CN112480913A - Silver-sodium mixed double perovskite alloy nano crystal material and preparation and application thereof - Google Patents
Silver-sodium mixed double perovskite alloy nano crystal material and preparation and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000000956 alloy Substances 0.000 title claims abstract description 28
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 28
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 26
- KIIUTKAWYISOAM-UHFFFAOYSA-N silver sodium Chemical compound [Na].[Ag] KIIUTKAWYISOAM-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011734 sodium Substances 0.000 claims abstract description 15
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical compound CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 9
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000005642 Oleic acid Substances 0.000 claims abstract description 7
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000460 chlorine Substances 0.000 claims abstract description 7
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000000084 colloidal system Substances 0.000 claims abstract description 6
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims abstract description 6
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229940071536 silver acetate Drugs 0.000 claims abstract description 6
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 6
- 239000001632 sodium acetate Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000002086 nanomaterial Substances 0.000 claims description 11
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 6
- -1 silver ions Chemical class 0.000 claims description 5
- ZOAIGCHJWKDIPJ-UHFFFAOYSA-M caesium acetate Chemical compound [Cs+].CC([O-])=O ZOAIGCHJWKDIPJ-UHFFFAOYSA-M 0.000 claims description 4
- 229910001415 sodium ion Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000006862 quantum yield reaction Methods 0.000 claims description 3
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 3
- WFSGQBNCVASPMW-UHFFFAOYSA-N 2-ethylhexanoyl chloride Chemical compound CCCCC(CC)C(Cl)=O WFSGQBNCVASPMW-UHFFFAOYSA-N 0.000 claims description 2
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 claims description 2
- 238000005401 electroluminescence Methods 0.000 claims description 2
- 229940049964 oleate Drugs 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000002707 nanocrystalline material Substances 0.000 claims 5
- 238000004519 manufacturing process Methods 0.000 claims 4
- 229910052738 indium Inorganic materials 0.000 claims 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- 230000005622 photoelectricity Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000005046 Chlorosilane Substances 0.000 description 4
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
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Abstract
The invention discloses a series of non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal materials, which comprise the steps of adding a cesium-containing compound, sodium acetate, silver acetate and indium acetate into a flask, adding 1-octadecene, oleic acid and oleylamine, stirring and mixing, and vacuumizing for 1h at 105 ℃; introducing nitrogen, heating to 185 ℃ at the temperature of 5 ℃/min, injecting a chlorine-containing compound at the temperature of 170 ℃, quickly carrying out ice bath to room temperature when the temperature reaches 185 ℃, centrifuging to remove supernatant, washing for 2 times by using toluene, centrifuging to remove supernatant, dispersing precipitate into n-hexane, centrifuging to remove precipitate, and obtaining the nanocrystal colloid. The preparation method is simple, solves the problem of toxicity of lead-based perovskite, improves the stability of perovskite nanocrystals, improves the fluorescence performance by regulating the ratio of sodium to silver, and has good application prospect in the field of photoelectricity.
Description
Technical Field
The invention belongs to the technical field of light emitting diodes, and particularly relates to synthesis and application of a novel light emitting diode nano luminescent material.
Background
Lead-based perovskite nanocrystal materials have good photoelectric properties and high fluorescence quantum yield, and have been used in the fields of light emitting diode preparation, laser preparation and the like. However, its toxicity and instability severely restrict its large-scale application. Therefore, the high-efficiency non-lead perovskite nano luminescent material is widely concerned by researchers all over the world.
Therefore, the use of non-toxic or low-toxic non-lead elements instead of lead for environmental friendliness and sustainable development is a necessary trend in the development of perovskite materials. In the non-lead perovskite ore, the double perovskite has potential application prospect due to excellent photoelectric property, three-dimensional structure and good stability. However, no lead-free all-inorganic silver-sodium-based double perovskite alloy nano material is reported at present.
Disclosure of Invention
The invention aims to provide a series of non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal materials and a preparation method thereof.
A series of non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal materials are characterized in that the chemical formula of the double perovskite alloy nano material is Cs2Na1-xAgxInCl6The double perovskite alloy nano material is prepared by substituting silver ions for sodium ions and still has a face-centered cubic structure.
The variable temperature thermal injection preparation method of the series of non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal materials comprises the following steps:
adding cesium compound, sodium acetate, silver acetate and indium acetate into a 50ml flask according to required amount, adding 1-octadecene, oleic acid and oleylamine, stirring and mixing, and vacuumizing at the temperature of 105-115 ℃ for 40-90 min; introducing nitrogen, heating to 180-200 ℃ at 4-8 ℃/min, injecting a chlorine-containing compound at 170 +/-5 ℃, rapidly performing ice bath when the temperature reaches 180-200 ℃, and cooling to room temperature; centrifuging at 9000 + -1500 rpm for 5-30 min to remove supernatant, washing with toluene for 1-4 times, centrifuging at 10000 + -500 rpm for 10 + -6 min to remove supernatant, dispersing precipitate in n-hexane, centrifuging at 6000 + -1000 rpm for 10 + -6 min to remove precipitate to obtain Cs2Na1-xAgxInCl6A nanocrystalline colloid.
