CN106947477B - Mn-CsPbCl3Preparation method of nanometer rods and products thereof and application - Google Patents
Mn-CsPbCl3Preparation method of nanometer rods and products thereof and application Download PDFInfo
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- 238000000034 method Methods 0.000 title description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 29
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 29
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 29
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000005642 Oleic acid Substances 0.000 claims abstract description 29
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 29
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 12
- -1 octadecylene Chemical group 0.000 claims abstract description 12
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 11
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012697 Mn precursor Substances 0.000 claims abstract description 10
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910000024 caesium carbonate Inorganic materials 0.000 claims abstract description 5
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000011565 manganese chloride Substances 0.000 claims abstract description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000002096 quantum dot Substances 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 239000012298 atmosphere Substances 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000013507 mapping Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 210000005252 bulbus oculi Anatomy 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The present invention relates to Mn-CsPbCl3Cesium carbonate is added in octadecylene and oleic acid mixture the preparation method of nanometer rods, heats and oleic acid caesium solution is made, by PbCl2And MnCl2·4H2Octadecylene, oleic acid and oleyl amine is added in O, is heated to 120 DEG C, it is kept for 30 minutes, increases the temperature to 165 DEG C, kept for 10 minutes, 200 DEG C are heated to, oleic acid and oleyl amine are added, until solution side is clarified, Pb/Mn precursor solution is formed, oleic acid caesium solution is injected into Pb/Mn precursor solution, 0 DEG C of ice bath is cooling, centrifugation, toluene washing, in triplicate, obtains Mn-CsPbCl3Nanometer rods.The technical program preparation method is easy to operate, and nanometer rods fluorescence efficiency is high, and crystal property is good and has biggish Stokes shift.
Description
Technical field
The invention belongs to nano material field of luminescent technology, in particular to Mn-CsPbCl3The preparation method of nanometer rods and its
Product and application.
Background technique
Semiconductor nano attracts numerous due to superior functions such as superpower luminescent properties and adjustable forbidden bandwidths
The eyeball of person, and perovskite nanocrystal has potential application value in photoelectric field with its unique optical property.Transition
Metal-doped semiconductor-quantum-point be improve semiconductor optics and electromagnetic performance pass through frequently with method.Such as D.D.Sarma
Group carries out additive Mn to zinc selenide, realizes the Effective Regulation of spectrum.Recently Matthew Sheldon group is prepared for photic
The Mn adulterated with Ca and Ti ore quantum dot of luminous efficiency.The optically and electrically performance of nano material is substantially better than body material, and controls and close
At the nano material (zero dimension, peacekeeping two dimension) of more high quality and controlled morphologies, and in micro- laser field, nanometer rods are opposite
For quantum dot, it is easier to form resonant cavity, and nanometer stick array is applied in LED, carrier transport faster, Ke Yizeng
The luminous efficiency of strong LED, nanometer rods not only facilitate basic research, and expand applications to nanostructures prospect.
Nowadays a kind of method is provided to prepare the Mn of high fluorescence efficiency and adulterate CsPbCl3Nanometer rods, method is simple, knot
Crystalline substance is good, and photoluminescence efficiency is high, and Stokes shift is big, and there is presently no one-dimensional Mn to adulterate CsPbCl3The phase of nanometer rods
Close report.
Summary of the invention
In view of this, the purpose of the present invention is to provide Mn-CsPbCl3Preparation method of nanometer rods and products thereof.
In order to achieve the above objectives, the invention provides the following technical scheme:
The preparation method of Mn-CsPbCl3 nanometer rods, includes the following steps:
(1) cesium carbonate is added in octadecylene and oleic acid mixture, is heated to 120 DEG C under nitrogen atmosphere, oleic acid is made
Caesium solution；
It (2) is the PbCl of 1:0.8~1.2 by mass ratio2And MnCl2·4H2O sequentially adds octadecylene, oleic acid and oleyl amine,
It stirs 10 minutes under nitrogen atmosphere, is heated to 120 DEG C, kept for 30 minutes, be heated to 165 DEG C, kept for 10 minutes, be denoted as A
Solution；
(3) step (2) described solution A is heated to 200 DEG C, adds oleic acid and oleyl amine, until solution side is clarified, formed
Pb/Mn precursor solution；
(4) the resulting oleic acid caesium solution of step (1) is injected into the resulting Pb/Mn precursor solution of step (3), 0 DEG C
Ice bath is cooling, and centrifugation, sediment is dispersed with toluene, is centrifuged again, in triplicate, obtains Mn-CsPbCl3Nanometer rods.
