CN106252529A - The NiO of a kind of doping, light emitting diode and preparation method thereof - Google Patents

The NiO of a kind of doping, light emitting diode and preparation method thereof Download PDF

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Publication number
CN106252529A
CN106252529A CN201610821482.6A CN201610821482A CN106252529A CN 106252529 A CN106252529 A CN 106252529A CN 201610821482 A CN201610821482 A CN 201610821482A CN 106252529 A CN106252529 A CN 106252529A
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nio
doping
preparation
salt
light emitting
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王宇
曹蔚然
杨行
杨一行
钱磊
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TCL Corp
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TCL Corp
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    • H—ELECTRICITY
    • H01—BASIC ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00—Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/50—Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for light emission, e.g. organic light emitting diodes [OLED] or polymer light emitting devices [PLED]
    • H01L51/5012—Electroluminescent [EL] layer
    • H01L51/502—Electroluminescent [EL] layer comprising active inorganic nanostructures, e.g. luminescent quantum dots
    • H—ELECTRICITY
    • H01—BASIC ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00—Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/50—Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for light emission, e.g. organic light emitting diodes [OLED] or polymer light emitting devices [PLED]
    • H01L51/5088—Carrier injection layer
    • H—ELECTRICITY
    • H01—BASIC ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00—Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/50—Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for light emission, e.g. organic light emitting diodes [OLED] or polymer light emitting devices [PLED]
    • H01L51/56—Processes or apparatus specially adapted for the manufacture or treatment of such devices or of parts thereof
    • H—ELECTRICITY
    • H01—BASIC ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L2251/00—Indexing scheme relating to organic semiconductor devices covered by group H01L51/00
    • H01L2251/30—Materials
    • H01L2251/301—Inorganic materials
    • H01L2251/303—Oxides, e.g. metal oxides

Abstract

The present invention discloses the NiO of a kind of doping, light emitting diode and preparation method thereof, it includes step: nickel salt, the first doping salt and the second doping salt are mixed in deionized water or 2 methyl cellosolves, add glycine or acetylacetone,2,4-pentanedione, then heat, prepare LixMyNiO；Wherein, the first doping salt is lithium salts, and the second doping salt is magnesium salt, mantoquita or zinc salt；LixMyIn NiO, M=Mg or Cu or Zn, 0 ＜ x ＜ 1,0 ＜ y ＜ 1.Li of the present inventionxMyThe preparation temperature of NiO thin film is low, can prepare within the temperature range of 150 ~ 200 DEG C.And at LixMyDuring NiO film preparation, add a small amount of ammonia, it is ensured that the stability of precursor solution.In the case of the work function ensureing nickel oxide does not reduces, improve the ability of its hole transport, reduce the injection barrier in hole；Light emitting diode of the present invention is made to achieve higher efficiency.

