CN108865127B - White-light perovskite, preparation method thereof and LED device - Google Patents
White-light perovskite, preparation method thereof and LED device Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 32
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 20
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 19
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 19
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000005642 Oleic acid Substances 0.000 claims abstract description 19
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 19
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 10
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 10
- 239000011565 manganese chloride Substances 0.000 claims abstract description 10
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- -1 thulium halide Chemical class 0.000 claims abstract description 7
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 57
- 239000000843 powder Substances 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 10
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- 239000000463 material Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- LZOMHYVAEHYDST-UHFFFAOYSA-K thulium(3+);triiodide Chemical compound I[Tm](I)I LZOMHYVAEHYDST-UHFFFAOYSA-K 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000006862 quantum yield reaction Methods 0.000 abstract description 10
- 230000003287 optical effect Effects 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 239000011572 manganese Substances 0.000 description 13
- 239000012300 argon atmosphere Substances 0.000 description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 1
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7704—Halogenides
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Abstract
A white perovskite, a preparation method thereof and an LED device relate to the technical field of optical display. White light calciumThe preparation method of the titanium ore comprises the following steps: mixing CsCO3Mixing with octadecene and oleic acid, heating to 115-125 ℃ in an inert gas atmosphere for reaction, heating to 145-155 ℃, and preserving heat to obtain a Cs acid precursor. Reacting PbBr2、MnCl2Mixing oleic acid, oleylamine, HBr and octadecene, and heating to 115-125 ℃ in an inert gas atmosphere to react to obtain a first solution. Mixing thulium halide and octadecene, heating to 155-165 ℃ in an inert gas atmosphere, and reacting to obtain a second solution. Cooling the second solution, and mixing the second solution with the first solution for reaction to obtain a third solution; and mixing the third solution and the Cs acid precursor for reaction, cooling in a water bath, and centrifuging to remove the supernatant to obtain a lower-layer substance. The white perovskite prepared by the method can display white light and has high white light quantum yield.
Description
Technical Field
The invention relates to the technical field of optical display, in particular to white-light perovskite, a preparation method thereof and an LED device.
Background
White light display (illumination) is an important research topic in the optical field, because white light illumination is ubiquitous, the white light illumination has a wide application prospect, and the improvement of the efficiency of white light illumination materials can save tens of thousands of energy sources for the whole world every year.
Existing white light displays (lighting) are mostly realized by the following three ways:
(1) blue LED chip + yellow phosphor or blue LED chip + red phosphor + green phosphor; (2) the LED fluorescent lamp comprises an ultraviolet LED chip, red fluorescent powder, green fluorescent powder and blue fluorescent powder; (3) ultraviolet LED chip + white light phosphor powder.
When white light is realized by mixing multiple phosphors in the manners of (1) and (2), the final device is very unstable due to different lifetimes, attenuations and stabilities of each phosphor, resulting in white light shift and color change. In addition, the energy is transferred and converted by different substances for many times, resulting in large energy loss. The efficiency of the device is affected and the energy is wasted.
The method (3) can overcome the defects caused by the methods (1) and (2), simplify the preparation process of the device and save the cost.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of white perovskite, which can prepare white perovskite with good quality.
The second purpose of the invention is to provide a white perovskite which is prepared by the preparation method of the white perovskite and has higher white quantum yield.
A third object of the present invention is to provide an LED device capable of emitting white light.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of white perovskite, which comprises the following steps:
mixing CsCO3Mixing with octadecene and oleic acid, heating to 115-125 ℃ in an inert gas atmosphere for reaction, heating to 145-155 ℃, and preserving heat to obtain a Cs acid precursor;
reacting PbBr2、MnCl2Mixing oleic acid, oleylamine, HBr and octadecene, and heating to 115-125 ℃ in an inert gas atmosphere to react to obtain a first solution;
mixing thulium halide and octadecene, heating to 155-165 ℃ in an inert gas atmosphere, and reacting to obtain a second solution;
reducing the temperature of the second solution to 115-125 ℃, and mixing the second solution with the first solution for reaction to obtain a third solution; and mixing the third solution and the Cs acid precursor for reaction, cooling in a water bath, and centrifuging to remove the supernatant to obtain a lower-layer substance.
