CN109980107A - CuMO2And preparation method thereof, luminescent device - Google Patents
CuMO2And preparation method thereof, luminescent device Download PDFInfo
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- CN109980107A CN109980107A CN201711464350.3A CN201711464350A CN109980107A CN 109980107 A CN109980107 A CN 109980107A CN 201711464350 A CN201711464350 A CN 201711464350A CN 109980107 A CN109980107 A CN 109980107A
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- H10K50/00—Organic light-emitting devices
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Abstract
The present invention provides a kind of CuMO2Preparation method, comprising the following steps: provide cupric salt solution reducing agent is added in the cupric salt solution under an inert atmosphere, the copper ion in the cupric salt generates cuprous ion under the action of reducing agent, obtains cuprous ion solution；M saline solution is provided, the M is selected from one of Ga, In, Cr, Al, and the pH value of the M saline solution is 5-6.5；Under an inert atmosphere, the M salting liquid is added in the cuprous ion solution, heating reaction generates CuMO2。
Description
Technical field
The invention belongs to field of display technology more particularly to a kind of CuMO2And preparation method thereof, luminescent device.
Background technique
Light emitting diode with quantum dots (QLED) have narrow FWHM (peak width at half height), Color tunable and can solution method preparation etc.
Excellent feature has become the candidate of next-generation display science and technology.Therefore different researcher studies from different angles
QLED, including the research of QDs (quantum dot), HTL (hole transmission layer), ETL (electron transfer layer) and electrode；There are also to device
The properity of part and the research of stability, and in these researchs most by commercial interest a little be exactly device stability.
At present in QLED device, since the acid and hygroscopic property of PEDOT:PSS hole injection layer all causes difference to ITO and device
The damage and decaying of degree, therefore the stability of device need to be improved.In the report in substitution PEODT:PSS at present, make
With it is most be exactly metal oxide, currently used for the limited material of hole transmission layer, and with preferable hole mobile material
Metal oxide is few, predominantly binary compound, embodies a concentrated reflection of molybdenum oxide, nickel oxide or copper oxide and concentrates material.Cause
This, the metal oxide materials with preferable hole transport performance need further to be developed.
Summary of the invention
The purpose of the present invention is to provide a kind of CuMO2And preparation method thereof, it is desirable to provide it is a kind of to have preferable sky
Cave transmission performance, and the ternary metal oxide material of luminescent device can be used for.
The purpose of the present invention is to provide one kind to contain CuMO2Luminescent device.
For achieving the above object, The technical solution adopted by the invention is as follows:
A kind of CuMO2Preparation method, comprising the following steps:
Cupric salt solution is provided, reducing agent, the divalent are added in the cupric salt solution under an inert atmosphere
Copper ion in mantoquita generates cuprous ion under the action of reducing agent, obtains cuprous ion solution；
M saline solution is provided, the M is selected from one of Ga, In, Cr, Al, and the pH value of the M saline solution is 5-
6.5；Under an inert atmosphere, the M salting liquid is added in the cuprous ion solution, heating reaction generates CuMO2。
Correspondingly, a kind of CuMO2, the CuMO2For the CuMO of above method preparation2。
And a kind of luminescent device, including anode and cathode, and setting between the anode and the cathode folded
Layer, the lamination include the hole transmission layer and luminescent layer that stacking combines, and the hole transmission layer is arranged in the anode and institute
It states between luminescent layer, and the material of the hole transmission layer is the CuMO of above method preparation2, wherein M be selected from Ga, In, Cr,
One of Al.
CuMO provided by the invention2Preparation method, using solwution method, after bivalent cupric ion is reduced to cuprous ion,
With M saline solution hybrid reaction, CuMO is prepared2.This method reaction condition is mild, the CuMO being prepared2, there is preferable point
Performance is dissipated, can be used as the hole transport layer material of luminescent device.Further, as hole transport layer material in use, can be with
It is directly prepared in situ in the functional layer of luminescent device or electrode, is conducive to the stability for improving hole transmission layer.
CuMO provided by the invention2, not only there is excellent optics light transmittance, it is often more important that, there is suitable energy level
Structure (conduction level is about -5.3eV, is conducive to the injection in hole) and higher hole mobility (10-2-101cm2V-1s-1),
When hole transmission layer as luminescent device, the mobility of carrier can be improved, mainly improve the injectability in hole,
Further balance injection, the transmission in hole and electronics.Further, since the CuMO2Itself has preferable stability, therefore,
When as luminescent device, the stability of device can be improved.
