/hour, continuously stirring the second solution at the rotating speed of 200-800rpm by using a magnetic stirrer in the process, and continuously stirring for 5 hours at the same stirring speed after dripping is finished to prepare a third solution;
(4) putting the third solution into a 100mL flask, introducing nitrogen, standing at 25-30 ℃ for 48h, then heating to 100 ℃, and putting in a vacuum environment for 12h to obtain a dry zeolite solid; washing the obtained zeolite solid with distilled water until the pH value is 7, and then drying the zeolite solid in a vacuum environment at 100 ℃ for 24 hours;
(5) dispersing 1.0-4.0 g of the prepared zeolite into 10.0-40 mL of aqueous solution of 1.0mol/LCsBr to prepare a fourth solution;
(6) stirring the fourth solution in a 70 ℃ water bath for 24 hours at the rotating speed of 200-800rpm by using a magnetic stirrer, centrifuging the stock solution, washing the stock solution twice by using deionized water, and drying the stock solution in air at the temperature of 80-100 ℃ for 12 hours to prepare first powder;
(7) 0.2mmol-1mmol of PbCl2And 0.2mmol to 1mmol of MnCl2Mixing with 5.0mL of 1-octadecene in a 25mL three-necked bottle, and vacuum drying at 80-120 deg.C for 20-80 min to obtain a fifth solution;
(8) introducing N after the fifth solution is dried2Heating to 150 ℃, injecting 2-8 mL of oleic acid and oleylamine with the same quantity as the oleic acid at the temperature, and simultaneously injecting 1-4 mL of tri-n-octylphosphine; PbCl in the second solution2And MnCl2After complete dissolution, the solution is in N2Naturally cooling to 20-30 ℃ under the environment to prepare a sixth solution;
(9) mixing 0.5g-2g of the first powder and 5mL-20mL of 1-octadecene in a 100mL three-necked bottle, and then carrying out vacuum drying at 80-120 ℃ for 20min-80min to prepare a seventh solution;
(10) and introducing N into the seventh solution after vacuum drying is finished2Heating to 190 ℃, quickly injecting 10-40 mL of sixth solution at 190 ℃, reacting for 10-20 min, and stopping the reaction by using ice bath cooling to obtain a crude product;
(11) the crude product is treated by normal hexane and isopropanolWashing and centrifuging to obtain pure composite material, Mn embedded in zeolite: CsPbCl3Powder;
(12) taking 0.03g of Mn embedded in the zeolite: CsPbCl3Placing 0.2g of polystyrene in a 50mL centrifuge tube, adding 10mL of toluene, and fully shaking and mixing by using a vortex mixer to obtain an eighth solution;
(13) putting 0.01g of green fluorescent powder and 0.2g of polystyrene into a 50mL centrifuge tube, then adding 10mL of toluene, and fully shaking and mixing by using a vortex mixer to prepare a ninth solution;
(14) respectively taking 1mL of the eighth solution and 1mL of the ninth solution by using two 1mL needle tubes, dropwise adding 0.15mL of the eighth solution onto a blue fluorescent lamp bead, and then placing the lamp bead in an oven at 80 ℃ for drying for 20 min; then taking out the lamp bead, dropwise adding 0.1mL of ninth solution after the lamp bead is cooled to room temperature, and drying in an oven at 80 ℃ for 20min after dropwise adding;
(15) and (5) after the drying in the step (14) is finished, taking the lamp bead cap to cover the light-emitting part of the lamp bead, and finishing the manufacturing.
Compared with the prior art, the invention has the advantages that: first, we prepared a zeolite solid for coating and protecting manganese doped perovskites. Then, Na in the pore structure of the zeolite crystallites is strongly stirred in an aqueous CsBr solution at 60 ℃+Is exchanged into Cs+。Cs+The zeolite crystals were washed and dried, dispersed in ODE and heated to 130 deg.C-170 deg.C. In N2Under the condition of environment and intense stirring, adding PbCl2With MnCl2The mixed solution of (2) is poured into the zeolite solution. The Mn-doped silicon oxide forms in the zeolite structure within 10-15 minutes2+The perovskite quantum dot of (1). The synthesized perovskite quantum dot has double emission peaks of about 400nm and about 600nm and is red-orange in luminescence. Finally, polystyrene is used as a carrier and a packaging material, and the polystyrene and green fluorescent powder are coated on the small lamp beads emitting blue-violet light to form a three-primary-color light source, so that the white perovskite quantum dot photoluminescence device is obtained. In Mn2+Under the dual action of doping and zeolite coating, the stability of the perovskite quantum dots is greatly improved, and the loss of devices is reducedConsuming and passing Mn2+For Pb2+The substitution reduces the use of toxic element lead, improves the photoluminescence efficiency, and leads the perovskite quantum dots to be better developed towards the green and environment-friendly direction.