A white perovskite is prepared by the preparation method of the white perovskite.
An LED device comprises an LED chip and a coating coated on the surface of the LED chip, wherein the coating is obtained by coating the white perovskite on the surface of the LED chip.
The embodiment of the invention has the beneficial effects that:
the preparation method of the white perovskite is used for obtaining CsPbBrxCl3-xIn the process, transition metal manganese (Mn) and rare earth metal thulium (Tm) are doped, the doped Mn can introduce a new potential well state, and partial excitons can be separated from host perovskite CsPbBrxCl3-xTransferred to the potential well state of Mn, and transited downwards through the energy level of Mn to emit orange light of about 600 nm. Host perovskite CsPbBrxCl3-xBlue-green light emission, host perovskite CsPbBr regulated by HBrxCl3-xThe halogen is used for coordinating the two light proportions, namely, the white light emission can be realized by internal mixing. The rare earth element Tm can be introduced into new potential well state, and Tm potential well state can promote exciton from host perovskite CsPbBrxCl3-xTransfer to the potential well state of Mn, and simultaneously improve the quantum yield.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a spectrum diagram of a white perovskite phosphor prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following describes a white perovskite, a preparation method thereof and an LED device according to an embodiment of the present invention.
A preparation method of white perovskite comprises the following steps:
mixing CsCO3Mixing with octadecene and oleic acid, heating to 115-125 ℃ in an inert gas atmosphere for reaction, heating to 145-155 ℃, and preserving heat to obtain a Cs acid precursor. Wherein CsCO3The ratio of octadecylene to octadecene is 0.7-0.9 g: 36-42 mL. Octadecene and oleic acid mainly play a role in dispersing CsCO3The function of (1).
Reacting PbBr2、MnCl2Mixing oleic acid, oleylamine, HBr and octadecene, and heating to 115-125 ℃ in an inert gas atmosphere to react to obtain a first solution. Wherein, PbBr2With MnCl2The molar ratio of (A) to (B) is 1-2: 1.
Mixing thulium halide and octadecene, heating to 155-165 ℃ in an inert gas atmosphere, and reacting to obtain a second solution. Wherein the thulium halide comprises TmCl3、TmBr3Or TmI3。
And cooling the second solution to 115-125 ℃, and mixing the second solution with the first solution for reaction to obtain a third solution. Since the temperature of the second solution is lowered, there is no or a small temperature difference with the temperature of the first solution, so that side reactions can be avoided. Wherein the reaction time of the second solution and the first solution is 50-70 min.
And mixing the third solution and the Cs acid precursor for reaction, cooling in a water bath, and centrifuging to remove the supernatant to obtain a lower-layer substance. And the third solution and the Cs acid precursor react for 20-30 s.
CsPbBr generated by mixing and reacting third solution with Cs acid precursorxCl3-xThe transition metal manganese (Mn) and the rare earth metal thulium (Tm) are doped, the doped Mn can introduce a new potential well state, and partial excitons can be separated from the host perovskite CsPbBrxCl3-xIs transferred to the potential well state of Mn and transits downwards by the energy level of Mn: (4T1-6T1) And orange light of about 600nm is emitted. Host perovskite CsPbBrxCl3-xBluish green light (about 491nm), and the host perovskite CsPbBr is regulated by HBrxCl3-xThe halogen is used for coordinating the two light proportions, namely, the white light emission can be realized by internal mixing. And whereinThe rare earth element Tm also introduces a new potential well state, and the Tm potential well state acts to promote exciton dissociation from the host perovskite CsPbBrxCl3-xTransfer to the potential well state of Mn, and simultaneously improve the quantum yield.
The inert gas atmosphere in the present embodiment includes, but is not limited to, an argon atmosphere and a nitrogen atmosphere.
In addition, the centrifugation step of the present embodiment includes centrifuging the mixture produced by the reaction of the third solution and the Cs acid precursor a plurality of times. Wherein the mixture comprises white perovskite generated by reaction and unreacted oleic acid, oleylamine and octadecene.