Luminescent device provided by the invention, due to using CuMO2As hole transmission layer, therefore, not only have preferable
Hole transport and injection efficiency improve carrier mobility, and can be improved the stability of device.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of eurymeric QLED device provided in an embodiment of the present invention；
Fig. 2 is the structural schematic diagram of transoid QLED device provided in an embodiment of the present invention.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
The embodiment of the invention provides a kind of CuMO2Preparation method, comprising the following steps:
S01., cupric salt solution is provided, reducing agent is added in the cupric salt solution under an inert atmosphere, it is described
Copper ion in cupric salt generates cuprous ion under the action of reducing agent, obtains cuprous ion solution；
S02. M saline solution is provided, the M is selected from one of Ga, In, Cr, Al, and the pH value of the M saline solution
For 5-6.5；Under an inert atmosphere, the M salting liquid is added in the cuprous ion solution, heating reaction generates CuMO2。
CuMO provided in an embodiment of the present invention2Preparation method, using solwution method, by bivalent cupric ion be reduced to it is cuprous from
After son, with M saline solution hybrid reaction, CuMO is prepared2.This method reaction condition is mild, the CuMO being prepared2, have preferable
Dispersion performance, can be used as the hole transport layer material of luminescent device.Further, as hole transport layer material in use,
It can be directly prepared in situ in the functional layer of luminescent device or electrode, be conducive to the stability for improving hole transmission layer.
Specifically, the cupric salt in the cupric salt solution is the cupric that can be dissolved in water in above-mentioned steps S01
Salt, including but not limited to copper chloride, copper sulphate etc., but do not use copper nitrate, to avoid nitrate anion aoxidize it is subsequent obtain it is cuprous
Ion.In the embodiment of the present invention, the reducing agent use weak reductant, to avoid the reducing agent directly by bivalent cupric ion also
It originally was metal copper simple substance.Preferably, the reducing agent is selected from least one of sodium thiosulfate, sodium citrate.Compared to second
The reducing agents such as glycol work, it is not only environmentally protective, do not have bio-toxicity, and for can effectively mention in aqueous phase reactions system
The high redox reaction efficiency with bivalent cupric ion, and the reducing degree for controlling bivalent cupric ion be only limitted to be formed it is cuprous from
Son, rather than it is reduced to metal copper simple substance.
In the embodiment of the present invention, reducing agent directly can be added in the cupric salt solution, can also provide respectively
Then cupric salt solution and reducing agent solution blend the two to obtain hybrid reaction system.Divalent of the embodiment of the present invention
The reaction that copper ion in mantoquita generates cuprous ion under the action of reducing agent carries out in an inert atmosphere.Specifically, when straight
When connecing the addition reducing agent in the cupric salt solution, cupric salt can be drained in a manner of first using through inert gas
The oxygen of solution；Then inert atmosphere is kept, reducing agent is added.When providing cupric salt solution and reducing agent solution respectively, so
When the two being blended to obtain hybrid reaction system afterwards, cupric can be drained respectively by the way of through inert gas
Oxygen in salting liquid and reducing agent solution, then keeps inert atmosphere, by the two mixed processing.
In above-mentioned steps S02, the M salt in the M saline solution is the M salt that can be dissolved in water, including but not limited to chlorate,
Acetate etc., and be not the nitrate of M, cuprous ion is aoxidized to avoid nitrate ion.M saline solution is provided, M is selected from
One of Ga, In, Cr, Al, therefore, M ion form [M (OH)4(H2O)2]-Or M (OH)3.3H2O.Due to [M (OH)4
(H2O)2]-Or M (OH)3.3H2O is strong acid weak base salt, and therefore, in order to avoid hydrolysis, the pH value of the M saline solution is 5-6.5.
Further, under an inert atmosphere, the M salting liquid is added in the cuprous ion solution, heating reaction
Generate CuMO2, reaction process are as follows: Cu1++[M(OH)4(H2O)2]-→CuMO2+H2O or Cu1++[M(OH)3(H2O)3]0→
CuMO2+H3O+。
In the embodiment of the present invention, under an inert atmosphere, the M salting liquid is added in the cuprous ion solution, is added
Thermal response generates CuMO2The step of in, heat reaction temperature be 180-250 DEG C, the reaction time be 1-3 hours.If reaction temperature
It is too short to spend the low or reaction time, then reflects insufficient, is unable to get the CuMO of high yield2, and CuMO2In be readily incorporated other
Impurity reduces product purity.If reaction temperature is excessively high or the reaction time is too long, on the one hand, the CuMO of generation2It can further react
It such as decomposes reaction, material property variation occurs for obtained product；On the other hand, the CuMO of generation2Particle is excessive, Wu Fayou
Effect dispersion, and it is used as hole mobile material.
