CN107058984A - A kind of graphical quantum dot film preparation method based on electrostatic induction - Google Patents
A kind of graphical quantum dot film preparation method based on electrostatic induction Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 96
- 230000006698 induction Effects 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 37
- 230000008569 process Effects 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims description 35
- 239000002243 precursor Substances 0.000 claims description 32
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 238000001259 photo etching Methods 0.000 claims description 8
- 238000004528 spin coating Methods 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 7
- 239000005642 Oleic acid Substances 0.000 claims description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- -1 caesium halide Chemical class 0.000 claims description 5
- 238000003754 machining Methods 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052792 caesium Inorganic materials 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 150000002367 halogens Chemical class 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 238000010411 cooking Methods 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims 1
- 239000006193 liquid solution Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000007493 shaping process Methods 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 18
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 12
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
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- 238000001556 precipitation Methods 0.000 description 3
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- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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Abstract
The invention discloses a kind of graphical quantum dot film preparation method based on electrostatic induction.The method comprising the steps of:(1)The preparation and processing of array mould plate;(2)The preparation and coating of quantum dot reaction solution;(3)The placement of electrostatic induction pole plate;(4)Electrostatic induction is molded.The method that the present invention is combined using electrostatic induction and micro-structural template, realizes the preparation of quantum dot color membrane substrates, the forming process of the preparation process of quantum dot and quantum stippling membrane array is combined together, settled at one go;The inventive method is simple to operate, efficiency high, and control accuracy is high, it is adaptable to the shaping of red, green, blue quantum stippling film, efficiently solves the problem of prior art is present, reduces manufacturing cost, suitable for large-scale production process.
Description
Technical field
The present invention relates to display technology field, more particularly to a kind of graphical quantum dot film preparation method.
Technical background
With continuing to develop for Display Technique, people require more and more higher to the display quality of display device.Quantum dot material
(Quantum Dots), which is expected, as a kind of new fluorescent material is increasingly subject to extensive concern.Quanta point material refers to that particle diameter exists
1-100nm semiconductor grain.Conventional fluorescent material is contrasted, quanta point material can send the monochromatic light of high-purity, luminous efficiency
It is higher, therefore display color is more bright-coloured, contrast is high, more preferable display effect is brought while efficient energy-saving, with without comparable
The advantage and potentiality of plan.Quanta point material is widely paid close attention to, and quantum dot Display Technique also emerges promptly.
Quantum dot Display Technique contrast available liquid crystal is shown and OLED Display Techniques, pure with colour gamut covering broadness, color
Degree is high, performance is stable and the advantages of long lifespan, therefore more efficient energy-saving, at the same improve color contrast and definition there is provided
More preferable display quality.The difficult point of quantum dot Display Technique is the shaping of high-quality high-precision RGB quantum dot arrays.At present,
Quantum dot Display Technique is mainly print process, ink-jet method and photoetching process etc. for the manufacturing process of color membrane substrates, and manufacture method is not
Reach maturation and there are many defects.Though ink-jet method precision is higher but cost is higher, realize that difficulty is big.Print process and photoetching process manufacture
Cost is relatively low, but precision is not high enough, influences the display quality of display.Realize high efficiency, manufacture RGB quantum dot array in high quality
Row, have huge impetus to quantum dot Display Technique.
The content of the invention
It is an object of the invention to provide a kind of graphical quantum dot film preparation method based on electrostatic induction, this method
Manufacturing cost is low and can realize high-precision control.
In order to achieve the above object, the technical scheme taken of the present invention is.
A kind of graphical quantum dot film preparation method based on electrostatic induction, comprises the following steps:
(1)The preparation and processing of array mould plate:Figure needed for conducting plate Surface Machining is gone out using photoetching and etching technics
Mini column array structure, is used as the array mould plate of electrostatic induction process;
(2)The preparation and coating of quantum dot reaction solution:Configure the precursor solution and poor solvent of quantum dot;Presoma is molten
The upper surface that liquid is coated on lower flat board forms quantum dot precursor layer, then the lower surface that poor solvent is coated on into upper flat plate is formed
Poor solvent layer;
(3)The placement of electrostatic induction pole plate:By the mini column array structure placed face down of array mould plate in upper flat plate without solution
On face, the surface of upper and lower flat board coating solution is inwardly placed, places and is compressed and horizontal positioned after cushion block between two plates, made upper and lower
The air gap is left between flat board;
(4)Electrostatic induction is molded:Array mould plate is connect into DC power anode, lower board joint DC power cathode, turn on the power into
Row electrostatic induction;After electrostatic induction terminates, upper flat plate is placed in into oven cooking cycle dries unnecessary poor solvent layer, needed for leaving
Quantum dot array array structure, obtain quantum dot film.