Removal of the supernatant removes unreacted oleic acid, oleylamine and octadecene by a first centrifugation treatment. And dispersing the lower-layer substance from which the supernatant is removed in toluene, cleaning the white-light perovskite again by using the toluene, centrifuging again, collecting the lower-layer substance, and centrifuging for multiple times to obtain the liquid white-light perovskite with a single substance.
And drying the liquid white perovskite with a single substance at the temperature of 45-50 ℃ for 5-7 h to obtain the white perovskite fluorescent powder. Tests prove that the white-light perovskite prepared by the method has high white-light quantum yield which can reach 54 percent at most
An LED device comprises an LED chip and a coating coated on the surface of the LED chip, wherein the coating is obtained by coating the white perovskite on the surface of the LED chip.
Specifically, in the embodiment, the white perovskite powder is coated on the surface of the LED chip through the AB glue, so that the LED device emitting pure white light can be prepared. The embodiment is not limited to the coating with the AB paste, and the coating with the uv curable paste may be applied as long as the white perovskite powder can be applied to the LED surface.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
(1) 0.8g of CsCO340mL of octadecene and 2.5 mmL of oleic acid were placed in a 100mmL three-necked flask and heated under an argon atmosphereReacting for 1h at 120 ℃, then heating the solution to 150 ℃, and preserving the temperature for ten minutes to form a Cs acid precursor.
(2) 0.3mmol of PbBr20.3mmol of MnCl21mmL of oleic acid, 1mmL of oleylamine, 25ul of HBr and 10mL of octadecene are placed in a 100mmL three-necked flask, and the mixture is heated to 120 ℃ under the argon atmosphere to react for 1h to obtain a first solution.
(3) 0.3mmol of TmCl3And 10mL of octadecene were placed in a 100mmL three-necked flask, and heated to 160 ℃ under an argon atmosphere to react for 1 hour to obtain a second solution.
(4) And cooling the second solution to 120 ℃, then quickly injecting the second solution into the first solution by using an injector, and mixing and reacting for 1h to obtain a third solution.
(5) Quickly injecting 1mLCs acid precursor solution into the third solution, reacting for 25s, quickly cooling to room temperature in a water bath, and collecting by using a centrifugal tube;
(6) centrifuging the collected solution at 10000r/min, removing supernatant, and dispersing the lower layer substance in 10mmL toluene.
Centrifuging the lower layer substance dispersed in toluene at 10000r/min, collecting the lower layer substance, and dispersing in 10mmL toluene;
centrifuging the lower-layer substance dispersed in the toluene at the rotating speed of 10000r/min, removing supernatant, collecting the lower-layer substance, and drying in a vacuum drying oven at 50 ℃ for 6 hours to obtain the single-substance white-light perovskite fluorescent powder.
Example 2
(1) 0.7g of CsCO3Putting 38mL of octadecene and 2.5 mmL of oleic acid into a 100mmL three-necked flask, heating to 115 ℃ under the argon atmosphere, reacting for 1h, heating the solution to 145 ℃, and preserving the temperature for ten minutes to form a Cs acid precursor.
(2) 0.4mmol of PbBr20.3mmol of MnCl21mmL of oleic acid, 1mmL of oleylamine, 25ul of HBr and 10mL of octadecene were placed in a 100mmL three-necked flask, and heated to 115 ℃ under an argon atmosphere to react for 1 hour to obtain a first solution.
(3) Adding 0.3mmol of TmBr3And 10mL of octadecene were placed in a 100mmL three-necked flask under an argon atmosphereHeating to 155 ℃ under the surrounding conditions, and reacting for 1h to obtain a second solution.
(4) And cooling the second solution to 120 ℃, then quickly injecting the second solution into the first solution by using an injector, and mixing and reacting for 50min to obtain a third solution.
(5) Quickly injecting 1mLCs acid precursor solution into the third solution, reacting for 25s, quickly cooling to room temperature in a water bath, and collecting by using a centrifugal tube;
(6) centrifuging the collected solution at 10000r/min, removing supernatant, and dispersing the lower layer substance in 10mmL toluene.
