CN108439456A - The preparation method of ZnLiMgO nano particles and product prepared therefrom - Google Patents
The preparation method of ZnLiMgO nano particles and product prepared therefrom Download PDFInfo
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- CN108439456A CN108439456A CN201810336972.6A CN201810336972A CN108439456A CN 108439456 A CN108439456 A CN 108439456A CN 201810336972 A CN201810336972 A CN 201810336972A CN 108439456 A CN108439456 A CN 108439456A
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/006—Compounds containing, besides zinc, two ore more other elements, with the exception of oxygen or hydrogen
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- H—ELECTRICITY
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Abstract
The invention discloses a kind of preparation method of ZnLiMgO nano particles and products prepared therefrom.Under room temperature and alkaline environment, lithium salts and alcohol ether are mixed, the first reaction system is obtained；Zinc salt is added into first reaction system, ZnLiO dispersions are obtained by the reaction；Magnesium salts is added into ZnLiO dispersions, ZnLiMgO nano particles are obtained by the reaction.It is the straight chain alcohol ether of C3 C5 that ZnLiMgO nano particles prepared by the method for the present invention, which have surface ligand, surface ligand,.When the ZnLiMgO nano particles of the present invention are used as the electron transfer layer of luminescent device, good film-forming property, and extend device lifetime.
Description
Technical field
The application belongs to field of semiconductor materials, and in particular to the preparation method of a kind of ZnLiMgO nano particles and by it
The product of preparation.
Background technology
ZnO nano particle is saturating due to its skin effect, bulk effect, quantum size effect and macroscopical tunnel-effect and height
The features such as lightness, polymolecularity, in the products such as the liquid crystal display, thin film transistor (TFT), light emitting diode of semiconductor applications
There is application.
ZnO is 3.3eV, band gap and exciton as a kind of novel wide bandgap semiconductor materials, at room temperature band gap width
Binding energy is larger, has higher electron mobility, is often used as the electron transfer layer of luminescent device.It has however been found that tradition side
ZnO nano particle prepared by method makees luminescent device high energy consumption when electron transfer layer, and short life cannot meet wanting for display industry
It asks.
Invention content
In view of the above technical problems, the application provides the preparation method of a kind of ZnLiMgO nano particles and prepared therefrom
Product.
In order to achieve the above-mentioned object of the invention, this application provides a kind of preparation methods of ZnLiMgO nano particles, including with
Lower step：
S1 under room temperature and alkaline environment, lithium salts and alcohol ether is mixed, the first reaction system is obtained；
Zinc salt is added into first reaction system by S2, and ZnLiO dispersions are obtained after reacting 0.5~48h；
Magnesium salts is added into the ZnLiO dispersions of S2 by S3, and water-bath temperature control is at 15~35 DEG C, 5~60min of ultrasound, reaction
Obtain ZnLiMgO compounds.
In this application, room temperature refers to temperature between 16 DEG C~25 DEG C.
Further, alcohol ether described in above-mentioned steps S1 is the straight chain alcohol ether of C3-C5.Such as：Ethylene glycol monomethyl ether, ethylene glycol
Ether, glycol propyl ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether.
Further, above-mentioned alcohol ether is ethylene glycol monomethyl ether.
Further, alkaline environment described in above-mentioned steps S1 is provided by tetramethylammonium hydroxide.
Further, the molar concentration of above-mentioned tetramethylammonium hydroxide is 0.1~0.3mol/L.
Further, the first reaction system is also one or more with polyethylene glycol, in glycol in above-mentioned steps S1.Example
Such as, polyethylene glycol can be PEG200, PEG400；Glycol can be ethylene glycol, diethylene glycol (DEG), triethylene glycol, tetraethylene glycol.
Further, lithium salts can be selected from but not limited to one in lithium acetate, lithium sulfate, lithium nitrate in above-mentioned steps S1
Kind.
Further, zinc salt can be selected from but not limited to zinc acetate, zinc sulfate, zinc nitrate, methyl-prop in above-mentioned steps S2
One kind in olefin(e) acid zinc.
Further, magnesium salts can be selected from but not limited to magnesium acetate, magnesium sulfate, magnesium nitrate, methyl-prop in above-mentioned steps S3
One kind in olefin(e) acid magnesium.
Further, with the gauge of substance, above-mentioned lithium salts, zinc salt, magnesium salts whole rate of charge be (0.5~1.5):1:
(0.05~0.3).
Further, be added magnesium salts while zinc salt is added in step s 2, addition account for magnesium salts total amount of feeding 0~
50%.
