CN105552185A - Full-inorganic quantum dot light emitting diode based on inorganic perovskite material and preparation method of full-inorganic quantum dot light emitting diode - Google Patents
Full-inorganic quantum dot light emitting diode based on inorganic perovskite material and preparation method of full-inorganic quantum dot light emitting diode Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims description 11
- 238000000151 deposition Methods 0.000 claims abstract description 22
- 239000004065 semiconductor Substances 0.000 claims abstract description 19
- 230000005540 biological transmission Effects 0.000 claims abstract description 17
- 238000004528 spin coating Methods 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 13
- 238000002207 thermal evaporation Methods 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 14
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000007772 electrode material Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000005525 hole transport Effects 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 abstract description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 abstract 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 abstract 1
- 229910001502 inorganic halide Inorganic materials 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 239000007773 negative electrode material Substances 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 4
- 238000003303 reheating Methods 0.000 description 4
- 238000005401 electroluminescence Methods 0.000 description 3
- 239000011368 organic material Substances 0.000 description 2
- 229920000144 PEDOT:PSS Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/14—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a carrier transport control structure, e.g. highly-doped semiconductor layer or current-blocking structure
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Abstract
The invention discloses a full-inorganic quantum dot light emitting diode based on an inorganic perovskite material. The full-inorganic quantum dot light emitting diode comprises indium tin oxide (ITO) glass, a p-type oxide semiconductor material NiO hole transmission layer, an inorganic perovskite CsPbX3 quantum dot light emitting layer, an n-type oxide semiconductor material electron transmission layer and a negative electrode material. The full-inorganic quantum dot light emitting diode is prepared according to the following steps of firstly, depositing a p-type inorganic oxide semiconductor material on the ITO glass as the hole transmission layer; secondly, spin-coating inorganic halide perovskite quantum dots, and then depositing an n-type inorganic oxide by magnetron sputtering as the electron transmission layer; and finally, depositing a metal electrode of the light emitting diode through thermal evaporation to obtain the full-inorganic CsPbX3 perovskite quantum dot light emitting diode with lighting uniformity. The full-inorganic quantum dot light emitting diode prepared according to the invention has the advantages of narrow half height width of light emitting spectrum, high color purity, high stability and excellent performance, and has wide application value.
Description
Technical field
The present invention relates to a kind of full-inorganic light emitting diode with quantum dots based on inorganic perovskite material and preparation method thereof, belong to quanta point electroluminescent device technical field.
Background technology
Light-emitting diode (LED) is widely used in display, illumination and the field such as backlight, because the luminous efficiency of its excellence and device performance replace the light source that traditional fluorescent lamp becomes a new generation gradually.Organic Light Emitting Diode (OLED) and light emitting diode with quantum dots (QLED) are considered to the two large Main way that following LED develops.Unique quantum effect imparting semiconductor-quantum-point material emission Wavelength tunable, emission spectrum peak width are narrow, quantum efficiency high, and semiconductor-quantum-point material has applications well prospect in fields such as light-emitting diode, display and solar cells.So far, the luminescent layer of most of light emitting diode with quantum dots all adopts cadmium based quantum dot, and its preparation process is loaded down with trivial details, and stability is in urgent need to be improved.Recently, inorganic calcium titanium ore quantum dot (CsPbX
3x=Cl, Br, I) excellent photoelectric properties cause to be paid close attention to widely, the study hotspot that solution synthesis easily, high-quantum efficiency (being greater than 80%) and narrow glow peak (being less than 30nm) make inorganic perovskite material become new, is expected to break through the application difficult problem in QLED field.
Hole transmission layer in common QLED and electron transport layer materials many employings organic material.Document 1 (HighlyEfficientQuantum-DotLight-EmittingDiodeswithDNA-CT MAasaCombinedHole-TransportingandElectron-BlockingLayer, ACSNano2009,3,737-743) utilize PEDOT:PSS, TPD, DNA-CTMA does hole transmission layer, TPBi, Alq3 does electron transfer layer, but these organic materials are very expensive, and be vulnerable to the impact of oxygen and moisture in atmospheric environment and reduce performance, cause QLED preparation process to require strict, add cost.Compared with organic transport layer material, inorganic material has higher electronics, hole mobility, and has good stability in atmosphere, and therefore inorganic carrier transport layer material has huge application potential in the light emitting diode.