Description

The NiO of a kind of doping, light emitting diode and preparation method thereof
Technical field
The present invention relates to LED technology field, particularly relate to the NiO of a kind of doping, light emitting diode and preparation thereof Method.
Background technology
At present in QLED device, red-green-blue all has been achieved for higher efficiency, but the life-span is still restriction The business-like principal element of QLED.In order to improve stability and the life-span of device, document has been had to use oxo transition metal Compound substitutes organic layer therein, the most mainly substitutes PEDOT:PSS (poly-(3,4-rthylene dioxythiophene)-polystyrene sulphur Acid).The most common metal-oxide mainly has V2O5, WO3, NiO and MoO3.NiO is as a kind of P-type semiconductor, because it has One transmitance the highest and high work function (5.2-5.4eV) so that it is become a kind of PEDOT:PSS of replacement and select.
In order to improve the performance of NiO further, Alex K.-Y. Jen is published on " Advance Matererial " In article, by using the NiO of Cu doping, improve and improve the open-circuit voltage of organic solar batteries device and short further The performance of road electric current.And in the article delivered on " RSC Advance " magazine of Chen wei in 2014, by using Mg The nickel oxide of doping changes the work function of nickel oxide, and improves the efficiency of DSSC.Above-mentioned improvement is all It is that the work function to nickel oxide improves, and these application are all to apply in the battery.And in QLED, hole transport Speed is less than the transfer rate of electronics, therefore while improving the work function of nickel oxide, will pass the carrier of nickel oxide Defeated speed improves and improves.
O. S. Bezkrovnyi in 2013 and Hasan Azimi Juybari in 2011 et al. use different sides respectively Method is doped Li unit and usually improves the performance of nickel oxide nickel oxide.But the work function that Li doping can make nickel oxide reduces, It is unfavorable in QLED device application, the potential barrier that in QLED, hole is injected can be made to improve.Therefore NiO hole injection energy is being improved Also to ensure while power that its work function does not reduces as far as possible.Deliver on " Science " at Chen wei in 2015 etc. By using the nickel oxide of Li and Mg doping in article so that the efficiency of large area perovskite solaode has reached 16%.Its In the preparation method of this nickel oxide be to use nickel acetylacetonate and four acetate hydrate magnesium and the mixed liquor of Quilonorm (SKB), use injection Method forms the nickel oxide of doping under the high temperature of 500 DEG C.Clearly can be seen that the high temperature of 500 DEG C is be not suitable for future suitable By property, be more not suitable for the flexible development in future.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide the NiO of a kind of doping, light emitting diode and Its preparation method, it is intended to solve prior art and cannot react the nickel oxide of preparation doping at low temperatures, and maintain the merit of nickel oxide The problem that function does not reduces.
Technical scheme is as follows:
A kind of preparation method of the NiO of doping, wherein, including step:
Nickel salt, the first doping salt and the second doping salt are mixed in deionized water or 2-methyl cellosolve, add glycine Or at least one in acetylacetone,2,4-pentanedione, then heat, prepare LixMyNiO；Wherein, the first doping salt is lithium salts, and second mixes Carnallite is magnesium salt, mantoquita or zinc salt；LixMyIn NiO, M=Mg or Cu or Zn, 0 ＜ x ＜ 1,0 ＜ y ＜ 1.
The preparation method of the NiO of described doping, wherein, after adding glycine or acetylacetone,2,4-pentanedione, is additionally added NH3•H2O Solution.
The preparation method of the NiO of described doping, wherein, described nickel salt is Ni (NO3)2·6H2O, described lithium salts is LiNO3。
The preparation method of the NiO of described doping, wherein, described magnesium salt is Mg (NO3)2。
The preparation method of the NiO of described doping, wherein, described mantoquita is Cu (NO3)2·2.5H2O。
The preparation method of the NiO of described doping, wherein, described zinc salt is Zn (NO3)2·6H2O or Zn (NO3)2。
The NiO of a kind of doping, wherein, the NiO of described doping uses the preparation side of the NiO of as above doping described in any one Method is prepared from.
A kind of preparation method of light emitting diode, wherein, including step:
A, deposit a hole injection layer on substrate；Wherein, the material of described hole injection layer is the NiO of doping as mentioned above；
B, then deposition of hole transport layer are on hole injection layer；
C, then deposition quantum dot light emitting layer are on hole transmission layer；
D, finally deposition electron transfer layer are on quantum dot light emitting layer, and evaporation cathode is on electron transfer layer, obtains luminous two Pole is managed.
A kind of light emitting diode, wherein, described light emitting diode quotes the preparation method of light emitting diode as above It is prepared from.
Beneficial effect: the present invention can prepare the NiO of doping at low temperatures.It addition, improved by doping Li in NiO The cavity transmission ability of nickel oxide, is then improving the work function of nickel oxide, is ensureing oxidation by mixing Mg or Cu or Zn In the case of the work function of nickel does not reduces, improve the ability of its hole transport.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method preferred embodiment of a kind of light emitting diode of the present invention.
Fig. 2 is the structural representation of QLED device of the present invention.
Detailed description of the invention
The present invention provides the NiO of a kind of doping, light emitting diode and preparation method thereof, for making the purpose of the present invention, technology Scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.Should be appreciated that described herein specifically Embodiment only in order to explain the present invention, is not intended to limit the present invention.