Centrifuging the lower layer substance dispersed in toluene at 10000r/min, collecting the lower layer substance, and dispersing in 10mmL toluene;
centrifuging the lower-layer substance dispersed in the toluene at the rotating speed of 10000r/min, removing supernatant, collecting the lower-layer substance, and drying in a vacuum drying oven at 45 ℃ for 6 hours to obtain the single-substance white-light perovskite fluorescent powder.
Example 3
(1) 0.9g of CsCO3Putting 42mL of octadecene and 2.5 mmL of oleic acid into a 100mmL three-necked flask, heating to 125 ℃ under the argon atmosphere, reacting for 1h, heating the solution to 155 ℃, and preserving the temperature for ten minutes to form a Cs acid precursor.
(2) 0.5mmol of PbBr20.3mmol of MnCl21mmL of oleic acid, 1mmL of oleylamine, 25ul of HBr and 10mL of octadecene are placed in a 100mmL three-necked flask, and the mixture is heated to 125 ℃ under the argon atmosphere to react for 1h to obtain a first solution.
(3) 0.3mmol of TmCl3And 10mL of octadecene were placed in a 100mmL three-necked flask, and heated to 165 ℃ under an argon atmosphere to react for 1 hour to obtain a second solution.
(4) And cooling the second solution to 125 ℃, then quickly injecting the second solution into the first solution by using an injector, and mixing and reacting for 70min to obtain a third solution.
(5) Quickly injecting 1mLCs acid precursor solution into the third solution, reacting for 25s, quickly cooling to room temperature in a water bath, and collecting by using a centrifugal tube;
(6) centrifuging the collected solution at 10000r/min, removing supernatant, and dispersing the lower layer substance in 10mmL toluene.
Centrifuging the lower layer substance dispersed in toluene at 10000r/min, collecting the lower layer substance, and dispersing in 10mmL toluene;
centrifuging the lower-layer substance dispersed in the toluene at the rotating speed of 10000r/min, removing supernatant, collecting the lower-layer substance, and drying in a vacuum drying oven at 50 ℃ for 6 hours to obtain the single-substance white-light perovskite fluorescent powder.
Example 4
(1) 0.8g of CsCO3Placing 36mL of octadecene and 2.5 mmL of oleic acid in a 100mmL three-necked flask, heating to 125 ℃ under the argon atmosphere, reacting for 1h, heating the solution to 150 ℃, and preserving the temperature for ten minutes to form a Cs acid precursor.
(2) 0.6mmol of PbBr20.3mmol of MnCl21mmL of oleic acid, 1mmL of oleylamine, 25ul of HBr and 10mL of octadecene are placed in a 100mmL three-necked flask, and the mixture is heated to 120 ℃ under the argon atmosphere to react for 1h to obtain a first solution.
(3) Adding 0.3mmol of TmI3And 10mL of octadecene were placed in a 100mmL three-necked flask, and heated to 160 ℃ under an argon atmosphere to react for 1 hour to obtain a second solution.
(4) And cooling the second solution to 120 ℃, then quickly injecting the second solution into the first solution by using an injector, and mixing and reacting for 1h to obtain a third solution.
(5) Quickly injecting 1mLCs acid precursor solution into the third solution, reacting for 25s, quickly cooling to room temperature in a water bath, and collecting by using a centrifugal tube;
(6) centrifuging the collected solution at 10000r/min, removing supernatant, and dispersing the lower layer substance in 10mmL toluene.
Centrifuging the lower layer substance dispersed in toluene at 10000r/min, collecting the lower layer substance, and dispersing in 10mmL toluene;
centrifuging the lower-layer substance dispersed in the toluene at the rotating speed of 10000r/min, removing supernatant, collecting the lower-layer substance, and drying in a vacuum drying oven at 48 ℃ for 6 hours to obtain the single-substance white-light perovskite fluorescent powder.
Test examples
(1) The quantum yield of the white perovskite fluorescent powder prepared in examples 1 to 4 was measured by a quantum yield measuring instrument, and the measurement results are shown in table 1.
