CN109411614A - A kind of organic-inorganic composite perovskite LED device and preparation method thereof - Google Patents
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Abstract
The invention belongs to LED technology field, in particular to a kind of organic-inorganic composite perovskite LED device and preparation method thereof, the perovskite nanocrystal (FA including different doping ratio coefficients1‑xMAxPbBr3) preparation method；Organic-inorganic composite perovskite light emitting diode be followed successively by from top to bottom transparent electro-conductive glass substrate, hole injection layer, hole transmission layer, organic-inorganic composite perovskite luminescent layer, electron transfer layer, Al and LiF combination electrode；Organic-inorganic composite perovskite nanocrystal (FA1‑xMAxPbBr3) it is to be made by raw material of the mixed solution of the FABr of different mol ratio example and MABr；The preparation method of organic-inorganic composite perovskite nanocrystal of the invention is simple, low in cost, and perovskite LED device obtained has very high photoelectric conversion efficiency, can effectively improve perovskite LED device performance.
Description
Technical field
The invention belongs to LED technology field, in particular to a kind of organic-inorganic composite perovskite light-emitting diodes
Tube device and preparation method thereof.
Background technique
Organic-inorganic metal perovskite nanocrystal is as a kind of new semiconductor optical material, simple low temperature system
Preparation Method, the characteristics such as tunable optical band gap and superior charge transport ability, in light emitting diode, solar energy electronic swashs
The fields such as light device and photodetector show great potential.The general formula of organic and inorganic perovskite is AMX3, A expression amine
Organic cation (such as CH3NH3 +, HC (NH2)2 +), M expression inorganic metal ion (such as Pb2+,Sn2+,Ge2+,Cu2+,Co2+
Deng), X is then halide ion (such as Cl-,Br-,I-).Material may be implemented by changing cation and halide ion in perovskite
Entire visible light shines.For example, using CH recently3NH3PbBr3The green light perovskite LED of preparation, maximum current effect
Rate has been more than 30cd A-1, there are also CH3NH3PbI3For the solar battery of light absorbent, photoelectric conversion efficiency has been more than 18%.
Furthermore utilize FAPbBr3Perovskite LED as luminescent material also comes into being, and maximum emission intensity has reached 13000cd m-2, maximum current efficiency is close to 6.4cd A-1。
The achievement that perovskite material obtains in nearest 2 years should not be underestimated, and exist on high efficiency high brightness device
Huge potential.On the one hand, Gu Zimite tolerance factor namely gold impact factor t,
Perovskite structure (r is A, the ionic radius of M, X) can be formed for decision element, tolerance factor is conducive between 0.9~1
The stability of crystal at room temperature, FA+Ionic radius ratio MA+It is big, tolerance factor is closer to 1, conducive to perovskite structure
It is formed.On the other hand, with FA+The light absorbent and MA of solar battery are generally used for for the perovskite of cation+For cation
Perovskite LED compare, FA+Report it is fewer and fewer.Meanwhile solar battery is used for about mixed-cation perovskite material
Increasingly cause researcher's note that minimal amount MA with light emitting diode report+It is doped to FA+In FAxMA1-xPb(IxBr1-x)3
Material makes the photoelectric conversion efficiency of solar battery be more than 20%.In the prior art, perovskite light emitting diode is generally adopted
With single MAPbX3、FAPbX3、CsSnX3Equal perovskites are as active light-emitting layer, and there are perovskite lumination of light emitting diode effects
The disadvantages such as rate is low, and external quantum efficiency is low, therefore the luminous efficiency of raising device and external quantum efficiency are need to solve at present one
A major issue.
Summary of the invention
The present invention solves the above-mentioned technical problems in the prior art, provides a kind of organic-inorganic composite perovskite hair
Optical diode device and preparation method thereof.
To solve the above problems, technical scheme is as follows:
A kind of organic-inorganic composite perovskite LED device from bottom to top successively includes transparent conductive anode
ITO, hole injection layer, hole transmission layer, organic-inorganic perovskite luminescent layer, electron transfer layer, cathode；The organic-inorganic calcium
Titanium ore luminescent layer is by being doped with the FAPbBr of methylamine ion (MA)3Nanocrystal constitute, ingredient FA1-xMAxPbBr3；Its
Middle FA indicates that carbonamidine ion, MA indicate methylamine ion.
Preferably, the hole injection layer is PEDOT:PSS (poly- 3,4-rthylene dioxythiophene/poly styrene sulfonate),
For level-density parameter, it is more favorable for the injection in hole.