Further, the M salting liquid is added in the cuprous ion solution, heating reaction generates CuMO2Step
It further include to obtained CuMO after rapid2Start the cleaning processing, the method for the cleaning treatment are as follows: successively using ammonium hydroxide, nitric acid and
The CuMO that deionized water obtains reaction2It is washed.By the washing sequence, first passing through ammonium hydroxide will be remaining in reaction system
Weak acid neutralizes, and then using the other impurities generated in nitre acid dissolution reaction, such as cuprous oxide or copper, further passes through water
Remove the lysigenous salt of nitric acid.
Further, the CuMO that can will be obtained2It is dispersed in alcoholic solution.
Correspondingly, the embodiment of the invention also provides a kind of CuMO2, the CuMO2For the CuMO of above method preparation2。
CuMO provided in an embodiment of the present invention2, not only there is excellent optics light transmittance, it is often more important that, it is suitable to have
Level structure (conduction level be about -5.3eV, be conducive to the injection in hole) and higher hole mobility (10-2-101cm2V-1s-1), when hole transmission layer as luminescent device, the mobility of carrier can be improved, mainly improve the note in hole
Enter ability, further balances injection, the transmission in hole and electronics.Further, since the CuMO2Itself there is preferable stablize
Property, therefore, when being used as luminescent device, the stability of device can be improved.
And a kind of luminescent device, including anode and cathode, and setting between the anode and the cathode folded
Layer, the lamination include the hole transmission layer and luminescent layer that stacking combines, and the hole transmission layer is arranged in the anode and institute
It states between luminescent layer, and the material of the hole transmission layer is the CuMO of above method preparation2, wherein M be selected from Ga, In, Cr,
One of Al.
Luminescent device provided in an embodiment of the present invention, due to using CuMO2As hole transmission layer, therefore, not only have
Preferable hole transport and injection efficiency, improve carrier mobility, and can be improved the stability of device.
Wherein, the luminescent device further includes electronic work ergosphere, and the electronic work ergosphere is that electron transfer layer and electronics are infused
Enter at least one layer in layer.
Luminescent layer described in the embodiment of the present invention is quantum dot light emitting layer or organic luminous layer.When the luminescent layer is quantum dot
When luminescent layer, the luminescent device corresponds to QLED device；When the luminescent layer is organic layer, the luminescent device is corresponded to
OLED (Organic Light Emitting Diode) device.Preferably, the luminescent device is QLED device.
In the embodiment of the present invention, the QLED device can be eurymeric QLED device, or transoid QLED device.Make
It is incorporated in described for a kind of specific embodiment as shown in Figure 1, the QLED device is eurymeric QLED device, including substrate 1
The anode 2 on 1 surface of substrate, hole injection layer 3, the hole transmission layer 4, quantum dot light emitting layer being successively set on the anode 2
5, electron transfer layer 6 and cathode 7.As another embodiment, as shown in Fig. 2, the QLED device is transoid QLED device,
Including substrate 1, combining station is successively set on electron transfer layer 6, the amount on 7 surface of cathode in the cathode 7 of the substrate surface
Son point luminescent layer 5, hole transmission layer 4, hole injection layer and anode 2.
Specifically, the selection of substrate 1 does not limit strictly, hard substrates or flexible substrate, hard substrates packet can be used
It includes but is not limited to glass plate.
Anode 2 can be selected from blended metal oxide, including but not limited to indium doping tin oxide (ITO), fluorine-doped tin oxide
(FTO), antimony-doped tin oxide (ATO), aluminium-doped zinc oxide (AZO), Ga-doped zinc oxide (GZO), indium doping zinc oxide
(IZO), magnesium doping zinc-oxide (MZO), aluminium doping one of magnesia (AMO) or a variety of selected from doping or non-can also be mixed
Clip the combination electrode of metal between miscellaneous transparent metal oxide, including but not limited to AZO/Ag/AZO, AZO/Al/AZO,
ITO/Ag/ITO、ITO/Al/ITO、ZnO/Ag/ZnO、ZnO/Al/ZnO、TiO2/Ag/TiO2、TiO2/Al/TiO2、ZnS/Ag/
ZnS, ZnS/Al/ZnS's is one or more.
Hole injection layer 3 can be NiO, CuO, CuS, MoO3In any one；Or be TFB, PVK, Poly-TPD,
At least one of TCTA, CBP.