Summary of the invention
The object of the present invention is to provide a kind of full-inorganic light emitting diode with quantum dots based on inorganic perovskite material and preparation method thereof.
To achieve these goals, technical scheme of the present invention is as follows: a kind of full-inorganic light emitting diode with quantum dots based on inorganic perovskite material, comprises ito glass, p-type oxide semi-conducting material NiO hole transmission layer, inorganic calcium titanium ore CsPbX
3quantum dot light emitting layer, N-shaped oxide semiconductor material electron transfer layer and cathode electrode material form, and described cathode electrode material is Ag or Al, and described full-inorganic light emitting diode with quantum dots is prepared by following steps:
Step 1, makes hole transmission layer at the ito glass surface deposition p-type oxide semi-conducting material NiO of cleaning, and heat-treats;
Step 2, gets CsPbX
3the dispersion liquid of quantum dot is spin-coated on the device surface after step 1 processes;
Step 3, the surface magnetic control sputtering depositing n-type oxide semiconductor material after step 2 spin coating makes electron transfer layer, and last thermal evaporation deposition cathode electrode material obtains full-inorganic light emitting diode with quantum dots.
Preferably, in step 1, described deposition of hole transport layer adopts spin-coating method or magnetron sputtering method, and the deposit thickness of described p-type oxide semi-conducting material NiO is 25 ~ 50nm, and heat treatment temperature is 300 DEG C ~ 450 DEG C.
Preferably, in step 2, described CsPbX
3x in quantum dot is Cl, Br, I element or the two combination arbitrarily, CsPbX
3the dispersion liquid of quantum dot is CsPbX
3quantum dot is dispersed in normal octane solvent, and the concentration of dispersion liquid is 10 ~ 15mg/mL, and spin speed is 1500 ~ 2000r/min, and spin-coating time is 45 ~ 60s.
Preferably, in step 3, described N-shaped oxide semiconductor material is ZnO or TiO
2, deposit thickness is 40 ~ 60nm; Described cathode electrode material is Ag or Al, and deposit thickness is 80 ~ 100nm.
Compared with prior art, advantage of the present invention is: the present invention adopts the device architecture of full-inorganic, adopts oxide semiconductor material as electron transfer layer and hole transmission layer, improves device stability while reducing costs; Adopt inorganic calcium titanium ore CsPbX simultaneously
3quantum dot, as luminescent layer, improves its luminous efficiency, and the high and excellent performance of the light-emitting diode luminance that the present invention obtains, is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the structural representation of light-emitting diode of the present invention.
Fig. 2 is that the current density of light-emitting diode prepared by embodiment 2 is with applied voltage variation relation figure.
Fig. 3 is the electroluminescence collection of illustrative plates of light-emitting diode prepared by embodiment 3.
Embodiment
Below by embodiment and accompanying drawing, the invention will be further described.
A kind of full-inorganic light emitting diode with quantum dots based on inorganic perovskite material of the present invention, structure as shown in Figure 1, comprises ito glass, is deposited on p-type oxide semi-conducting material NiO hole transmission layer, the inorganic calcium titanium ore CsPbX on ito glass surface
3quantum dot light emitting layer, N-shaped oxide semiconductor material electron transfer layer and cathode electrode material, preparation method is as follows: first on clean ito glass, make hole transmission layer by the p-type oxide NiO of spin coating or magnetron sputtering deposition 25 ~ 50nm, spin-on inorganic perovskite CsPbX3 quantum dot light emitting layer again after 300 DEG C ~ 450 DEG C heat treatments, then by N-shaped oxide ZnO or TiO of magnetron sputtering deposition 40 ~ 60nm
2make electron transfer layer, cathode electrode material Ag or Al of last thermal evaporation deposition 80 ~ 100nm, finally obtain luminous uniform full-inorganic CsPbX
3perovskite light emitting diode with quantum dots.