The present invention provides the preparation method preferred embodiment of the NiO of a kind of doping, and its preparation method includes step:
Nickel salt, the first doping salt and the second doping salt are mixed in deionized water or 2-methyl cellosolve, add glycine Or at least one in acetylacetone,2,4-pentanedione, then heating (preferably, heating-up temperature is 150 ~ 200 DEG C), prepares LixMyNiO； Wherein, the first doping salt is lithium salts, and the second doping salt is magnesium salt, mantoquita or zinc salt；LixMyIn NiO, M=Mg or Cu or Zn, 0 ＜ x ＜ 1,0 ＜ y ＜ 1.Wherein, the numerical value of x and y can regulate according to different hole transmission layers or different preparation conditions.
Preferably, the present invention is after adding glycine or acetylacetone,2,4-pentanedione, it is also possible to add 5 ~ 10uL(such as 7uL or 8uL) NH3•H2O solution.This is because by adding a small amount of ammonia, be possible to prevent the stability of the hydrolysis of solution, more conducively solution.
The Li of the present inventionxMyNiO(wherein M=Mg or Cu or Zn；0<x<1；0 < y < 1) preparation temperature is low, can be at 150-200 The nickel oxide of doping is prepared within the temperature range of DEG C.It addition, the present invention improves the hole of nickel oxide in NiO by doping Li Transmittability, is then improving the work function of nickel oxide, is injecting effect improving nickel oxide hole by mixing Mg or Cu or Zn While rate, do not reduce the work function of nickel oxide.Why the present invention selects this several metals, be because these several metals from Sub-radius (Li+=0.076nm、Mg2+=0.072nm、Cu2+=0.073nm) and in Ni2+Ionic radius (0.069nm) compare and connect Closely, so these are metal-doped after nickel oxide, lattice comparison match.NiO of the present invention is not limited to Mg or Cu or Zn that adulterate, Multiple element can also be mixed, such as, mix any two or three in Mg, Cu, Zn.
Preferably, heretofore described nickel salt can be but be not limited to Ni (NO3)2·6H2O。
Preferably, heretofore described lithium salts can be but be not limited to LiNO3。
Preferably, heretofore described magnesium salt can be but be not limited to Mg (NO3)2。
Preferably, heretofore described mantoquita can be but be not limited to Cu (NO3)2·2.5H2O。
Preferably, heretofore described zinc salt can be but be not limited to Zn (NO3)2·6H2O or Zn (NO3)2。
Below by some embodiments, the preparation method of the NiO of a kind of doping of the present invention is described in detail.
Embodiment 1
By the Ni (NO of 0.8mmol3)2•6H2Cu (the NO of O and 0.015mmol3)2·2.5H2O(or Zn (NO3)2•6H2O or Zn (NO3)2) and 0.05mmolLiNO3It is dissolved in 10mL deionized water, adds 0.1mol glycine, be subsequently adding the NH of 8uL3•H2O Solution.Then by the solution deposition that configured to the substrate containing hearth electrode, 170 DEG C of heating, generate LixCuyNiO thin film (or LixZnyNiO thin film), wherein, wherein the numerical value of x and y can come according to different hole transmission layers or different preparation conditions Regulation.
Embodiment 2
By the Ni (NO of 0.8mmol3)2•6H2Cu (the NO of O and 0.015mmol3)2·2.5H2O(or Zn (NO3)2•6H2O or Zn (NO3)2) and 0.05mmolLiNO3It is dissolved in 10mL deionized water, adds 0.05mol glycine and the acetylacetone,2,4-pentanedione of 5ul, then Add the NH of 8uL3•H2O solution.Then by the solution deposition that configured to the substrate containing hearth electrode, 170 DEG C of heating, generate LixCuyNiO thin film (or LixZnyNiO thin film), wherein, wherein the numerical value of x and y can according to different hole transmission layers or Different preparation conditions regulates.
Embodiment 3
By the Ni (NO of 0.8mmol3)2•6H2Mg (the NO of O and 0.015mmol3)2And 0.05mmolLiNO3It is dissolved in the 2-of 10mL In methoxyethanol solution, add in the acetylacetone,2,4-pentanedione solution of 10uL, add the NH of 7uL3•H2O solution.Then will configure Solution deposition on the substrate containing hearth electrode, 190 DEG C of heating, generate LixMgyNiO thin film, wherein, wherein the numerical value of x and y can To regulate according to different hole transmission layers or different preparation conditions.
Embodiment 4
By the Ni (NO of 0.8mmol3)2•6H2Mg (the NO of O and 0.015mmol3)2And 0.05mmolLiNO3It is dissolved in the 2-of 10mL In methoxyethanol solution, add in the acetylacetone,2,4-pentanedione solution of 8uL and the glycine of 0.02mol, add the NH of 7uL3•H2O is molten Liquid.Then by the solution deposition that configured to the substrate containing hearth electrode, 190 DEG C of heating, generate LixMgyNiO thin film, its In, wherein the numerical value of x and y can regulate according to different hole transmission layers or different preparation conditions.Based on above-mentioned side Method, the present invention also provides for the NiO of a kind of doping, and wherein, the NiO particle of described doping quotes as above preparation side described in any one Method is prepared from.The NiO preparation temperature of present invention doping is low, can prepare within the temperature range of 150-200 DEG C.Separately Outward, the NiO particle of present invention doping, in the case of the work function ensureing nickel oxide does not reduces, improves nickel oxide hole and injects Efficiency.
The present invention also provides for the flow chart of the preparation method preferred embodiment of a kind of light emitting diode, as it is shown in figure 1, its In, including step:
S100, deposition of hole implanted layer are on substrate, and wherein, the material of described hole injection layer is the NiO of doping as mentioned above；
S200, then deposition of hole transport layer are on hole injection layer；
S300, then deposition quantum dot light emitting layer are on hole transmission layer；
S400, finally deposition electron transfer layer are on quantum dot light emitting layer, and evaporation cathode is on electron transfer layer, obtains luminescence Diode.