The present invention also provides a kind of ZnLiMgO nano particles, are prepared according to the above method.ZnLiMgO nanometers
In particle, the molar ratio of Zn elements, Li elements and Mg elements is 100:(1~30):(1~30).ZnLiMgO nano particles have
It is ethylene glycol monomethyl ether to have surface ligand, surface ligand.Li exists in the form of interstitial atom in ZnLiMgO nano particles, and Mg is former
The part Zn atoms in lattice are substituted in son, and band gap width is 3.55~3.68eV, meets electron transfer layer pair in luminescent device
The requirement of band gap width.
Advantageous effect：The preparation method of the application can obtain the ZnLiMgO nano particles of doping Li and Mg, wherein Zn members
The molar ratio 100 of element, Li elements and Mg elements:(1~30):(1~30).Through XRD test analysis, mixed using the application method
Miscellaneous ZnLiMgO is wurtzite structure, and wherein Li exists in the form of interstitial atom, and the part Zn in lattice is substituted in Mg atoms
The doping of atom, Li and Mg do not have an impact the crystal structure of ZnO.
In reaction, ethylene glycol monomethyl ether is connected to the surface of ZnLiMgO nano particles as surface ligand, is reacted by controlling
Time regulates and controls the particle size of ZnLiMgO nano particles, obtains suitable size.Since the chain length of small molecule straight chain alcohol ether is closed
It is suitable, the spacing between the ZnLiMgO nano particles as electron transfer layer can be made moderate, to keep electron-transport distance suitable
In, electronics can preferably be matched with hole in luminescent layer, to extend device lifetime.In addition, small molecule straight chain alcohol ether is in second
Dissolubility in alcohol is excellent so that ZnLiMgO nano particles will not reunite in ethanol, and spin coating liquid film forming is uniform, device
Performance gets a promotion.Entire reaction is to carry out at room temperature, avoids pyroreaction, and mild condition is dangerous low.
Description of the drawings
Fig. 1 is the XRD spectra of ZnLiMgO nano particles in Examples 1 to 4 in the application.The corresponding song of Examples 1 to 4
Line is followed successively by A, B, C, D.
Specific implementation mode
Below in conjunction with the application embodiment, technical solutions in the embodiments of the present application is described in detail.It answers
It is noted that described embodiment is only a part of embodiment of the application, rather than whole embodiments.
Embodiment 1：
Include the following steps：
S1 at 25 DEG C, the hydration lithium acetates of 6mmol bis- is mixed with 20mL ethylene glycol monomethyl ethers, are additionally added five water of 6mmol in addition
Tetramethylammonium hydroxide is closed, the first reaction system is obtained.
4mmol Zinc diacetate dihydrates are added into the first reaction system by S2, stir 2h, obtain ZnLiO dispersions.
0.6mmol Magnesium acetate (Mg(OAc)2) tetrahydrates, 15 DEG C of bath temperature, ultrasound are added into the ZnLiMgO dispersions of S2 by S3
20min obtains ZnLiMgO nano particles.
Ethylene glycol monomethyl ether is connected to the surface of ZnLiMgO nano particles as surface ligand.
It is tested through ICP-MS, in ZnLiMgO, the molar ratio of Zn elements, Li elements and Mg elements is 100:24:28.Through
XRD test analysis (as shown in A curves in Fig. 1), ZnLiMgO nano particles are wurtzite structure.It is computed, ZnLiMgO nanometers
The band gap width of particle is 3.57eV.Computational methods are well known to those skilled in the art, such as can pass through UV absorption number
According to calculating, which is not described herein again.
The electron transfer layer of electroluminescent device is made by above-mentioned ZnLiMgO nano particles, and is applied to feux rouges CdSe amounts
On sub- point luminescent diode.The light emitting diode with quantum dots includes adjacent successively ito anode, PEDOT:PSS hole injection layers,
TFB hole transmission layers, CdSe quantum dot luminescent layer, ZnLiMgO electron transfer layers and cathode aluminium.The light emitting diode with quantum dots
Service life T50@1000cd/m2Extension reaches 1937h, other device performances are shown in Table 1.
Embodiment 2：
Include the following steps：
S1 at 22 DEG C, the hydration lithium acetates of 6mmol bis- is mixed with 20mL glycol propyl ethers, are additionally added five water of 6mmol in addition
Tetramethylammonium hydroxide is closed, the first reaction system is obtained.
4mmol Zinc diacetate dihydrates and 0.2mmol Magnesium acetate (Mg(OAc)2) tetrahydrates are added into the first reaction system by S2, stir 2h,
Obtain ZnLiMgO dispersions.
0.4mmol Magnesium acetate (Mg(OAc)2) tetrahydrates, 20 DEG C of bath temperature, ultrasound are added into the ZnLiMgO dispersions of S2 by S3
45min obtains ZnLiMgO nano particles.