Detailed Description
The following embodiments are described in detail with reference to the accompanying drawings, so that how to implement the technical features of the present invention to solve the technical problems and achieve the technical effects can be fully understood and implemented.
Example 1: a preferred embodiment of the present invention. The method comprises the following steps:
1) firstly 2.337g NaAlO2Adding the solution into 8mL of 1.25mol/L NaOH solution, and stirring for 1h at the rotating speed of 300rpm by using a magnetic stirrer to prepare a first solution;
2) 9.845g of silica sol (HS-4015) was dissolved in 3.62mL of distilled water, and stirred for 1h at 200rpm using a magnetic stirrer to prepare a second solution;
3) after the first solution and the second solution are stirred for 1 hour, slowly dripping the first solution into the second solution at the speed of 10mL/h, continuously stirring the second solution at the rotating speed of 300rpm by using a magnetic stirrer in the process, and continuously stirring for 5 hours at the same stirring speed after finishing dripping to prepare a third solution;
4) and putting the third solution into a 100mL flask, introducing nitrogen, standing at 25-30 ℃ for 48h, then heating to 100 ℃, and standing in a vacuum environment for 12h to obtain a dry zeolite solid. Washing the obtained zeolite solid with distilled water until the pH value is 7, and then drying the zeolite solid in a vacuum environment at 100 ℃ for 24 hours;
5) dispersing 1.0g of the prepared zeolite in 10.0mL of aqueous solution of 1.0mol/LCsBr to prepare a fourth solution;
6) stirring the fourth solution in a 70 ℃ water bath for 24 hours at the rotating speed of 300rpm by using a magnetic stirrer, centrifuging the stock solution, washing the centrifuged stock solution twice by using deionized water, and drying the centrifuged stock solution in 80 ℃ air for 12 hours to prepare first powder;
7)0.5mmol of PbCl2And 0.5mmol of MnCl2Mixed with ODE (5.0mL) in a 25mL three-necked flask,vacuum drying at 80-120 deg.C for 30min to obtain fifth solution;
8) introducing N after the fifth solution is dried2And heated to 150 c at which temperature 2mL of Oleic Acid (OA) and an equivalent amount of Oleylamine (OAM) were injected, while 1mL of tri-n-octylphosphine was injected. PbCl in the second solution2And MnCl2After complete dissolution, the solution is in N2Naturally cooling to 20-30 ℃ under the environment to prepare a sixth solution;
9) mixing 0.5g of the first powder with 5mL of 1-Octadecene (ODE) in a 100mL three-necked flask, and vacuum drying at 80 deg.C for 20min to obtain a seventh solution;
10) introducing N into the seventh solution after vacuum drying2And the temperature is increased to 190 ℃, 10mL of sixth solution is quickly injected at 190 ℃, the reaction is stopped by using ice bath cooling after 10min of reaction, and a crude product is obtained.
11) And (3) cleaning and centrifuging the crude product by using normal hexane and isopropanol to obtain a pure composite material, namely Mn embedded in zeolite: CsPbCl3;
12) Taking 0.03g of Mn embedded in zeolite: CsPbCl3The powder was placed with 0.2g polystyrene in a 50mL centrifuge tube, then 10mL toluene was added and mixed thoroughly with shaking using a vortex mixer. An eighth solution is prepared.
13) 0.01g of green phosphor and 0.2g of polystyrene were placed in a 50mL centrifuge tube, then 10mL of toluene was added, and mixed by shaking thoroughly using a vortex mixer. A ninth solution is prepared.
14) And (3) respectively taking 1mL of the eighth solution and 1mL of the ninth solution by using two 1mL needle tubes, dropwise adding 0.03mL of the eighth solution onto a blue fluorescent lamp bead, and then placing the lamp bead in an oven at 80 ℃ for drying for 20 min. And then taking out the lamp bead, dropwise adding 0.1mL of ninth solution after the lamp bead is cooled to room temperature, and drying in an oven at 80 ℃ for 20min after dropwise adding.
15) And (5) after the drying in the step 14) is finished, taking the lamp bead cap to cover the light-emitting part of the lamp bead, and finishing the manufacturing.
