CN107523296A - The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor - Google Patents
The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor Download PDFInfo
- Publication number
- CN107523296A CN107523296A CN201710690085.4A CN201710690085A CN107523296A CN 107523296 A CN107523296 A CN 107523296A CN 201710690085 A CN201710690085 A CN 201710690085A CN 107523296 A CN107523296 A CN 107523296A
- Authority
- CN
- China
- Prior art keywords
- silicon dioxide
- dioxide microsphere
- composite phosphor
- big yield
- halogen perovskite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C211/00—Compounds containing amino groups bound to a carbon skeleton
- C07C211/01—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms
- C07C211/02—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C211/03—Monoamines
- C07C211/04—Mono-, di- or tri-methylamine
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C257/00—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines
- C07C257/10—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines with replacement of the other oxygen atom of the carboxyl group by nitrogen atoms, e.g. amidines
- C07C257/12—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines with replacement of the other oxygen atom of the carboxyl group by nitrogen atoms, e.g. amidines having carbon atoms of amidino groups bound to hydrogen atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention provides a kind of one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor, comprise the following steps：By amidized silicon dioxide microsphere, lead halide or tin halides, cesium carbonate or bromination methylamine or formamidine acetate and octadecylene are put into flask, surfactant is added thereto, surfactant is oleic acid or oleyl amine and the mixture of oleic acid same volume, it is placed on 150 300 DEG C, 1200r/min is stirred 5 10 minutes, then cools down 30s with ice-water bath；Composite phosphor luminescent properties prepared by the present invention are excellent, simple to operate, are produced on a large scale.
Description
Technical field
The invention belongs to photoelectron material preparation field, and in particular to a kind of big yield halogen perovskite/silica is micro-
The one-step method for synthesizing of ball composite phosphor.
Background technology
Ca-Ti ore type quantum dot or nano particle, as Ca-Ti ore type Organic leadP halogen compound (CH3NH3PbX3, X=F,
Cl, Br, I) or full-inorganic Ca-Ti ore type lead halide (CsPbX3, X=Cl, Br, I) due to its synthesize cost it is low, fluorescence efficiency
Height, the advantages such as luminous half-peak width and energy gap are adjustable, so as in solar cell, laser, photo-detector, light-emitting diodes
The neighborhoods such as pipe have potential application value (Nature 2013,499,316).Liu Ru Shi team finds perovskite fluorescence
Powder has very high stability and color saturation, is the potential competitor that novel backlight is shown
(Angew.Chem.Int.Ed.2016,55,7924–7929).But perovskite fluorescent material preparation process is complicated, need to first prepare calcium
Titanium ore is nanocrystalline, and fluorescent powder grain size is difficult to regulation and control and causes to excite not exclusively so that light efficiency reduces.The colour developing of device refers to
Number is relatively low, and fluorescence quantum efficiency is not high, and the optical attenuation of device is obvious.
The content of the invention
Technical problem：In order to solve the defects of prior art, the invention provides a kind of big yield halogen perovskite/dioxy
The one-step method for synthesizing of SiClx microballoon composite phosphor.
Technical scheme：The invention provides the conjunction of a step of big yield halogen perovskite/silicon dioxide microsphere composite phosphor
Into method, comprise the following steps：By amidized silicon dioxide microsphere, lead halide or tin halides, cesium carbonate under normal temperature condition
Or bromination methylamine or formamidine acetate and octadecylene are put into flask, then surfactant is added thereto, all substances need not
Further processing, protection gas then need not be added at 150-300 DEG C or is vacuumized, stirs 5-10 minutes, then use ice-water bath
Cooling；Amidized silicon dioxide microsphere, lead halide or the tin halides, cesium carbonate or bromination methylamine or formamidine acetate, 18
The amount ratio of alkene and surfactant is：0.3g：0.0834-0.1289g：0.0208-0.0336g：10-15ml：1-1.4ml.
By adjusting the content and ratio of cation type and halogen, it can obtain total visible light wave band and light；I ratio is got in raw material
Height, emission wavelength are longer；Cl content is higher in raw material, and emission wavelength is shorter；When halogen is pure Br, green light；Pass through tune
The content and ratio of whole halogen, can obtain 20-46nm halfwidth, and luminous efficiency is high.
Preferably：Surfactant is oleyl amine and/or oleic acid.