The material of hole transmission layer 4 is above-mentioned CuMO2Or CuMO2With the mixture of conventional hole mobile material, often
The hole mobile material of rule can be any one in NiO, CuO, CuS；Or be TFB, PVK, Poly-TPD, TCTA,
At least one of CBP.Hole transmission layer 4 with a thickness of 20-30nm.The too thin then electric conductivity of the thickness of hole transmission layer 4 is weaker,
And cause both hole and electron uneven；The thickness of hole transmission layer 4 is too thick, is unfavorable for hole transport into luminescent layer.
The material of quantum dot light emitting layer 5 can be common red, green, blue and yellow light quantum and infrared and ultraviolet light quantum
At least one of point, specifically can be selected from II-VI group compound, III-V compound, II-V compounds of group, III-VI chemical combination
One of object, group IV-VI compound, I-III-VI group compound, II-IV-VI compounds of group or IV race simple substance are a variety of.Amount
Son point luminescent layer 4 with a thickness of 10-100nm.
Electron transfer layer 6 is the metal oxide with electron transport property, such as TiO2、ZnO、SnO2Deng.Electron transfer layer
6 with a thickness of 30-60nm.
Cathode 7 can choose the metal or alloy such as Ag, Al, Cu, Au.
Correspondingly, the embodiment of the invention also provides a kind of preparation methods of QLED device.
As an implementation, the QLED device preparation method the following steps are included:
E01., anode grid substrate is provided, is sequentially prepared hole injection layer in the anode grid substrate；
E02. CuMO is deposited on the hole injection layer2, prepare hole transmission layer；
E03. it is sequentially prepared quantum dot light emitting layer, electron transfer layer and cathode on the hole transport layer.
As another embodiment, the preparation method of the QLED device, comprising the following steps:
Q01., cathode base is provided, electron transfer layer, quantum dot light emitting layer are sequentially prepared on the cathode base；
Q02. hole transmission layer is prepared on the quantum dot light emitting layer；
Q03. it is sequentially prepared hole injection layer and anode on the hole transport layer.
Specifically, the material of each layer is as described above in above two method, in order to save length, do not repeating herein.
Deposit CuMO2Method, including chemical method and physical method, wherein the physical method includes physical coating method and molten
Liquid processing method.Specifically, chemical method include: chemical vapour deposition technique, successive ionic layer adsorption and reaction method, anodizing,
Strike, coprecipitation.The physical coating method includes: thermal evaporation coating method, electron beam evaporation deposition method, magnetron sputtering
Method, multi-arc ion coating embrane method, physical vaporous deposition, atomic layer deposition method, pulsed laser deposition etc..The solution processing method
Including spin-coating method, print process, impact system, dip-coating method, infusion method, spray coating method, roll coating process, casting method, slit coating method,
Strip rubbing method.The embodiment of the present invention preferably uses solution processing method that uniform and fine and close interface-modifying layer is prepared.Into one
Step is preferred, in deposition CuMO2Afterwards, it is made annealing treatment under conditions of 70-9 DEG C, is more preferably moved back under the conditions of 80 DEG C
Fire processing.
In the embodiment of the present invention, the method that the cathode, anode can be deposited by using mask plate is realized, the hole
Implanted layer, quantum dot light emitting layer, electron transfer layer can be realized using conventional deposition method, specifically, reference can be made to preparation circle
The above method of face decorative layer.
The anode grid substrate or the cathode base further include cleaning treatment before depositing functional material.As a kind of excellent
Select mode, by the anode grid substrate or the cathode base be placed in acetone, washing lotion, deionized water and isopropanol in order into
Row ultrasonic cleaning, each of the above step ultrasound are both needed to continue 10-20 minutes, more preferably 15 minutes or so.It will after the completion of ultrasound
The anode grid substrate or the cathode base are placed in cleaning oven and are dried for standby.
It is illustrated combined with specific embodiments below.
Embodiment 1
A kind of CuMO2Preparation method, comprising the following steps:
5mmol copper chloride is dissolved into configuration copper chloride solution (solution A) in 5ml water, is passed through inert gas to exclude water
The oxygen of middle dissolution；Then weak reductant, such as 10mmol sodium thiosulfate are dissolved into configuration weak reductant solution in 5ml water
(B solution), is passed through inert gas, to exclude oxygen therein.5mmol gallium chloride is dissolved into 5ml aqueous solution, and by its pH
It is adjusted between 5-6.5, C solution is configured, and be passed through in a large amount of inert gas, to exclude oxygen in water gas.
By B solution addition solution A be stirred to react, make wherein cupric be reduced into monovalence copper, after complete reaction；And then
C solution is added, and is sufficiently stirred.Then obtained mixed solution is added in reaction kettle, reacts 2h in 200 DEG C of heating, most
Obtained precipitating will will be reacted afterwards to wash by ammonium hydroxide, nitric acid and deionized water, be then dispersed in alcoholic solution.