Glycol propyl ether is connected to the surface of ZnLiMgO nano particles as surface ligand.
It is tested through ICP-MS, in ZnLiMgO, the molar ratio of Zn elements, Li elements and Mg elements is 100:16:23.Through
XRD test analysis (as shown in B curves in Fig. 1), ZnLiMgO nano particles are wurtzite structure.It is computed, ZnLiMgO nanometers
The band gap width of particle is 3.6eV.Computational methods are well known to those skilled in the art, such as can pass through UV absorption data
It calculates, which is not described herein again.
The electron transfer layer of electroluminescent device is made by above-mentioned ZnLiMgO nano particles, and is applied to feux rouges CdSeS amounts
On sub- point luminescent diode, which includes adjacent successively ito anode, PEDOT:PSS hole injection layers,
TFB hole transmission layers, CdSeS quantum dot light emitting layers, ZnLiMgO electron transfer layers and cathode aluminium.The light emitting diode with quantum dots
Service life T50@1000cd/m2Extension reaches 1594h, other device performances are shown in Table 1.
Embodiment 3
Include the following steps：
S1 at 23 DEG C, 3mmol lithium sulfates is mixed with 10mL ethylene glycol monomethyl ethers, 10mL PEG200, are additionally added in addition
3mmol five is hydrated tetramethylammonium hydroxide, obtains the first reaction system.
3mmol Zinc diacetate dihydrates and 0.1mmol magnesium nitrates are added into the first reaction system by S2, stir 0.5h, obtain
ZnLiMgO dispersions.
S3,0.2mmol magnesium nitrates, 35 DEG C of bath temperature are added into the ZnLiMgO dispersions of S2, and ultrasonic 60min is obtained
To ZnLiMgO nano particles.
Ethylene glycol monomethyl ether is connected to the surface of ZnLiMgO nano particles as surface ligand.
It is tested through ICP-MS, in ZnLiMgO, the molar ratio of Zn elements, Li elements and Mg elements is 100:7:12.Through
XRD test analysis (as shown in C curve in Fig. 1), ZnLiMgO nano particles are wurtzite structure.It is computed, ZnLiMgO nanometers
The band gap width of particle is 3.68eV.Computational methods are well known to those skilled in the art, such as can pass through UV absorption number
According to calculating, which is not described herein again.
The electron transfer layer of electroluminescent device is made by above-mentioned ZnLiMgO nano particles, and is applied to green light CdSe amounts
On sub- point luminescent diode, which includes adjacent successively ito anode, PEDOT:PSS hole injection layers,
TFB hole transmission layers, CdSe quantum dot luminescent layer, ZnLiMgO electron transfer layers and cathode aluminium.The light emitting diode with quantum dots
Service life T50@1000cd/m2Extension reaches 361h, other device performances are shown in Table 1.
Embodiment 4
Include the following steps：
S1 at 20 DEG C, the hydration lithium acetates of 4.5mmol bis- is mixed with 15mL propylene-glycol ethyl ethers, 5mL diethylene glycol (DEG)s, additionally
3mmol five is added and is hydrated tetramethylammonium hydroxide, obtains the first reaction system.
3.5mmol zinc nitrates and 0.3mmol magnesium sulfate are added into the first reaction system by S2, stir 12h, obtain
ZnLiMgO dispersions.
S3,0.4mmol magnesium sulfate, 20 DEG C of bath temperature are added into the ZnLiMgO dispersions of S2, and ultrasonic 30min is obtained
To ZnLiMgO nano particles.
Propylene-glycol ethyl ether is connected to the surface of ZnLiMgO nano particles as surface ligand.
It is tested through ICP-MS, in ZnLiMgO, the molar ratio of Zn elements, Li elements and Mg elements is 100:27:29.Through
XRD test analysis (as shown in D curves in Fig. 1), ZnLiMgO nano particles are wurtzite structure.It is computed, ZnLiMgO nanometers
The band gap width of particle is 3.58eV.Computational methods are well known to those skilled in the art, such as can pass through UV absorption number
According to calculating, which is not described herein again.
The electron transfer layer of electroluminescent device is made by above-mentioned ZnLiMgO nano particles, and is applied to green light CdZnSeS
On light emitting diode with quantum dots, which includes adjacent successively ito anode, PEDOT:The holes PSS are injected
Layer, TFB hole transmission layers, CdZnSeS quantum dot light emitting layers, ZnLiMgO electron transfer layers and cathode aluminium.The quantum dot light emitting two
The service life T of pole pipe50@1000cd/m2Extension reaches 332h, other device performances are shown in Table 1.