Embodiment 1
Step 1, gets ito glass through acetone, and ethanol and washed with de-ionized water final vacuum are dried, and the NiO thick by magnetron sputtering deposition 20nm makes hole transmission layer, in atmosphere through 350 DEG C of process 15min;
Step 2, gets the CsPbBr of appropriate 10mg/mL high―temperature nuclei
3quantum dot dispersion liquid is spin-coated on device surface after step 1 processes, and rotating speed is 1500r/min, spin-coating time 45s;
Step 3, electron transfer layer is made by the ZnO that magnetron sputtering deposition 40nm is thick in the surface after step 2 spin coating, Ag (or Al) electrode of reheating hydatogenesis one deck 80nm, obtained based on CsPbBr
3full-inorganic light emitting diode with quantum dots.
Embodiment 2
Step 1, gets ito glass through acetone, and ethanol and washed with de-ionized water final vacuum are dried, and the NiO thick by magnetron sputtering deposition 40nm makes hole transmission layer, in atmosphere through 450 DEG C of process 10min;
Step 2, gets the CsPbBr of appropriate 15mg/mL high―temperature nuclei
3quantum dot dispersion liquid is spin-coated on device surface after step 1 processes, and rotating speed is 2000r/min, spin-coating time 45s;
Step 3, electron transfer layer is made by the ZnO that magnetron sputtering deposition 50nm is thick in the surface after step 2 spin coating, Ag (or Al) electrode of reheating hydatogenesis one deck 100nm, obtained based on CsPbBr
3full-inorganic light emitting diode with quantum dots, the current density of device with apply voltage relationship figure as shown in Figure 2, can find out that the starting resistor of device is lower, meet energy-saving and cost-reducing demand.
Embodiment 3
Step 1, gets ito glass through acetone, and ethanol and washed with de-ionized water final vacuum are dried, and the NiO thick by magnetron sputtering deposition 20nm makes hole transmission layer, in atmosphere through 350 DEG C of process 15min;
Step 2, gets the CsPbBr of appropriate 10mg/mL high―temperature nuclei
3quantum dot dispersion liquid is spin-coated on device surface after step 1 processes, and rotating speed is 1500r/min, spin-coating time 45s;
Step 3, the thick TiO of magnetron sputtering deposition 40nm is passed through on the surface after step 2 spin coating
2make electron transfer layer, Ag (or Al) electrode of reheating hydatogenesis one deck 80nm, obtained based on CsPbBr
3full-inorganic light emitting diode with quantum dots.
As shown in Figure 3, have very pure glow peak, without other assorted peaks, and the halfwidth of emission peak is narrow, only has about 30nm for electroluminescence (EL) spectrum of full-inorganic light emitting diode with quantum dots device prepared by the present embodiment.
Embodiment 4
Step 1, gets ito glass through acetone, and ethanol and washed with de-ionized water final vacuum are dried, and the NiO thick by magnetron sputtering deposition 20nm makes hole transmission layer, in atmosphere through 350 DEG C of process 15min;
Step 2, gets the CsPbIBr of appropriate 10mg/mL high―temperature nuclei
2quantum dot dispersion liquid is spin-coated on device surface after step 1 processes, and rotating speed is 1500r/min, spin-coating time 45s;
Step 3, electron transfer layer is made by the ZnO that magnetron sputtering deposition 40nm is thick in the surface after step 2 spin coating, Ag (or Al) electrode of reheating hydatogenesis one deck 80nm, obtained based on CsPbIBr
2full-inorganic light emitting diode with quantum dots.
Claims (7)
1. based on a full-inorganic light emitting diode with quantum dots for inorganic perovskite material, it is characterized in that, by ito glass, p-type oxide semi-conducting material NiO hole transmission layer, inorganic calcium titanium ore CsPbX
3quantum dot light emitting layer, N-shaped oxide semiconductor material electron transfer layer and cathode electrode material form.