Preferably, the hole transmission layer is TFB (poly- (9,9- dioctyl fluorene-CO-N- (4- butyl phenyl) diphenylamines).
Preferably, the electron transfer layer is TPBi (1,3,5- tri- (1- phenyl -1H- benzimidazolyl-2 radicals-yl) benzene).
Preferably, the cathode is the combination electrode of metal or metal and fluoride；It is highly preferred that the cathode selection gold
When category, aluminium；When the cathode selection combination electrode, the combination electrode of LiF and Al is selected.
A kind of organic-inorganic composite perovskite nanocrystal (FA1-xMAxPbBr3) preparation method, comprising the following steps:
Step 1, by the hydrobromic acid (HBr) and methylamine (CH of equimolar amounts ratio3NH2) be sufficiently stirred under conditions of ice bath, it washes
Drying is washed, is made methyl bromide ammonium (MABr)；
Step 2, the FABr of different mol ratio example (bromination carbonamidine) and MABr are dissolved in n,N-Dimethylformamide (DMF)
In, obtained solution A；
Step 3, by lead bromide (PbBr2) be dissolved in DMF, obtained solution B；
Step 4, oleic acid (OA) and oleyl amine (OLA) are added dropwise in solution A and the mixing liquid of B, stirring is until mix molten
Liquid bleach, obtains solution C；
Step 5, solution C is dropped in toluene, acetonitrile, obtained solution D is added after stirring；
Step 6, solution D is taken precipitating, precipitating is dissolved in tetrahydrofuran after 5000-6000 turns centrifugation 4-5 minutes,
Obtained solution E；
Step 7, solution E is turned into centrifugation 4-5 minutes through 5000-5500, takes supernatant, that dissolve in supernatant is FA1- xMAxPbBr3Organic-inorganic perovskite nanocrystal.
A kind of preparation method of organic-inorganic composite perovskite LED device, comprising the following steps:
Step 1, the transparent anode layer using ito glass as device；
Step 2, the preparation of hole injection layer: PEDOT:PSS is spun on transparent anode layer ito glass, annealing；
Step 3, prepare hole transmission layer on hole transmission layer prepared by step 2: it is thin that TFB is spun on PEDOT:PSS
On film, annealing；
Step 4, perovskite luminescent layer is prepared on hole transmission layer prepared by step 3: being dissolved in tetrahydrofuran
FA1-xMAxPbBr3Nanocrystal is spun on hole transmission layer TFB, without annealing；
Step 5, the vacuum evaporation electron transfer layer TPBi on perovskite luminescent layer prepared by step 4, makes it be attached to calcium
The top of titanium ore nano particle；
Step 6, the preparation of cathode: keep the vacuum cavity pressure of step 5 constant, on the electron transport layer evaporation metal fluorine
Compound LiF and cathode layer of the metal Al composite layer as device；Or evaporation metal aluminium on the electron transport layer；It obtains after the completion
Above-mentioned organic-inorganic composite perovskite LED device.
Preferably, the transparent anode layer is with a thickness of 200nm；Electron transport layer thickness is 40nm.
Preferably, the annealing condition of the step 2 are as follows: 150 DEG C are annealed 30 minutes；The annealing conditions of the step 3
It anneals 20 minutes for 120 DEG C.
Preferably, in the step 6, evaporation metal fluoride LiF and metal Al composite layer conduct on the electron transport layer
When the cathode layer of device, LiF with a thickness of 1nm, Al with a thickness of 120nm.
Compared with the existing technology, advantages of the present invention is as follows,
The diameter of perovskite nano particle after doping MA of the invention is than pure FAPbBr3Want almost one times small, it is average
Diameter reaches 8nm, but luminescence peak does not change；LED after adulterating based on perovskite is than pure FAPbBr3LED electricity
Stream efficiency wants nearly 5 times high, and external quantum efficiency is 4 times high, and quantum yield is more than 60%；It is effective to improve perovskite light emitting diode
Photoelectric conversion efficiency.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of organic-inorganic composite perovskite light emitting diode of the invention；1 is LiF/Al electricity
Pole, 2 be (1,3,5- tri- (1- phenyl -1H- benzimidazolyl-2 radicals-yl) benzene), and 3 be organic-inorganic composite perovskite luminescent layer, and 4 are
(poly- 3,4-rthylene dioxythiophene/poly styrene sulfonate), 5 be ITO electro-conductive glass；
Fig. 2 is the FA for adulterating different proportion MA1-xMAxPbBr3(x=0,0.1,0.2) the XRD diffracting spectrum of nano particle；
Fig. 3 is the FA for adulterating different proportion MA1-xMAxPbBr3The TEM of nano particle schemes, and (a) is pure FAPbBr3Nanometer
Grain, average diameter is 13.5nm；It (b) is FA0.9MA0.1PbBr3Nano particle；It (c) is FA0.8MA0.2PbBr3Nano particle, it is average
Diameter is 8nm.