Further, the mass volume ratio (mg:ml:ml) of cesium carbonate, octadecylene and oleic acid described in step (1) is 100:4:
0.6；
Further, PbCl described in step (2)2, octadecylene, oleic acid and oleyl amine quality volume (mg:ml:ml:ml) ratio be
100:8:0.8:1.3；
Further, oleic acid described in step (3) and oleyl amine are added volume and are added respectively with oleic acid in step (2) and oleyl amine
Volume is equal；
Further, step (4) the oleic acid caesium and Pb/Mn precursor solution volume ratio are 1:20；
Further, step (4) centrifugal condition is that 8000rpm is centrifuged 5 minutes；
The Mn-CsPbCl3 nanometer rods obtained by above-described preparation method.
Mn-CsPbCl3Nanometer rods are preparing the application in solar battery, light emitting diode with quantum dots or laser.
The beneficial effects of the present invention are: 1, the preparation method is that a kind of simple hot injection reaction method, operation
Simply.2, which is up to 50%, and crystal property is good and has biggish Stokes shift, such as Fig. 2 and 3
It is shown, there is excellent optical property, in solar battery, is with a wide range of applications in terms of light emitting diode and micro- laser.
It is very promising to large-scale production 3. used pre-reaction material is very economical in preparation method reaction.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is Mn-CsPbCl3Perovskite nanometer rods are scattered in n-hexane photo (a) under fluorescent light and its ultraviolet
(λ=365nm) photo (b) under lamp；
Fig. 2 is Mn-CsPbCl3The luminescence generated by light photo of perovskite nanometer rods；
Fig. 3 is Mn-CsPbCl3The absorption spectrum photo of perovskite nanometer rods；
Fig. 4 is Mn-CsPbCl3The XRD photo of perovskite nanometer rods；
Fig. 5 is Mn-CsPbCl3The stereoscan photograph of perovskite nanometer rods；
Fig. 6 is Mn-CsPbCl3The scanning electron microscope mapping photo of perovskite nanometer rods；
Wherein:
A figure is SEM figure in Fig. 6, and Elemental redistribution mapping figure is swept in the face that b-e figure is, wherein b figure is Mn element, is shown red
Color；C figure is CSElement, display green；D figure indicates Pb element, is displayed in blue；E figure is Cl element, shows aubergine.
Specific embodiment
Below in conjunction with attached drawing, a preferred embodiment of the present invention will be described in detail.
Embodiment 1
Mn-CsPbCl3The preparation method of perovskite nanometer rods
1. 100mg cesium carbonate is added in the flask of 100mL, 4mL octadecylene and 0.6mL oleic acid are injected, in nitrogen atmosphere
Under be heated to 120 DEG C, form oleic acid caesium solution.
2. by 61.5mg PbCl2With 61.5mg MnCl24H2O is put into the flask of 50mL, and 5mL octadecylene is added,
0.5mL oleic acid and 0.8mL oleyl amine stir 10 minutes under nitrogen atmosphere.Then 120 DEG C are heated to flask, are kept for 30 minutes,
165 DEG C are increased the temperature to, is kept for 10 minutes, then increase the temperature to 200 DEG C, 0.5mL oleic acid and 0.8mL oleyl amine is added, keeps 10
Minute, it can be seen that the clarification of solution side forms Pb/Mn precursor solution.
3. 0.4mL oleic acid caesium solution is injected into Pb/Mn precursor solution, ice bath is cooling.The sample that will finally obtain
It is washed, is centrifuged 5 minutes in 8000rpm, removes supernatant, sediment toluene is dispersed, is centrifuged again, in triplicate,
By finally obtained sample dispersion in n-hexane.
The Mn-CsPbCl obtained by embodiment 13Perovskite nanometer rods are scattered in n-hexane photo (a) under fluorescent light
And its (λ=365nm) photo in the UV lamp, referring to attached drawing 1；Fig. 2 is that embodiment 1 obtains Mn-CsPbCl3Perovskite nanometer rods
Luminescence generated by light photo；Fig. 3 embodiment 1 obtains being Mn-CsPbCl3The absorption spectrum photo of perovskite nanometer rods；Fig. 4 is real
Apply the Mn-CsPbCl that example 1 obtains3The XRD photo of perovskite nanometer rods；Fig. 5 is the Mn-CsPbCl that embodiment 1 obtains3Perovskite
The stereoscan photograph of nanometer rods；Fig. 6 is the Mn-CsPbCl that embodiment 1 obtains3The scanning electron microscope of perovskite nanometer rods
Mapping photo；
Fig. 1 a can be seen that Mn-CsPbCl3Nanometer rods show colourless in fluorescent lamp, and show yellow in the UV lamp, and
And brightness is higher, illustrates good crystallization effect.Fig. 2 can be seen that Mn-CsPbCl3Nanometer rods there are two emission peak, 400nm's
It is CsPbCl3Peak, 600nm be Mn ion peak, illustrate that Mn adulterates well.What Fig. 4 showed is receiving for synthesis
Meter Jing Ti belongs to perovskite structure, and the doping of Mn does not change its crystal structure.Fig. 5 can observe directly the nanometer of synthesis
The form of stick, length is in 50nm or so.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (8)
1. Mn-CsPbCl3The preparation method of nanometer rods, which comprises the steps of:
(1) cesium carbonate is added in octadecylene and oleic acid mixture, is heated to 120 DEG C under nitrogen atmosphere, it is molten that oleic acid caesium is made
Liquid；
It (2) is the PbCl of 1:0.8 ~ 1.2 by mass ratio2And MnCl2·4H2O sequentially adds octadecylene, oleic acid and oleyl amine, in nitrogen
It is stirred 10 minutes under atmosphere, is heated to 120 DEG C, kept for 30 minutes, be heated to 165 DEG C, kept for 10 minutes, be denoted as solution A；
(3) step (2) described solution A is heated to 200 DEG C, adds oleic acid and oleyl amine, until solution side is clarified, form Pb/Mn
Precursor solution；
(4) the resulting oleic acid caesium solution of step (1) is injected into the resulting Pb/Mn precursor solution of step (3), 0 DEG C of ice bath
Cooling, centrifugation, sediment is dispersed with toluene, is centrifuged again, in triplicate, obtains Mn-CsPbCl3Nanometer rods.