Use the NiO material as hole injection layer of present invention doping so that before not reducing nickel oxide work function Put, improve its current-carrying electrons transmittability, the injection barrier in reduction hole, thus improve the efficiency of QLED.
Further, in step S100, substrate of the present invention can be ito substrate, and described ito substrate can be as sun Pole uses.The present invention can prepare high-quality thin film on the substrate.It addition, prepare on the substrate QLED device it Before, described substrate is carried out by the present invention.The cleaning process of substrate specifically includes: the substrate (such as ito substrate) that will be patterned into First use dry non-dust cloth and a moistening wiping of non-dust cloth, remove the big dust in surface and granule, be placed in the most in order Carrying out ultrasonic cleaning in cleaning mixture, ultra-pure water, acetone water and isopropanol, ultrasonic being both needed to of each of the above step continues 15 minutes left sides Right.After ultrasonic completing, substrate is positioned over dry for standby in cleaning oven.After substrate is dried, the present invention also uses ultraviolet smelly Oxygen processes (Ultraviolet Ozone) substrate surface 10 ~ 15min(such as 12min), to remove substrate surface attachment further Organic substance also improves the work function of substrate, and this process may be used without gas ions and processes (Plasma treatment) and complete.
In step S100 of the present invention, the method for spin coating is used to deposit a hole injection layer on substrate；Wherein, described hole The material of implanted layer is the NiO, i.e. Li of doping as mentioned abovexMyNiO(wherein M=Mg or Cu or Zn, 0 < x < 1,0 < y < 1).Spin coating Time different rotating speeds (preferably, rotating speed is between 2000 ~ 6000rpm) can be used to regulate the thickness of film, then in 150 ~ 200 DEG C (such as 180 DEG C) add and are thermally generated LixMyNiO thin film.This step can be annealed in atmosphere, can also be moved back in nitrogen atmosphere Fire, but different annealing atmosphere has different performances, with specific reference to being actually needed selective annealing atmosphere.
In step S200 of the present invention, use method one layer of hole transmission layer of deposition of spin coating or evaporation in hole injection layer On, the material of conventional hole transmission layer can be TFB, PVK, Poly-TPD, TCTA or CBP etc. or be its combination in any Mixture, can also be other high performance hole mobile material.
In step S300 of the present invention, by any one quantum dot or other gold-tinted quantum of common red, green, blue three kinds Point is deposited on hole transmission layer as the material of quantum dot light emitting layer, and this step quantum dot can be containing cadmium or without cadmium.
In step S400 of the present invention, on quantum dot light emitting layer, and then deposit electron transfer layer, most common of which electricity The material of sub-transport layer is the N-shaped ZnO with high electronic transmission performance, can also be the metals such as the Ca of low work function, Ba, also Can be CsF, LiF, CsCO3And Alq3Deng compound-material.Finally, the substrate having deposited each functional layer is placed in evaporation storehouse Silver or aluminum by mask plate heat one layer of about 100nm of evaporation are as negative electrode.Preferably, described negative electrode is silver.
It, after device has been deposited with, is packaged by the present invention, it is possible to use conventional machine encapsulation can also use Simple manually encapsulation.But the process of whole encapsulation must be below in the atmosphere of 0.1ppm entering at oxygen content and water content OK, to protect the stability of device.
The present invention also provides for a kind of light emitting diode, and wherein, described light emitting diode quotes light-emitting diodes as above The preparation method of pipe is prepared from.
Shown in Fig. 2, the structural representation of a kind of light emitting diode preferred embodiment of the present invention, as in figure 2 it is shown, from Lower and on include successively: substrate 1, substrate (anode) 2, hole injection layer 3, hole transmission layer 4, quantum dot light emitting layer 5, electronics pass Defeated layer 6 and negative electrode 7, wherein, the material of described hole injection layer is the NiO of doping of the present invention.This light-emitting diodes of the present invention Pipe has higher efficiency and excellent electronic transmission performance.
Compared with prior art, present invention have the advantage that
1、LixMyNiO(wherein M=Mg or Cu or Zn;0<x<1;0 < y < 1) preparation temperature is low, can be the temperature of 150-200 DEG C The NiO of doping is prepared in the range of degree.
2, the NiO of doping prepared by the present invention, while improving NiO hole injection efficiency, does not reduce the work function of NiO, Can regulate by mixing metal or improve the work function of NiO, to lower injection barrier, mix Li element simultaneously and improve The carrier charge velocity of NiO.
3, can be by mixing multiple element, such as: Mg or Cu or Zn, or the mixing of these three element.
4, the present invention is by adding a small amount of ammonia, to prevent the stability of the hydrolysis of solution, more conducively precursor solution.
In sum, the NiO of a kind of doping of present invention offer, light emitting diode and preparation method thereof, at LixMyNiO is thin During film preparation, add a small amount of ammonia, to ensure the stability of precursor solution.Ensureing the work function of nickel oxide not In the case of reduction, improve the ability of its hole transport, reduce the injection barrier in hole；Make the NiO system of the above-mentioned doping of employing Standby light emitting diode achieves higher efficiency.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can To be improved according to the above description or to convert, all these modifications and variations all should belong to the guarantor of claims of the present invention Protect scope.