As further preferred scheme：The rotating speed of stirring is 1200r/min.
As further preferred scheme：The time of ice-water bath cooling is 30s.
As further preferred scheme：The oleyl amine and oleic acid volume ratio of addition are 1:1.
Beneficial effect：Composite phosphor luminescent properties prepared by the present invention are excellent, and nanocrystalline structure is perovskite knot
Structure, by the way that presoma and part are all blended in octadecylene solution without protective gas, thus it is simple to operate, it can advise
Modelling produces.
Brief description of the drawings
Fig. 1 is the fluorescence spectra of the composite phosphor prepared by 1-6 of the embodiment of the present invention；
Fig. 2 is the fluorescence spectra of the composite phosphor of other kind of cationoid prepared by 7-9 of the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
The present invention rather than limitation the scope of the present invention, after the present invention has been read, those skilled in the art are each to the present invention's
The modification of the kind equivalent form of value falls within the application appended claims limited range.
The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor, comprises the following steps：Will
Amidized silicon dioxide microsphere, lead halide or tin halides, cesium carbonate or bromination methylamine or formamidine acetate and octadecylene are put into burning
In bottle, surfactant is added thereto, surfactant is oleic acid or oleyl amine and the mixture of oleic acid same volume, in 150-
At 300 DEG C, rotating speed 1200r/min, 5-10 minutes are stirred, then cool down 30s with ice-water bath.
Amidized silicon dioxide microsphere, lead halide or tin halides, cesium carbonate or bromination methylamine or formamidine acetate, octadecylene
Amount ratio with surfactant is：0.3g：0.11g：0.02-0.03g：10-15ml：1-1.4ml.
Embodiment 1
The amidized silicon dioxide microsphere of 0.0326g cesium carbonates, 0.3g, 0.0834g lead chlorides are weighed, measures 15 milliliter ten
Eight alkene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, at 200 degrees celsius with 1200r/
Min rotating speed be stirred vigorously reaction 5 minutes after with ice-water bath cool down 30s.The luminous maximum luminous ripple of the composite phosphor of preparation
A length of 407nm, halfwidth 20nm, fluorescence quantum efficiency 11%.
Embodiment 2
Weigh the amidized silicon dioxide microsphere of 0.0326g cesium carbonates, 0.3g, 0.0417g lead chlorides, 0.055g brominations
Lead, measure 15 milliliters of octadecylenes, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, 200
After being stirred vigorously reaction 5 minutes under degree Celsius with 1200r/min rotating speed 30s is cooled down with ice-water bath.The composite phosphor of preparation
Luminous maximum emission wavelength be 463nm, halfwidth 28nm, fluorescence quantum efficiency 19%.
Embodiment 3
Weigh the amidized silicon dioxide microsphere of 0.0326g cesium carbonates, 0.3g, 0.0556g lead chlorides, 0.0367g brominations
Lead, measure 15 milliliters of octadecylenes, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, 200
After being stirred vigorously reaction 5 minutes under degree Celsius with 1200r/min rotating speed 30s is cooled down with ice-water bath.The composite phosphor of preparation
Luminous maximum emission wavelength be 487nm, halfwidth 22nm, fluorescence quantum efficiency 27%.
Embodiment 4
The amidized silicon dioxide microsphere of 0.0326g cesium carbonates, 0.3g, 0.1101g lead bromides are weighed, measures 15 milliliter ten
Eight alkene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, at 200 degrees celsius with 1200r/
Min rotating speed be stirred vigorously reaction 5 minutes after with ice-water bath cool down 30s.The luminous maximum luminous ripple of the composite phosphor of preparation
A length of 520nm, halfwidth 26nm, fluorescence quantum efficiency 56%.
Embodiment 5
Weigh the amidized silicon dioxide microsphere of 0.0326g cesium carbonates, 0.3g, 0.0691g lead iodides, 0.055g brominations
Lead, measure 15 milliliters of octadecylenes, 0.7 milliliter of oleyl amine, 0.7 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, 150
After being stirred vigorously reaction 5 minutes under degree Celsius with 1200r/min rotating speed 30s is cooled down with ice-water bath.The composite phosphor of preparation
Luminous maximum emission wavelength be 595nm, halfwidth 44nm, fluorescence quantum efficiency 38%.