The reaction temperature used in the preparation process is a gradient temperature changing process and a temperature changing thermal injection process.
The cesium-containing compound used in the preparation process is one of cesium acetate or cesium oleate.
The chlorine-containing compound used in the preparation process is one of trimethylchlorosilane, benzoyl chloride or 2-ethylcaproyl chloride.
The preparation process comprises the following steps: 0.5mmol Cs per synthesis2Na1-xAgxInCl6Nanocrystals required 10ml of 1-octadecene, 2.9ml of oleic acid, 0.65ml of oleylamine.
The side length of the nano material is 12 +/-5 nm, the optical band gap is 4.2eV, and the nano material can be used as a photosensitive material and is suitable for an ultraviolet photoelectric detector.
In the nanomaterial, silver ions occupy lattice sites of sodium ions, and the sodium ions and the silver ions can be substituted in any ratio.
The material has strong orange fluorescence at room temperature, has a wide fluorescence peak, has a peak center position of 540 +/-5 nm, can be used as orange fluorescent powder, and is suitable for forming a white light emitting diode with a blue light material.
The fluorescence quantum yield of the material is as high as 14%, and the material can be used as a luminescent material for electroluminescence in a light-emitting diode.
The material can be stable for more than 1 month at both 25 ℃ and 55% relative humidity.
Has the advantages that: the invention provides a series of non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal materials, and silver element replaces partial sodium element, so that the prepared three-dimensional non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal has strong orange fluorescence, excellent stability and good photoelectric application prospect.
The preparation method is simple, solves the problem of toxicity of lead-based perovskite, improves the stability of perovskite nanocrystals, improves the fluorescence performance by regulating the ratio of sodium to silver, and has good application prospect in the field of photoelectricity.
Drawings
FIG. 1 is a powder XRD diffraction spectrum of three non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal materials of the invention.
FIG. 2 is a Transmission Electron Microscope (TEM) picture of a non-lead all-inorganic silver-sodium mixed double perovskite alloy nano-crystal material of the invention.
FIG. 3 shows the ultraviolet-visible absorption spectrum and the room temperature stable fluorescence spectrum of three non-lead all-inorganic silver-sodium mixed double perovskite alloy nano-crystal materials of the invention.
FIG. 4 is a picture of a non-lead all-inorganic silver-sodium mixed double perovskite alloy nanocrystal colloid according to the present invention.
Detailed Description
The invention is further described with reference to the accompanying drawings and specific embodiments:
example 1
Adding 115.2mg of cesium acetate, 9.2mg of sodium acetate, 56.4mg of silver acetate and 146.0mg of indium acetate into a 50ml flask, adding 10ml of 1-octadecene, 2.9ml of oleic acid and 0.65ml of oleylamine, stirring and mixing, and vacuumizing for 1h at 106 ℃; introducing nitrogen, heating to 190 ℃ at the temperature of 6 ℃/min, injecting 0.4ml of trimethylchlorosilane at the temperature of 175 ℃, rapidly carrying out ice bath when the temperature reaches 190 ℃, cooling to room temperature, centrifuging for 10 minutes at 9000 +/-1000 r/min to remove supernatant, washing for 2 times with toluene, centrifuging for 5 minutes at 10000 r/min to remove supernatant, dispersing precipitate into n-hexane, centrifuging for 5 minutes at 6000 r/min to remove precipitate to obtain Cs2Na0.25Ag0.75InCl6A nanocrystalline colloid.
Through a powder XRD diffraction test, as shown in figure 1, the obtained non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal material has high crystallinity, is a single pure phase and has an obvious face-centered cubic structure.
EXAMPLE 2
Adding 115.2mg of cesium acetate, 27.7mg of sodium acetate, 18.8mg of silver acetate and 146.0mg of indium acetate into a 50ml flask, adding 10ml of 1-octadecene, 2.9ml of oleic acid and 0.65ml of oleylamine, stirring and mixing, and vacuumizing at 105 ℃ for 1 hour; introducing nitrogen, heating to 190 deg.C at 6 deg.C/min, and injecting 0.4ml trimethyl chloride at 175 deg.CQuick ice-bath is carried out on the chlorosilane when the temperature reaches 190 ℃, the chlorosilane is cooled to the room temperature, the chlorosilane is centrifuged for 10 minutes at 9000 +/-1000 r/min to remove supernatant, then the chlorosilane is washed for 2 times by toluene, centrifuged for 5 minutes at 10000 r/min to remove supernatant, then the precipitate is dispersed into n-hexane, and centrifuged for 5 minutes at 6000 r/min to remove the precipitate to obtain Cs2Na0.75Ag0.25InCl6A nanocrystalline colloid.