Example 2:
1) firstly 4.674g NaAlO2Adding into 16mL of 1.25mol/L NaOH solution, and stirring with a magnetic stirrerStirring at the rotating speed of 400rpm for 1h to prepare a first solution;
2) dissolving 19.69g of silica sol (HS-4015) in 7.24mL of distilled water, and stirring for 1h at the rotating speed of 400rpm by using a magnetic stirrer to prepare a second solution;
3) after the first solution and the second solution are stirred for 1 hour, slowly dripping the first solution into the first solution at the speed of 10mL/h, continuously stirring the first solution at the rotating speed of 400rpm by using a magnetic stirrer in the process, and continuously stirring for 5 hours at the same stirring speed after finishing dripping to prepare a third solution;
4) the third solution was placed in a 100mL flask, purged with nitrogen, left at 30 ℃ for 48h, then warmed to 100 ℃ and placed under vacuum for 12h to give a dry zeolite solid. Washing the obtained zeolite solid with distilled water until the pH value is 7, and then drying the zeolite solid in a vacuum environment at 100 ℃ for 24 hours;
5) dispersing 2g of the prepared zeolite into 20mL of aqueous solution of 1.0mol/LCsBr to prepare a fourth solution;
6) stirring the fourth solution in a 70 ℃ water bath for 24 hours at the rotating speed of 400rpm by using a magnetic stirrer, centrifuging the stock solution, washing the centrifuged stock solution twice by using deionized water, and drying the centrifuged stock solution in 100 ℃ air for 12 hours to prepare first powder;
7) 0.2mmol of PbCl2And 0.5mmol of MnCl2Mixing with ODE (5.0mL) in 25mL three-necked flask, and vacuum drying at 80 deg.C for 30min to obtain fifth solution;
8) introducing N after the fifth solution is dried2And heated to 150 c at which temperature 2mL of Oleic Acid (OA) and an equivalent amount of Oleylamine (OAM) were injected, while 1mL of tri-n-octylphosphine was injected. PbCl in the second solution2And MnCl2After complete dissolution, the solution is in N2Naturally cooling to 25 ℃ in the environment to prepare a sixth solution;
9) mixing 1g of the first powder with 10mL of 1-Octadecene (ODE) in a 100mL three-necked flask, and vacuum drying at 80 deg.C for 30min to obtain a seventh solution;
10) introducing N into the seventh solution after vacuum drying2Heating to 190 deg.C, rapidly injecting 10mL of sixth solution at 190 deg.C, and reactingThe reaction was stopped after 15min by cooling with an ice bath to obtain the crude product.
11) And (3) cleaning and centrifuging the crude product by using normal hexane and isopropanol to obtain a pure composite material, namely Mn embedded in zeolite: CsPbCl3。
12) Taking 0.02g of Mn embedded in zeolite: CsPbCl3The powder was placed with 0.2g polystyrene in a 50mL centrifuge tube, then 10mL toluene was added and mixed thoroughly with shaking using a vortex mixer. An eighth solution is prepared.
13) 0.01g of green phosphor and 0.2g of polystyrene were placed in a 50mL centrifuge tube, then 10mL of toluene was added, and mixed by shaking thoroughly using a vortex mixer. A ninth solution is prepared.
14) And (3) respectively taking 1mL of the eighth solution and 1mL of the ninth solution by using two 1mL needle tubes, dropwise adding 0.015mL of the eighth solution onto a blue fluorescent lamp bead, and then placing the lamp bead in an oven at 80 ℃ for drying for 20 min. And then taking out the lamp bead, dropwise adding 0.1mL of ninth solution after the lamp bead is cooled to room temperature, and drying in an oven at 80 ℃ for 20min after dropwise adding.
15) And (5) after the drying in the step 14) is finished, taking the lamp bead cap to cover the light-emitting part of the lamp bead, and finishing the manufacturing.