Embodiment 6
Weigh the amidized silicon dioxide microsphere of 0.0326g cesium carbonates, 0.3g, 0.0922g lead chlorides, 0.0367g brominations
Lead, measure 15 milliliters of octadecylenes, 0.7 milliliter of oleyl amine, 0.7 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, 150
After being stirred vigorously reaction 5 minutes under degree Celsius with 1200r/min rotating speed 30s is cooled down with ice-water bath.The composite phosphor of preparation
Luminous maximum emission wavelength be 644nm, halfwidth 46nm, fluorescence quantum efficiency 35%.
Embodiment 7
0.0336g Diethylaminoethyls ammonium, the amidized silicon dioxide microspheres of 0.3g, 0.1101g lead bromides are weighed, measures 15 millis
Rise octadecylene, 1 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, with 1200r/min rotating speed under 150 degrees Celsius
It is stirred vigorously after reacting 5 minutes and cools down 30s with ice-water bath.The luminous maximum emission wavelength of the composite phosphor of preparation is 509nm.
Embodiment 8
The amidized silicon dioxide microsphere of 0.0208g formamidine acetates, 0.3g, 0.1101g lead bromides are weighed, measures 15 milliliters
Octadecylene, 1 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, it is acute with 1200r/min rotating speed under 150 degrees Celsius
Strong stirring reaction cools down 30s after 5 minutes with ice-water bath.The luminous maximum emission wavelength of the composite phosphor of preparation is 522nm.
Embodiment 9
The amidized silicon dioxide microsphere of 0.1127g stannic iodides, 0.3g, 0.0261g cesium carbonates are weighed, measures 10 milliliter ten
Eight alkene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid.It is fitted into after above-mentioned raw materials are mixed in flask, at 300 degrees Celsius with 1200r/
Min rotating speed be stirred vigorously reaction 10 minutes after with ice-water bath cool down 30s.The luminous maximum luminous ripple of the composite phosphor of preparation
A length of 620nm.
Table 1：The fluorescence parameter of composite phosphor prepared by embodiment 1-6：
Table 2：Fluorescence photo color of the composite phosphor under natural light and uviol lamp prepared by embodiment 1-6 is shown
As a result such as following table：
| Photo color under natural light | Photo color under uviol lamp | |
| Embodiment 1 | White | Lavender |
| Embodiment 2 | It is faint yellow | Blueness |
| Embodiment 3 | Yellow | Green |
| Embodiment 4 | It is faint yellow | Green |
| Embodiment 5 | It is coffee-like | It is orange-yellow |
| Embodiment 6 | Grey | It is red |
Composite phosphor luminescent properties prepared by the present invention are excellent, available for LED backlit display, white LED lamp illumination
And other photoelectric display fields.
Claims (5)
1. the one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor, it is characterised in that：This method
Comprise the following steps：By amidized silicon dioxide microsphere, lead halide or tin halides, cesium carbonate or bromination methylamine or formamidine acetate
It is put into octadecylene in flask, then adds surfactant thereto, 5-10 minutes is stirred at 150-300 DEG C, then use ice
Water-bath cooling；Amidized silicon dioxide microsphere, lead halide or the tin halides, cesium carbonate or bromination methylamine or formamidine acetate,
The amount ratio of octadecylene and surfactant is：0.3g：0.0834-0.1289g：0.0208-0.0336g：10-15ml：1-
1.4ml。
2. the one-step synthesis side of big yield halogen perovskite/silicon dioxide microsphere composite phosphor according to claim 1
Method, it is characterised in that：Surfactant is oleyl amine and/or oleic acid.
3. the one-step synthesis side of big yield halogen perovskite/silicon dioxide microsphere composite phosphor according to claim 1
Method, it is characterised in that：The rotating speed of stirring is 1200r/min.
4. the one-step synthesis side of big yield halogen perovskite/silicon dioxide microsphere composite phosphor according to claim 1
Method, it is characterised in that：The time of ice-water bath cooling is 30s.