2. full-inorganic light emitting diode with quantum dots according to claim 1, is characterized in that, described N-shaped oxide semiconductor material is ZnO or TiO
2.
3. full-inorganic light emitting diode with quantum dots according to claim 1, is characterized in that, described cathode electrode material is Ag or Al.
4., according to the preparation method of the arbitrary described full-inorganic light emitting diode with quantum dots of claims 1 to 3, it is characterized in that, comprise the following steps:
Step 1, makes hole transmission layer at the ito glass surface deposition p-type oxide semi-conducting material NiO of cleaning, and heat-treats;
Step 2, gets CsPbX
3the dispersion liquid of quantum dot is spin-coated on the device surface after step 1 processes;
Step 3, the surface magnetic control sputtering depositing n-type oxide semiconductor material after step 2 spin coating makes electron transfer layer, and last thermal evaporation deposition cathode electrode material obtains full-inorganic light emitting diode with quantum dots.
5. preparation method according to claim 4, it is characterized in that, in step 1, described deposition of hole transport layer adopts spin-coating method or magnetron sputtering method, the deposit thickness of described p-type oxide semi-conducting material NiO is 25 ~ 50nm, and heat treatment temperature is 300 DEG C ~ 450 DEG C.
6. preparation method according to claim 4, is characterized in that, in step 2, and described CsPbX
3x in quantum dot is Cl, Br, I element or the two combination arbitrarily, CsPbX
3the dispersion liquid of quantum dot is CsPbX
3quantum dot is dispersed in normal octane solvent, and the concentration of dispersion liquid is 10 ~ 15mg/mL, and spin speed is 1500 ~ 2000r/min, and spin-coating time is 45 ~ 60s.
7. preparation method according to claim 4, is characterized in that, in step 3, described N-shaped oxide semiconductor material is ZnO or TiO
2, deposit thickness is 40 ~ 60nm; Described cathode electrode material is Ag or Al, and deposit thickness is 80 ~ 100nm.
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Cited By (13)
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| CN106450042A (en) * | 2016-09-26 | 2017-02-22 | Tcl集团股份有限公司 | Metal oxide, QLED and preparation method |
| CN106450021A (en) * | 2016-11-24 | 2017-02-22 | 南方科技大学 | Organic electroluminescent device and preparation method thereof |
| CN107146854A (en) * | 2017-05-11 | 2017-09-08 | 安徽熙泰智能科技有限公司 | A kind of microdisplay on silicon part of perovskite light emitting diode and preparation method thereof |
| CN107170908A (en) * | 2017-05-23 | 2017-09-15 | 华灿光电（浙江）有限公司 | Epitaxial wafer of light emitting diode and preparation method |
| CN107275523A (en) * | 2017-06-13 | 2017-10-20 | 苏州大学 | Preparation method of pure inorganic perovskite light-emitting diode device |
| WO2017200732A1 (en) * | 2016-05-20 | 2017-11-23 | Brown University | Method for manufacturing perovskite solar cells and multijunction photovoltaics |
| CN107681058A (en) * | 2016-08-01 | 2018-02-09 | 成功大学 | Light emitting diode and its manufacture method |
| CN107863424A (en) * | 2017-11-13 | 2018-03-30 | 吉林大学 | A kind of full-inorganic luminescent device based on perovskite thin film and preparation method thereof |
| CN109004091A (en) * | 2018-06-11 | 2018-12-14 | 南京理工大学 | A kind of light emitting diode with quantum dots and preparation method thereof based on room temperature perovskite material |
| CN110492012A (en) * | 2019-08-26 | 2019-11-22 | 京东方科技集团股份有限公司 | A kind of quantum dot light emitting device and preparation method thereof, display panel, display device |
| CN110649133A (en) * | 2019-09-26 | 2020-01-03 | 河南科技大学 | All-inorganic perovskite LED light-emitting device based on InN electron transport layer |
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| CN106450042A (en) * | 2016-09-26 | 2017-02-22 | Tcl集团股份有限公司 | Metal oxide, QLED and preparation method |
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