Example 3:
1) firstly 9.348g NaAlO2Adding the solution into 36mL of 1.25mol/L NaOH solution, and stirring for 1h at the rotating speed of 800rpm by using a magnetic stirrer to prepare a first solution;
2) dissolving 39.38g of silica sol (HS-4015) in 14.48mL of distilled water, and stirring for 1h at the rotating speed of 800rpm by using a magnetic stirrer to prepare a second solution;
3) after the first solution and the second solution are stirred for 1 hour, slowly dripping the first solution into the first solution at the speed of 10mL/h, continuously stirring the first solution at the rotating speed of 800rpm by using a magnetic stirrer in the process, and continuously stirring for 5 hours at the same stirring speed after finishing dripping to prepare a third solution;
4) the third solution was placed in a 100mL flask, purged with nitrogen, left at 30 ℃ for 48h, then warmed to 100 ℃ and placed under vacuum for 12h to give a dry zeolite solid. Washing the obtained zeolite solid with distilled water until the pH value is 7, and then drying the zeolite solid in a vacuum environment at 100 ℃ for 24 hours;
5) dispersing 4.0g of the prepared zeolite into 40mL of aqueous solution of 1.0mol/LCsBr to prepare a fourth solution;
6) stirring the fourth solution in a 70 ℃ water bath for 24 hours at the rotating speed of 800rpm by using a magnetic stirrer, centrifuging the stock solution, washing the centrifuged stock solution twice by using deionized water, and drying the centrifuged stock solution in 100 ℃ air for 12 hours to prepare first powder;
7)0.5mmol of PbCl2And 0.2mmol of MnCl2Mixing with ODE (5.0mL) in a 25mL three-necked flask, and vacuum drying at 120 deg.C for 60min to obtain a fifth solution;
8) introducing N after the fifth solution is dried2And heated to 150 c at which temperature 2mL of Oleic Acid (OA) and an equivalent amount of Oleylamine (OAM) were injected, while 1mL of tri-n-octylphosphine was injected. PbCl in the second solution2And MnCl2After complete dissolution, the solution is in N2Naturally cooling to 30 ℃ in the environment to prepare a sixth solution;
9) mixing 0.5g of the first powder with 5mL of 1-Octadecene (ODE) in a 25mL three-necked flask, and vacuum drying at 80 deg.C for 20min to obtain a seventh solution;
10) introducing N into the seventh solution after vacuum drying2And the temperature is increased to 190 ℃, 10mL of sixth solution is quickly injected at 190 ℃, the reaction is stopped by using ice bath cooling after 10min of reaction, and a crude product is obtained.
11) And (3) cleaning and centrifuging the crude product by using normal hexane and isopropanol to obtain a pure composite material, namely Mn embedded in zeolite: CsPbCl3。
12) Taking 0.03g of Mn embedded in zeolite: CsPbCl3The powder was placed with 0.2g polystyrene in a 50mL centrifuge tube, then 10mL toluene was added and mixed thoroughly with shaking using a vortex mixer. An eighth solution is prepared.
13) 0.01g of green phosphor and 0.2g of polystyrene were placed in a 50mL centrifuge tube, then 10mL of toluene was added, and mixed by shaking thoroughly using a vortex mixer. A ninth solution is prepared.
14) And (3) respectively taking 1mL of the eighth solution and 1mL of the ninth solution by using two 1mL needle tubes, dropwise adding 0.015mL of the eighth solution onto a blue fluorescent lamp bead, and then placing the lamp bead in an oven at 80 ℃ for drying for 20 min. And then taking out the lamp bead, dropwise adding 0.1mL of ninth solution after the lamp bead is cooled to room temperature, and drying in an oven at 80 ℃ for 20min after dropwise adding.
15) And (5) after the drying in the step 14) is finished, taking the lamp bead cap to cover the light-emitting part of the lamp bead, and finishing the manufacturing.
The foregoing is merely illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary. All changes which come within the scope of the invention as defined by the independent claims are intended to be embraced therein.
Claims (1)
1. A preparation method of a manganese ion doped chlorine lead cesium high-stability perovskite quantum dot white light emitting diode based on being embedded in zeolite is characterized by comprising the following steps: the method comprises the following steps of,
(1) firstly, 2.337g to 9.348g of NaAlO are mixed2Adding the solution into 8-36 mL of 1.25mol/L NaOH solution, and stirring for 1h at the rotation speed of 200-800rpm by using a magnetic stirrer to prepare a first solution;
(2) 9.845g to 39.38g of silica sol (HS-4015) is dissolved in 3.62mL to 14.48mL of distilled water, and a magnetic stirrer is used for stirring for 1h at the rotating speed of 200 and 800rpm to prepare a second solution;
(3) after the first solution and the second solution are stirred for 1 hour, slowly dripping the first solution into the second solution at the speed of 10 mL/hour, continuously stirring the second solution at the rotating speed of 200-800rpm by using a magnetic stirrer in the process, and continuously stirring for 5 hours at the same stirring speed after dripping is finished to prepare a third solution;