5. the one-step synthesis side of big yield halogen perovskite/silicon dioxide microsphere composite phosphor according to claim 2
Method, it is characterised in that：The oleyl amine and oleic acid volume ratio of addition are 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710690085.4A CN107523296A (en) | 2017-08-14 | 2017-08-14 | The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710690085.4A CN107523296A (en) | 2017-08-14 | 2017-08-14 | The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107523296A true CN107523296A (en) | 2017-12-29 |
Family
ID=60681187
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710690085.4A Pending CN107523296A (en) | 2017-08-14 | 2017-08-14 | The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107523296A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531987A (en) * | 2018-03-30 | 2018-09-14 | 南京理工大学 | A kind of preparation method that halogen perovskite is nanocrystalline |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106634961A (en) * | 2016-12-19 | 2017-05-10 | 中央民族大学 | Organic-inorganic hybrid perovskite quantum dot and preparation method thereof |
| CN106675550A (en) * | 2016-11-18 | 2017-05-17 | 吉林大学 | Perovskite quantum dot gel and preparation method thereof |
-
2017
- 2017-08-14 CN CN201710690085.4A patent/CN107523296A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106675550A (en) * | 2016-11-18 | 2017-05-17 | 吉林大学 | Perovskite quantum dot gel and preparation method thereof |
| CN106634961A (en) * | 2016-12-19 | 2017-05-10 | 中央民族大学 | Organic-inorganic hybrid perovskite quantum dot and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| XIAOMING LI等: "Amino-Mediated Anchoring Perovskite Quantum Dots for Stable and Low-Threshold Random Lasing", 《ADV.MATER.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531987A (en) * | 2018-03-30 | 2018-09-14 | 南京理工大学 | A kind of preparation method that halogen perovskite is nanocrystalline |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2591943C2 (en) | Red light emitting luminescent materials | |
| CN105637063A (en) | Luminescent material, method for producing a luminescent material and use of a luminescent material | |
| JP5730286B2 (en) | Luminescent material based on Eu2 + (co) doped mixed garnet and its manufacture and use | |
| CN105018080B (en) | A kind of preparation method of specular removal fluorescent material | |
| CN105733572A (en) | Red fluoride fluorescent powder as well as preparation method and application thereof | |
| Ran et al. | Luminescence properties and energy transfer of CdWO4: Sm3+, Bi3+, M+ (M= Li, Na, K) phosphors for white LEDs | |
| Tian et al. | A new oxyapatite red phosphor Eu3+-doped Ca3Y7 (BO4)(SiO4) 5O: synthesis, structure and luminescence properties | |
| TW201000599A (en) | Green color fluorescent element | |
| CN108531987A (en) | A kind of preparation method that halogen perovskite is nanocrystalline | |
| CN106146519B (en) | Preparation, sign and the application of bivalent manganese fluorescent material of the one kind based on 1,4 diethyl of dibromo 1,4 diazabicylo [2.2.2] octane | |
| CN110066657B (en) | High-temperature luminescence enhanced rare earth lutetium-based molybdate material and preparation method thereof | |
| CN114958351A (en) | Ultraviolet excited bluish violet fluorescent powder, preparation method and luminescent device | |
| CN110878206A (en) | Eu (Eu)3+Rare earth doped lutetium-based tungsten molybdate material and preparation method thereof | |
| CN107523296A (en) | The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor | |
| KR101098337B1 (en) | Process for preparing molybdate based red light emitting fluorescent material | |
| CN110003908A (en) | White light LEDs silicate red fluorescent powder and preparation method and White LED light-emitting device | |
| Yingli et al. | High thermal stability and quantum yields of green-emitting Sr3Gd2 (Si3O9) 2: Tb3+ phosphor by co-doping Ce3+ | |
| Rudnicka et al. | Preliminary spectroscopic properties of K4SrSi3O9 doped with Eu3+ | |
| CN112608742A (en) | beta-Al activated by europium2O3Defect structure blue fluorescent powder and preparation method thereof | |
| CN106753346B (en) | Nitrogen oxides fluorophor and its luminescent device | |
| CN110527508A (en) | A kind of nitride red fluorescent powder for white light LED and preparation method thereof | |
| shan Wang et al. | Effect of flux on the composition and luminescent properties of Ca0. 68Mg0. 2SiO3: 0.12 Eu3+ red phosphor | |
| CN108794465A (en) | Manganese chloride fluorescent chemicals and its preparation based on 1- isopropyl -1- azabicyclics [2.2.2] octane and application | |
| CN110982519A (en) | Carbon nano-dot composite fluorescent powder and preparation method and application thereof | |
| CN107312529B (en) | Narrow half-peak-width green silicate fluorescent powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171229 |