Through a powder XRD diffraction test, as shown in figure 1, the obtained non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal material has high crystallinity, is a single pure phase and has an obvious face-centered cubic structure.
Through the test of a transmission electron microscope, as shown in figure 2, the obtained non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal material has uniform particle size distribution and side length of about 12 nm.
Through an ultraviolet-visible absorption test and a steady-state fluorescence test, as shown in fig. 3, the obtained non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal material has a wider fluorescence emission spectrum. As shown in FIG. 4, Cs2Na0.75Ag0.25InCl6The nanocrystals emitted an orange fluorescent picture under an ultraviolet lamp at 254 nm.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are merely illustrative and not restrictive, and all technical solutions obtained by means of equivalents and equivalent changes fall within the protection scope of the present invention.
Claims (10)
1. A silver-sodium mixed double perovskite alloy nano crystal material is a series of non-lead all-inorganic silver-sodium mixed double perovskite alloy nano crystal materials, and is characterized in that: the chemical formula of the double perovskite alloy nano material is Cs2Na1-xAgxInCl6Nanocrystals having a face-centered cubic structure with 0.1 < x ≦ 0.95, preferably 0.25.
2. The double perovskite alloy nanocrystalline material of claim 1, wherein: the side length of the nano material is 12 +/-5 nm, and the double perovskite alloy nano material has a face-centered cubic structure, and silver ions replace sodium ions.
3. A method of preparing a double perovskite alloy nanocrystalline material according to claim 1 or 2, characterized in that the following steps are carried out:
adding a cesium-containing compound, sodium acetate, silver acetate and indium acetate into a reaction vessel according to required amounts, adding 1-octadecene, oleic acid and oleylamine, stirring and mixing, and vacuumizing at the temperature of 105-115 ℃ for 40-90 min;
introducing nitrogen, heating to 180-class 200 ℃ from room temperature at 4-8 ℃/min, injecting a chlorine-containing compound at 165-class 175 ℃, cooling the reaction container to room temperature in an ice bath when the temperature reaches 180-class 200 ℃;
(III) centrifuging at 9000 +/-1500 rpm for 5-30 minutes to remove supernatant, washing the precipitate with toluene for 1-4 times, centrifuging at 10000 +/-500 rpm for 10 +/-6 minutes to remove supernatant, dispersing the precipitate in n-hexane, centrifuging at 6000 +/-1000 rpm for 10 +/-6 minutes to remove precipitate, and obtaining Cs2Na1-xAgxInCl6A nanocrystalline colloid.
4. The production method according to claim 3, characterized in that: the cesium-containing compound used in the preparation process is one or more than two of cesium acetate or cesium oleate.
5. The production method according to claim 3, characterized in that: the chlorine-containing compound used in the preparation process is one or more than two of trimethylchlorosilane, benzoyl chloride or 2-ethylcaproyl chloride.
6. The production method according to claim 3, characterized in that: in the preparation process, 0.5mmol Cs is synthesized2Na1- xAgxInCl6Nanocrystals required 12 + -3 ml 1-octadecene, 3 + -0.2 ml oleic acid, 0.8 + -0.2 ml oleylamine.
7. The production method according to any one of claims 3 to 6, characterized in that: the mol dosage ratio of the cesium-containing compound, sodium acetate, silver acetate, indium acetate and the chlorine-containing compound calculated by Cs, (Na + Ag), In and Cl is (1-1.6), (0.8-1) and (8-16), wherein Na/(Na + Ag) is more than or equal to 0.05 and less than 0.9.
8. Use of a double perovskite alloy nanocrystalline material according to claim 1 or 2, characterized in that: the side length of the nano material is 12 +/-5 nm, the optical band gap is 4.2eV, and the nano material can be used as a photosensitive material and is suitable for an ultraviolet photoelectric detector.
9. Use of a double perovskite alloy nanocrystalline material according to claim 1 or 2, characterized in that: the material has strong orange fluorescence at room temperature, has a wide fluorescence peak (400-.
10. Use of a double perovskite alloy nanocrystalline material according to claim 1 or 2, characterized in that: the fluorescence quantum yield of the material is as high as 14%, and the material can be used as a luminescent material for electroluminescence in a light-emitting diode.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072933A (en) * | 2021-04-08 | 2021-07-06 | 南京理工大学 | Non-lead all-inorganic indium-based zero-dimensional perovskite nanocrystal and preparation method thereof |
| CN113088282A (en) * | 2021-04-08 | 2021-07-09 | 南京理工大学 | Non-lead all-inorganic indium-based zero-dimensional perovskite nanocrystal containing coordinated water and preparation method |
| CN115490259A (en) * | 2022-10-24 | 2022-12-20 | 吉林大学 | Inorganic non-lead perovskite nanocrystal with high fluorescence efficiency and preparation method thereof |
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| CN115490259B (en) * | 2022-10-24 | 2023-06-23 | 吉林大学 | Inorganic lead-free perovskite nanocrystalline with high fluorescence efficiency and preparation method thereof |
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