Claims (9)

1. the preparation method of NiO of a doping, it is characterised in that include step:
Nickel salt, the first doping salt and the second doping salt are mixed in deionized water or 2-methyl cellosolve, add glycine Or at least one in acetylacetone,2,4-pentanedione, then heat, prepare LixMyNiO；Wherein, the first doping salt is lithium salts, and second mixes Carnallite is magnesium salt, mantoquita or zinc salt；LixMyIn NiO, M=Mg or Cu or Zn, 0 ＜ x ＜ 1,0 ＜ y ＜ 1.
The preparation method of the NiO of doping the most according to claim 1, it is characterised in that adding glycine or levulinic After at least one in ketone, it is additionally added NH3·H2O solution.
The preparation method of the NiO of doping the most according to claim 1, it is characterised in that described nickel salt is Ni (NO3)2· 6H2O, described lithium salts is LiNO3。
The preparation method of the NiO of doping the most according to claim 1, it is characterised in that described magnesium salt is Mg (NO3)2。
The preparation method of the NiO of doping the most according to claim 1, it is characterised in that described mantoquita is Cu (NO3)2· 2.5H2O。
The preparation method of the NiO of doping the most according to claim 1, it is characterised in that described zinc salt is Zn (NO3)2· 6H2O or Zn (NO3)2。
7. the NiO of a doping, it is characterised in that the NiO of described doping uses the doping as described in any one of claim 1 ~ 6 The preparation method of NiO be prepared from.
8. the preparation method of a light emitting diode, it is characterised in that include step:
A, deposition of hole implanted layer are on substrate；Wherein, the material of described hole injection layer is doping described in claim 7 NiO；
B, then deposition of hole transport layer are on hole injection layer；
C, then deposition quantum dot light emitting layer are on hole transmission layer；
D, finally deposition electron transfer layer are on quantum dot light emitting layer, and evaporation cathode is on electron transfer layer, obtains luminous two Pole is managed.
9. a light emitting diode, it is characterised in that described light emitting diode quotes light emitting diode as claimed in claim 8 Preparation method be prepared from.
CN201610821482.6A 2016-09-14 2016-09-14 The NiO of a kind of doping, light emitting diode and preparation method thereof Pending CN106252529A (en)

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CN106784124A (en) * 2016-12-23 2017-05-31 浙江大学 One kind is based on P NiO/N ZnO:Ultraviolet detector of Al heterojunction structures and preparation method thereof
CN106784124B (en) * 2016-12-23 2018-04-20 浙江大学 One kind is based on P NiO/N ZnO:Ultraviolet detector of Al heterojunction structures and preparation method thereof
CN107482122A (en) * 2017-08-23 2017-12-15 中节能万润股份有限公司 A kind of perovskite solar cell and preparation method
CN107482122B (en) * 2017-08-23 2019-12-17 中节能万润股份有限公司 perovskite solar cell and preparation method
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