TABLE 1 Quantum yields of white perovskite phosphors of examples 1-4
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Quantum yield | 54％ | 52％ | 52％ | 53％ |
(2) The white perovskite phosphor prepared in example 1 was detected in a spectrometer, and the resulting spectrum is shown in fig. 1.
And (4) analyzing results: as can be seen from the spectrum diagram of fig. 1, the spectrum diagram is a spectrum of white light. And pouring the spectrogram into an analytical instrument for measurement and calculation, wherein the color coordinates corresponding to the obtained spectrum are (0.34,0.33), the color temperature is 5600k, and the obtained spectrum is standard normal white light. The white perovskite phosphor prepared in the example 1 can display white light.
In summary, the first embodiment of the present inventionThe prepared white perovskite can realize white light emission, and the Tm potential well state can promote excitons from the main perovskite CsPbBrxCl3-xTransfer to the potential well state of Mn, and simultaneously improve the quantum yield.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of white perovskite is characterized by comprising the following steps:
mixing CsCO3Mixing with octadecene and oleic acid, heating to 115-125 ℃ in an inert gas atmosphere for reaction, heating to 145-155 ℃, and preserving heat to obtain a Cs acid precursor;
reacting PbBr2、 MnCl2Mixing oleic acid, oleylamine, HBr and octadecene, and heating to 115-125 ℃ in an inert gas atmosphere to react to obtain a first solution; wherein, PbBr2The ratio of HBr to HBr is 0.3mmol: 25. mu.L, 0.4mmol: 25. mu.L, 0.5mmol: 25. mu.L or 0.6mmol: 25. mu.L;
mixing thulium halide and octadecene, heating to 155-165 ℃ in an inert gas atmosphere, and reacting to obtain a second solution;
reducing the temperature of the second solution to 115-125 ℃, and mixing the second solution with the first solution for reaction to obtain a third solution; and mixing the third solution and the Cs acid precursor for reaction, cooling in a water bath, and centrifuging to remove the supernatant to obtain a lower-layer substance.
2. The method of preparing the white-light perovskite of claim 1, wherein the centrifuging step comprises centrifuging the mixture of the third solution and the Cs acid precursor a plurality of times.
3. The method for producing a white perovskite according to claim 2, wherein the lower layer material obtained after each centrifugation of the mixture is dispersed in toluene.
4. The method for preparing the white perovskite as claimed in any one of claims 1 to 3, wherein the lower layer material is dried at 45-50 ℃ to obtain the white perovskite fluorescent powder.
5. The method of preparing a white-light perovskite of claim 1, wherein the thulium halide comprises TmCl3、TmBr3Or TmI3。
6. The method for preparing white perovskite according to claim 1, wherein CsCO is added to the solution3The ratio of the octadecene to the total amount of octadecene is 0.7-0.9 g/36-42 mL.
7. The method of preparing a white perovskite as claimed in claim 1 wherein the PbBr is2With MnCl2The molar ratio of (A) to (B) is 1-2: 1.
8. The method for preparing the white perovskite according to claim 1, wherein the reaction time of the second solution and the first solution is 50-70 min.
9. A white perovskite produced by the method for producing a white perovskite according to any one of claims 1 to 8.
10. An LED device comprising an LED chip and a coating applied to a surface of the LED chip, wherein the coating is obtained by applying the white perovskite of claim 9 to the surface of the LED chip.
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| CN107189778A (en) * | 2017-06-08 | 2017-09-22 | 东南大学 | A kind of method for the additive Mn perovskite quantum dot for preparing high-brightness white-light transmitting |
| CN108117870A (en) * | 2017-12-18 | 2018-06-05 | 吉林师范大学 | A kind of method for improving manganese and mixing perovskite quantum dot light emitting thermal stability |
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| CN107189778A (en) * | 2017-06-08 | 2017-09-22 | 东南大学 | A kind of method for the additive Mn perovskite quantum dot for preparing high-brightness white-light transmitting |
| CN108117870A (en) * | 2017-12-18 | 2018-06-05 | 吉林师范大学 | A kind of method for improving manganese and mixing perovskite quantum dot light emitting thermal stability |
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