Specific embodiment
Embodiment 1:
Referring to Fig. 1, FA-MA organic-inorganic composite perovskite of the invention is given out light diode component, from the bottom to top successively
For transparent conductive anode ITO, hole injection layer, hole transmission layer, organic-inorganic perovskite luminescent layer, electron transfer layer, metal
Conductive electrode.Each layer is described in detail below.
Wherein transparent conductive anode layer uses inorganic material, and tin indium oxide (ITO), thickness is about 200nm；
Hole injection layer of the invention uses PEDOT:PSS (poly- 3,4-rthylene dioxythiophene/poly styrene sulfonate), special
Sign is that implanted layer will be used to improve the work function of conductive anode ITO, is more favorable for the injection in hole；
Hole transmission layer of the invention is TFB (poly- (9,9- dioctyl fluorene-CO-N- (4- butyl phenyl) diphenylamines)；Electronics
Transport layer is TPBi (1,3,5- tri- (1- phenyl -1H- benzimidazolyl-2 radicals-yl) benzene)；
Cathode is the combination electrode of metal or metal and fluoride；For example, when the cathode selection metal, aluminium；Institute
When stating cathode selection combination electrode, the combination electrode of LiF and Al is selected.
Organic-inorganic perovskite luminescent layer of the invention is the FAPbBr by being doped with methylamine ion (MA)3Perovskite receive
Rice grain is constituted, ingredient FA1-xMAxPbBr3；The doping ratio used in example is (x=0,0.1,0.2)；Ingredient difference
For FA0.9MA0.1PbBr3, FA0.8MA0.2PbBr3And FAPbBr3。
It is above-mentioned with doping after perovskite (FA0.9MA0.1PbBr3, FA0.8MA0.2PbBr3) based on LED than pure FAPbBr3
LED current efficiency want nearly 5 times high, external quantum efficiency is 4 times high, and quantum yield is more than 60%.
Embodiment 2:
For FA1-xMAxPbBr3The preparating example method of perovskite nanocrystal:
Step 1, by the hydrobromic acid (HBr) and methylamine (CH of equimolar amounts ratio3NH2) stirred two hours under conditions of ice bath,
After the two is sufficiently reacted, it is dried to obtain reactant in 60 DEG C, is done in a vacuum after then cleaning reactant three times with ether
It obtains fluffy white powder within dry 24 hours, is made methyl bromide ammonium (MABr)；
Step 2, the FABr and MABr of 0.8mmol different mol ratio example (9:1 and 8:2) are dissolved in respectively in 0.5ml DMF,
Obtained solution A；
Step 3, by 1mmol PbBr2It is dissolved in 0.5ml DMF, obtained solution B；
Step 4, suitable oleic acid (OA) and oleyl amine (OLA) are added dropwise in solution A and the mixing liquid of B, stirring until
Mixed solution bleach, obtains solution C；
Step 5, solution C is slowly dropped in 10ml toluene, and is stirred, until solution becomes limpid green, then
5ml acetonitrile, obtained solution D are added in green solution；
Step 6, solution D is taken into precipitating, then precipitating is dissolved in 1ml tetrahydro furan after 5000-6000 turns centrifugation 4-5 minutes
In muttering, obtained solution E；
Step 7, solution E is turned into centrifugation 4-5 minutes by another secondary 5000-5500, takes supernatant, is dissolved in supernatant
It is perovskite nano particle.
Fig. 2 is the X-ray diffraction peak of the perovskite nanocrystal of three kinds of difference MA proportionality coefficients.From the figure, it can be seen that
The same FAPbBr of all samples3It equally, is all Pm3m cubic crystal structure, and diffraction highest peak is nearly all in (001),
(011), (002) and (012) these peak positions.
Fig. 3 is dissolved in the perovskite nanocrystal of tetrahydrofuran, drips in ultrathin carbon films dropwise, and aobvious with transmitted electron
Micro mirror obtains FAPbBr3, MA-FAPbBr3The aspect graph of quantum dot；It can be seen that pure FAPbBr3Being averaged for nano particle is straight
Diameter is 13.5nm, and with the increase of MA ratio, the diameter of perovskite nano particle is gradually become smaller, and it is big to be gradually decreased as average diameter
Small is 8nm.