Comparative example：
It is incorporated in 2mmol Zinc diacetate dihydrates in 20mL DMSO, stirs 2h, purification obtains ZnO nano particle.
The electron transfer layer of electroluminescent device is made by above-mentioned ZnLiMgO nano particles, and is applied to green light CdSe amounts
On sub- point luminescent diode, which includes adjacent successively ito anode, PEDOT:PSS hole injection layers,
TFB hole transmission layers, CdSe quantum dot luminescent layer, ZnLiMgO electron transfer layers and cathode aluminium.The light emitting diode with quantum dots
Service life T50@1000cd/m2For 100h, other device performances are shown in Table 1.
Table 1
As shown in Table 1, for light emitting diode with quantum dots, using the ZnLiMgO nano particles of the application as photophore
When the electron transfer layer of part, 1) red device：T50@1000cd/m2Up to 1937h, current efficiency can be to 24.5cd/A, outer quantum
Efficiency can be to 13.8%；2) green device：T50@1000cd/m2For up to 375h, current efficiency can be to 48.6cd/A, outer quantum
Efficiency can be much better than the luminescent device that the common ZnO nano particle without alcohol ether ligand makees electron transfer layer, have to 10.6%
The energy consumption of luminescent device is reduced to effect, and improves the service life of device.
Although inventor has done more detailed elaboration to the technical solution of the application and has enumerated, it should be understood that for
For those skilled in the art, above-described embodiment is modified and/or the flexible or equivalent alternative solution of use is obvious
, cannot all be detached from the essence of the application spirit, the term occurred in the application be used for elaboration to technical scheme and
Understand, the limitation to the application can not be constituted.
Claims (10)
1. a kind of preparation method of ZnLiMgO nano particles, it is characterized in that including the following steps：
S1 under room temperature and alkaline environment, lithium salts and alcohol ether is mixed, the first reaction system is obtained；
S2 is added zinc salt into first reaction system, ZnLiO dispersions is obtained by the reaction；
S3 is added magnesium salts into the ZnLiO dispersions of S2, ZnLiMgO nano particles is obtained by the reaction.
2. the preparation method of ZnLiMgO nano particles according to claim 1, which is characterized in that the alcohol ether is C3-C5
Straight chain alcohol ether.
3. the preparation method of ZnLiMgO nano particles according to claim 2, which is characterized in that the alcohol ether is second two
Alcohol methyl ether.
4. the preparation method of the ZnLiMgO nano particles according to any one of Claim 1-3, which is characterized in that described
Alkaline environment is provided by tetramethylammonium hydroxide.
5. the preparation method of ZnLiMgO nano particles according to claim 4, which is characterized in that the tetramethyl hydrogen-oxygen
The molar concentration for changing ammonium is 0.1~0.3mol/L.
6. the preparation method of the ZnLiMgO nano particles according to any one of claim 1 to 5, which is characterized in that in institute
It states in the first reaction system also with one or more in polyethylene glycol, glycol.
7. the preparation method of the ZnLiMgO nano particles according to any one of claim 1 to 6, which is characterized in that with object
The gauge of matter, the lithium salts, zinc salt, magnesium salts whole inventory ratio be (0.5~1.5):1:(0.05~0.3).
8. the preparation method of ZnLiMgO nano particles according to claim 7, which is characterized in that in S2, zinc salt is added
While magnesium salts is added.
9. the preparation method of ZnLiMgO nano particles according to claim 8, which is characterized in that with the gauge of substance,
The addition of magnesium salts accounts for the 0~50% of magnesium salts total amount of feeding in the S2.
10.ZnLiMgO nano particles are prepared according to method as described in any one of claim 1 to 9, and feature exists
In in the ZnLiMgO nano particles that the preparation method obtains, the molar ratio of Zn elements, Li elements and Mg elements is 100:
(1~30):The surface ligand of (1~30), the ZnLiMgO nano particles is the alcohol ether.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109825285A (en) * | 2019-02-01 | 2019-05-31 | 苏州星烁纳米科技有限公司 | Zinc oxide base nano particle and preparation method thereof, electroluminescent device |
| CN113948647A (en) * | 2020-07-17 | 2022-01-18 | Tcl科技集团股份有限公司 | Nano material, preparation method thereof and quantum dot light-emitting diode |
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| CN109825285A (en) * | 2019-02-01 | 2019-05-31 | 苏州星烁纳米科技有限公司 | Zinc oxide base nano particle and preparation method thereof, electroluminescent device |
| CN113948647A (en) * | 2020-07-17 | 2022-01-18 | Tcl科技集团股份有限公司 | Nano material, preparation method thereof and quantum dot light-emitting diode |
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