(4) putting the third solution into a 100mL flask, introducing nitrogen, standing at 25-30 ℃ for 48h, then heating to 100 ℃, and putting in a vacuum environment for 12h to obtain a dry zeolite solid; washing the obtained zeolite solid with distilled water until the pH value is 7, and then drying the zeolite solid in a vacuum environment at 100 ℃ for 24 hours;
(5) dispersing 1.0-4.0 g of the prepared zeolite into 10.0-40 mL of aqueous solution of 1.0mol/LCsBr to prepare a fourth solution;
(6) stirring the fourth solution in a 70 ℃ water bath for 24 hours at the rotating speed of 200-800rpm by using a magnetic stirrer, centrifuging the stock solution, washing the stock solution twice by using deionized water, and drying the stock solution in air at the temperature of 80-100 ℃ for 12 hours to prepare first powder;
(7) 0.2mmol-1mmol of PbCl2And 0.2mmol to 1mmol of MnCl2Mixing with 5.0mL of 1-octadecene in a 25mL three-necked bottle, and vacuum drying at 80-120 deg.C for 20-80 min to obtain a fifth solution;
(8) introducing N after the fifth solution is dried2Heating to 150 ℃, injecting 2-8 mL of oleic acid and oleylamine with the same quantity as the oleic acid at the temperature, and simultaneously injecting 1-4 mL of tri-n-octylphosphine; PbCl in the second solution2And MnCl2After complete dissolution, the solution is in N2Naturally cooling to 20-30 ℃ under the environment to prepare a sixth solution;
(9) mixing 0.5g-2g of the first powder and 5mL-20mL of 1-octadecene in a 100mL three-necked bottle, and then carrying out vacuum drying at 80-120 ℃ for 20min-80min to prepare a seventh solution;
(10) and introducing N into the seventh solution after vacuum drying is finished2Heating to 190 ℃, quickly injecting 10-40 mL of sixth solution at 190 ℃, reacting for 10-20 min, and stopping the reaction by using ice bath cooling to obtain a crude product;
(11) and cleaning and centrifuging the crude product by using normal hexane and isopropanol to obtain a pure composite material, namely Mn embedded in zeolite: CsPbCl3Powder;
(12) taking 0.03g of Mn embedded in the zeolite: CsPbCl3Placing 0.2g of polystyrene in a 50mL centrifuge tube, adding 10mL of toluene, and fully shaking and mixing by using a vortex mixer to obtain an eighth solution;
(13) putting 0.01g of green fluorescent powder and 0.2g of polystyrene into a 50mL centrifuge tube, then adding 10mL of toluene, and fully shaking and mixing by using a vortex mixer to prepare a ninth solution;
(14) respectively taking 1mL of the eighth solution and 1mL of the ninth solution by using two 1mL needle tubes, dropwise adding 0.15mL of the eighth solution onto a blue fluorescent lamp bead, and then placing the lamp bead in an oven at 80 ℃ for drying for 20 min; then taking out the lamp bead, dropwise adding 0.1mL of ninth solution after the lamp bead is cooled to room temperature, and drying in an oven at 80 ℃ for 20min after dropwise adding;
(15) and (5) after the drying in the step (14) is finished, taking the lamp bead cap to cover the light-emitting part of the lamp bead, and finishing the manufacturing.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111534301A (en) * | 2020-03-31 | 2020-08-14 | 厦门大学 | CsPbBr3Preparation method of perovskite quantum dots |
CN111739995A (en) * | 2020-07-03 | 2020-10-02 | 青岛科技大学 | White light LED based on dual-waveband white light perovskite quantum dots and preparation method |
CN113025311A (en) * | 2021-03-17 | 2021-06-25 | 广东工业大学 | Manganese-doped cesium-lead-chlorine luminophor based on silicon dioxide coating and preparation method and application thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106268926A (en) * | 2015-05-18 | 2017-01-04 | 中国科学院大连化学物理研究所 | A kind of MCM-22 molecular sieve with multistage pore canal and its preparation method and application |
CN109266344A (en) * | 2018-11-21 | 2019-01-25 | 南京邮电大学 | The preparation method of one type halogen perovskite quanta point material |
-
2019
- 2019-09-12 CN CN201910862520.6A patent/CN110635012A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106268926A (en) * | 2015-05-18 | 2017-01-04 | 中国科学院大连化学物理研究所 | A kind of MCM-22 molecular sieve with multistage pore canal and its preparation method and application |
CN109266344A (en) * | 2018-11-21 | 2019-01-25 | 南京邮电大学 | The preparation method of one type halogen perovskite quanta point material |
Non-Patent Citations (1)
Title |
---|
孙佳奕: ""钙钛矿量子点与分子筛复合材料的制备与性能研究"", 《中国优秀硕士学位论文全文数据库》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111534301A (en) * | 2020-03-31 | 2020-08-14 | 厦门大学 | CsPbBr3Preparation method of perovskite quantum dots |
CN111739995A (en) * | 2020-07-03 | 2020-10-02 | 青岛科技大学 | White light LED based on dual-waveband white light perovskite quantum dots and preparation method |
CN113025311A (en) * | 2021-03-17 | 2021-06-25 | 广东工业大学 | Manganese-doped cesium-lead-chlorine luminophor based on silicon dioxide coating and preparation method and application thereof |
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