Embodiment 3:
Based on the structural schematic diagram of organic-inorganic composite perovskite light emitting diode shown in FIG. 1, the present invention provides
A kind of preparation method of the perovskite light emitting diode of embodiment, method includes the following steps:
1) ito glass is etched into narrowband with laser marking machine, uses acetone, isopropanol, deionized water ultrasonic cleaning respectively
20 minutes, using ito glass as the transparent anode layer of device, wherein the square resistance of ito glass was about 15~30 Ω, and thickness is about
For 200nm；
2) preparation of hole injection layer: the ito glass that step 1) is handled well is divided using ultraviolet cleaning machine ozone treatment 30
Then PEDOT:PSS is spun on transparent anode layer ito glass, 4 layers of spin coating, PEDOT by clock with the speed of 5000rpm/min:
PSS film thickness is about 220~240nm；Then it is annealed 30 minutes with 150 DEG C；
3) preparation of hole transmission layer: step 2) preparation hole transmission layer on prepare hole transmission layer: by TFB with
The speed of 3000rpm/min is spun on PEDOT:PSS film, and is annealed 20 minutes with 120 DEG C；
4) preparation of organic-inorganic composite perovskite luminescent layer: calcium titanium is prepared on the hole transmission layer of step 3) preparation
Mine luminescent layer: the FA being dissolved in tetrahydrofuran1-xMAxPbBr3Nano particle is spun on hole transmission layer TFB, without moving back
Fire；
5) preparation of electron transfer layer: the vacuum evaporation electron transfer layer TPBi on the perovskite luminescent layer of step 4) preparation
(40nm) makes it be attached to the top of perovskite nano particle；
6) preparation of cathode: keeping the vacuum cavity pressure of step 5) constant, and evaporation metal is fluorinated on the electron transport layer
Object LiF (1nm) and cathode layer of metal Al (120nm) composite layer as device, after the completion above-mentioned organic-inorganic composite calcium
Titanium ore light emitting diode.
It should be noted that above-described embodiment is only presently preferred embodiments of the present invention, there is no for the purpose of limiting the invention
Protection scope, the equivalent substitution or substitution made on the basis of the above all belong to the scope of protection of the present invention.
Claims (10)
1. a kind of organic-inorganic composite perovskite LED device, from bottom to top successively include transparent conductive anode ITO,
Hole injection layer, hole transmission layer, organic-inorganic perovskite luminescent layer, electron transfer layer, cathode；It is characterized in that, described have
The inorganic perovskite luminescent layer of machine is by being doped with the FAPbBr of MA3Nanocrystal constitute, wherein FA indicate carbonamidine ion, MA indicate
Methylamine ion.
2. organic-inorganic composite perovskite luminescent layer as described in claim 1, which is characterized in that ingredient FA1- xMAxPbBr3。
3. organic-inorganic composite perovskite LED device as described in claim 1, which is characterized in that the hole
Implanted layer is poly- 3,4- ethene dioxythiophene/poly styrene sulfonate.
4. organic-inorganic composite perovskite LED device as described in claim 1, which is characterized in that the hole
Transport layer is poly- (9,9- dioctyl fluorene-CO-N- (4- butyl phenyl) diphenylamines.
5. organic-inorganic composite perovskite LED device as described in claim 1, which is characterized in that the electronics
Transport layer is 1,3,5- tri- (1- phenyl -1H- benzimidazolyl-2 radicals-yl) benzene.
6. organic-inorganic composite perovskite LED device as described in claim 1, which is characterized in that the cathode
For the combination electrode of Al and LiF.
7.FA1-xMAxPbBr3The preparation method of perovskite nanocrystal, which comprises the following steps:
Step 1, the hydrobromic acid of equimolar amounts ratio and methylamine are sufficiently stirred under conditions of ice bath, wash drying, methyl is made
Amine bromide；
Step 2, the bromination carbonamidine of different mol ratio example and methyl bromide amine are dissolved in n,N-Dimethylformamide, are made molten
Liquid A；
Step 3, lead bromide is dissolved in n,N-Dimethylformamide, obtained solution B；
Step 4, oleic acid and oleyl amine are added dropwise in solution A and the mixing liquid of B, stirring obtains until mixed solution bleach
Solution C；
Step 5, solution C is dropped in toluene, acetonitrile, obtained solution D is added after stirring；
Step 6, solution is taken precipitating, precipitating is dissolved in tetrahydrofuran, be made molten after 5000-6000 turns centrifugation 4-5 minutes
Liquid E；
Step 7, solution E is turned into centrifugation 4-5 minutes through 5000-5500, takes supernatant, that dissolve in supernatant is FA1- xMAxPbBr3Perovskite nanocrystal.