Embodiment 2
A kind of CuMO2Preparation method, comprising the following steps:
5mmol copper acetate is dissolved into configuration copper chloride solution (solution A) in 5ml water, is passed through inert gas to exclude water
The oxygen of middle dissolution；Then weak reductant, such as 10mmol sodium citrate are dissolved into configuration weak reductant solution (B in 5ml water
Solution), it is passed through inert gas, to exclude oxygen therein.5mmol acetic acid gallium is dissolved into 5ml aqueous solution, and by its pH tune
Section configures C solution, and be passed through in a large amount of inert gas, to exclude oxygen in water gas between 5-6.5.
Will B solution be added solution A in be stirred to react, make wherein cupric be reduced into monovalence copper, after complete reaction；Immediately
C solution is added, and is sufficiently stirred.Then obtained mixed solution is added in reaction kettle, reacts 2h in 200 DEG C of heating, most
Obtained precipitating will will be reacted afterwards to wash by ammonium hydroxide, nitric acid and deionized water, be then dispersed in alcoholic solution.
Embodiment 3
A kind of preparation method of QLED device, comprising the following steps:
The deposition of hole implanted layer on ITO substrate, anneal at 150 DEG C 15min；
The CuMO that embodiment 1 obtains is deposited on hole injection layer2, anneal at 150 DEG C 30min, prepares hole transmission layer；
Quantum dot light emitting layer is prepared on the hole transport layer, and electron transfer layer is deposited on quantum dot light emitting layer,
Cathode is prepared on electron transfer layer.
Embodiment 4
A kind of preparation method of QLED device, comprising the following steps:
Electron transfer layer, quantum dot light emitting layer are prepared on ITO substrate；
The CuMO that embodiment 1 obtains is deposited on the quantum dot light emitting layer2, anneal at 150 DEG C 30min, prepares hole
Transport layer；
It is sequentially prepared hole injection layer and anode on the hole transport layer.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of CuMO2Preparation method, which comprises the following steps:
Cupric salt solution is provided, reducing agent, the cupric salt are added in the cupric salt solution under an inert atmosphere
In copper ion generate cuprous ion under the action of reducing agent, obtain cuprous ion solution；
M saline solution is provided, the M is selected from one of Ga, In, Cr, Al, and the pH value of the M saline solution is 5-6.5；
Under an inert atmosphere, the M salting liquid is added in the cuprous ion solution, heating reaction generates CuMO2。
2. CuMO as described in claim 12Preparation method, which is characterized in that under an inert atmosphere, the M salting liquid is added
Enter into the cuprous ion solution, heating reaction generates CuMO2The step of in, heat reaction temperature be 180-250 DEG C, instead
It is 1-3 hours between seasonable.
3. CuMO as described in claim 12Preparation method, which is characterized in that the reducing agent be selected from sodium thiosulfate, lemon
At least one of lemon acid sodium.
4. CuMO as described in any one of claims 1-32Preparation method, which is characterized in that in the cupric salt solution
Cupric salt is the cupric salt that can be dissolved in water, and is not copper nitrate；And/or
M salt in the M saline solution is the M salt that can be dissolved in water, and is not the nitrate of M.
5. CuMO as described in any one of claims 1-32Preparation method, which is characterized in that the M salting liquid is added to
In the cuprous ion solution, heating reaction generates CuMO2The step of after, further include to obtained CuMO2It starts the cleaning processing,
The method of the cleaning treatment are as follows: the CuMO that successively reaction is obtained using ammonium hydroxide, nitric acid and deionized water2It is washed.
6. a kind of CuMO2, which is characterized in that the CuMO2For the CuMO of any one of claim 1-5 the method preparation2。
7. a kind of luminescent device, which is characterized in that including anode and cathode, and setting is between the anode and the cathode
Lamination, the lamination includes the hole transmission layer and luminescent layer that stacking combines, and the hole transmission layer is arranged in the anode
Between the luminescent layer, and the material of the hole transmission layer is any one of claim 1-5 the method preparation
CuMO2, wherein M is selected from one of Ga, In, Cr, Al.
8. luminescent device as claimed in claim 7, which is characterized in that the luminescent device further includes electronic work ergosphere, described
Electronic work ergosphere is at least one layer in electron transfer layer and electron injecting layer.
9. luminescent device as claimed in claim 7 or 8, which is characterized in that the hole transmission layer with a thickness of 20-30nm.
10. luminescent device as claimed in claim 7 or 8, which is characterized in that the luminescent layer is quantum dot light emitting layer or organic
Luminescent layer.
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| CN109980107B (en) | 2020-12-01 |
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