2. Mn-CsPbCl according to claim 13The preparation method of nanometer rods, which is characterized in that carbon described in step (1)
The mass volume ratio of sour caesium, octadecylene and oleic acid is 100:4:0.6, mg:ml:ml.
3. Mn-CsPbCl according to claim 13The preparation method of nanometer rods, which is characterized in that described in step (2)
PbCl2, octadecylene, oleic acid and oleyl amine mass volume ratio be 100:8:0.8:1 ~ 2, mg:ml:ml:ml.
4. Mn-CsPbCl according to claim 13The preparation method of nanometer rods, which is characterized in that oil described in step (3)
Acid is equal with oleic acid in step (2) and oleyl amine addition volume respectively with oleyl amine addition volume.
5. Mn-CsPbCl according to claim 13The preparation method of nanometer rods, which is characterized in that step (4) described oleic acid
Caesium and Pb/Mn precursor solution volume ratio are 1:20.
6. Mn-CsPbCl according to claim 13The preparation method of nanometer rods, which is characterized in that step (4) it is described from
The heart is that 8000 rpm are centrifuged 5 minutes.
7. the Mn-CsPbCl obtained by the described in any item preparation methods of claim 1 ~ 63Nanometer rods.
8. Mn-CsPbCl described in claim 73Nanometer rods are in preparing solar battery, light emitting diode with quantum dots or laser
Application.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108258104A (en) * | 2017-12-11 | 2018-07-06 | 温州大学 | A kind of electrostatic preparation method of lead halide caesium fluorescent glass film for mixing manganese |
| CN108585030B (en) * | 2018-04-26 | 2019-09-17 | 吉林大学 | A kind of small size Mn:CsPbCl of Color tunable3Nanocrystalline preparation method |
| CN108504356B (en) * | 2018-05-14 | 2020-08-18 | 华中科技大学 | Manganese-doped inorganic halogen perovskite quantum dot and preparation method and application thereof |
| CN108998015B (en) * | 2018-06-21 | 2021-06-22 | 杭州电子科技大学 | Solvothermal preparation method of manganese-doped cesium-lead halogen perovskite quantum dots |
| CN110079312A (en) * | 2019-04-02 | 2019-08-02 | 济南大学 | A kind of high additive Mn full-inorganic Cs (Pb of hypotoxicity1-xMnx)Cl3The preparation method of perovskite quantum dot |
| CN111710745B (en) * | 2020-06-28 | 2023-03-21 | 重庆邮电大学 | Manganese-doped pure inorganic perovskite-Au nanocrystalline heterojunction and preparation method and application thereof |
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| CN105441074A (en) * | 2015-11-18 | 2016-03-30 | 重庆大学 | Preparation method based on regulating and controlling CsPbBr3 perovskite quantum dots from blue light to green light |
| CN105883909A (en) * | 2016-01-22 | 2016-08-24 | 重庆大学 | Method for preparing CsPbBrxI3-x nanorod |
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| CN105441074A (en) * | 2015-11-18 | 2016-03-30 | 重庆大学 | Preparation method based on regulating and controlling CsPbBr3 perovskite quantum dots from blue light to green light |
| CN105883909A (en) * | 2016-01-22 | 2016-08-24 | 重庆大学 | Method for preparing CsPbBrxI3-x nanorod |
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| Title |
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| Colloidal Mn-Doped Cesium Lead Halide Perovskite Nanoplatelets;Wasim J. Mir等;《ACS Energy Lett.》;20170127;第2卷(第3期);537–543 |
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