8. a kind of preparation method of organic-inorganic composite perovskite LED device, which is characterized in that including following step
It is rapid:
Step 1, the transparent anode layer using ito glass as device；
Step 2, the preparation of hole injection layer: PEDOT:PSS is spun on transparent anode layer ito glass, annealing；
Step 3, hole transmission layer is prepared on hole transmission layer prepared by step 2: TFB is spun on PEDOT:PSS film,
Annealing；
Step 4, perovskite luminescent layer is prepared on hole transmission layer prepared by step 3: the FA being dissolved in tetrahydrofuran1- xMAxPbBr3Nanocrystal is spun on hole transmission layer TFB, without annealing；
Step 5, the vacuum evaporation electron transfer layer TPBi on perovskite luminescent layer prepared by step 4, makes it be attached to perovskite
The top of nano particle；
Step 6, the preparation of cathode: keep the vacuum cavity pressure of step 5 constant, on the electron transport layer evaporation metal fluoride
LiF and cathode layer of the metal Al composite layer as device；Above-mentioned organic-inorganic composite perovskite light-emitting diodes are obtained after the completion
Tube device.
9. the preparation method of organic-inorganic composite perovskite LED device as claimed in claim 8, feature exist
In the transparent anode layer is with a thickness of 200nm；The hole injection layer is with a thickness of 220~240nm；Electron transport layer thickness is
40nm；Cathode layer is metal fluoride LiF and metal Al composite layer, LiF with a thickness of 1nm, Al with a thickness of 120nm.
10. the preparation method of organic-inorganic composite perovskite LED device as claimed in claim 8, feature exist
In the annealing condition of the step 2 are as follows: 150 DEG C are annealed 30 minutes；The annealing conditions of the step 3 are 120 DEG C of annealing 20
Minute.
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| CN110120457A (en) * | 2019-05-14 | 2019-08-13 | 南京邮电大学 | A kind of perovskite light emitting diode and preparation method thereof based on double emitting layers |
| CN110120467A (en) * | 2019-05-14 | 2019-08-13 | 南京邮电大学 | Perovskite light emitting diode and preparation method thereof based on pre- spin coating FABr |
| CN111048690A (en) * | 2019-11-25 | 2020-04-21 | 苏州大学 | Blue light perovskite film and blue light perovskite light emitting diode |
| CN111634949A (en) * | 2020-05-15 | 2020-09-08 | 桂林电子科技大学 | WO (WO)xSolution preparation method, ultraviolet device using the same and preparation method thereof |
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| CN110120457A (en) * | 2019-05-14 | 2019-08-13 | 南京邮电大学 | A kind of perovskite light emitting diode and preparation method thereof based on double emitting layers |
| CN110120467A (en) * | 2019-05-14 | 2019-08-13 | 南京邮电大学 | Perovskite light emitting diode and preparation method thereof based on pre- spin coating FABr |
| CN110120457B (en) * | 2019-05-14 | 2021-09-14 | 南京邮电大学 | Perovskite light-emitting diode based on double light-emitting layers and preparation method thereof |
| CN111048690A (en) * | 2019-11-25 | 2020-04-21 | 苏州大学 | Blue light perovskite film and blue light perovskite light emitting diode |
| CN113571641A (en) * | 2020-04-28 | 2021-10-29 | 杭州纤纳光电科技有限公司 | Perovskite solar cell with composite transmission layer and preparation method thereof |
| CN111634949A (en) * | 2020-05-15 | 2020-09-08 | 桂林电子科技大学 | WO (WO)xSolution preparation method, ultraviolet device using the same and preparation method thereof |
| CN113846373A (en) * | 2020-06-28 | 2021-12-28 | 厦门稀土材料研究所 | Perovskite CsPbX3Nanocrystalline and preparation method and application thereof |
| CN111883693A (en) * | 2020-07-27 | 2020-11-03 | 湖北工业大学 | Perovskite light-emitting diode based on oxide hole injection layer and preparation method thereof |
| CN111952473A (en) * | 2020-08-18 | 2020-11-17 | 福州大学 | Preparation method of perovskite thin film doped with amphiphilic silicon dioxide ions and preparation method of light-emitting diode |
| CN111952473B (en) * | 2020-08-18 | 2023-12-12 | 福州大学 | Preparation method of perovskite light-emitting diode doped with amphiphilic silica particles |
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