Further, step(1)In, the array mould plate is conductive plate, and material is any one in copper, iron and aluminium
Kind.
Further, step(1)In, the micro-pillar array is any one in cylindrical-array and square column array.
Further, step(1)In, the central shaft distance range between the microtrabeculae is 0.5-15 μm.
Further, step(1)In, the diameter range of the cylindrical-array is 0.1-10 μm, and cylinder height scope is
1-100μm。
Further, step(1)In, the bottom surface side size range of the square column array is 0.1-10 μm, square column height model
Enclose for 1-100 μm.
Further, step(2)In, the quantum dot is perovskite quantum dot.
Further, step(2)In, the glow color of the quantum dot is any one in red, green and blue.
Further, step(2)In, the quantum dot precursor solution is formulated as:Lead halide and caesium halide are dissolved in
Dimethylformamide(DMF)In, surfactant oleyl amine and oleic acid are added, it is molten that stirring obtains quantum dot presoma after being completely dissolved
Liquid.
Further, step(2)In, in the quantum dot precursor solution, halogen is included in Cl, Br and I
More than one, the mol ratio of caesium, lead and halogen is 1:1:3, the volume ratio of dimethylformamide, oleic acid and oleyl amine is 20:
2:1。
Further, step(2)In, the concentration of the quantum dot precursor solution is 0.01-0.03g/mL.
Further, step(2)In, the thickness range of the quantum dot precursor layer is 1-100 μm.
Further, step(2)In, the upper flat plate, lower flat board are that ITO electro-conductive glass and height mix conductive silicon chip
In any one.
Further, step(2)In, the method for the coating is any one in blade coating, spin coating and spraying.
Further, step(2)In, the poor solvent is any in toluene, dimethylbenzene, dichloromethane and chloroform
It is a kind of.
Further, step(2)In, the thickness range of the poor solvent layer is 1-100 μm.
Further, step(3)In, the material of the cushion block includes glass.
Further, step(3)In, the thickness range of the air gap is 10 μm -1000 μm.
Further, step(3)In, the altitude range of the cushion block is 10 μm -1000 μm.
Further, step(4)In, the voltage range of the electrostatic induction process is 50-500V, the time of electrostatic induction
Scope is 1-30min.
Further, step(4)In, the temperature of the baking is 60-120 DEG C, and the time of baking is 1-10min.
Further, the fluorescence color of quantum dot, repeat step are changed(3)With(4), prepare the color film with RGB array
Substrate.
The inventive method is patterned during the preparation of quantum dot film, electrostatic induction, micro- due to array mould plate
The electric charge of post lower zone is more concentrated, and electrostatic force is bigger, and precursor layer deforms under electrostatic force, is adsorbed to microtrabeculae
Lower section, precipitation quantum dot is contacted with poor solvent layer, the quantum dot of generation is in array distribution, leaves required quantum dot array knot
Structure.By changing array mold pattern, voltage and electrostatic induction time, the regulation and control to color membrane substrates molding effect are realized.
Compared with prior art, the invention has the advantages that and beneficial effect:
(1)The method that the present invention is combined using electrostatic induction and micro-structural template, realizes the preparation of quantum dot color membrane substrates, will measure
The preparation process of son point and the forming process of quantum stippling membrane array are combined together, and are settled at one go;
(2)The inventive method is simple to operate, efficiency high, and control accuracy is high, it is adaptable to the shaping of red, green, blue quantum stippling film, has
Effect solves the problem of prior art is present, and manufacturing cost is reduced, suitable for large-scale production process.
Brief description of the drawings
Fig. 1 is the flow chart of the graphical quantum dot film preparation method based on electrostatic induction;
Fig. 2 is the schematic device that electrostatic induction is molded;
Fig. 3 is two isogonism axonometric drawings of cylindrical-array template;
Fig. 4 is two isogonism axonometric drawings of square column array mould plate.
Embodiment
To make those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and specific embodiment party
Formula is described in further detail to the present invention.
As shown in figure 1, be the flow chart of the graphical quantum dot film preparation method based on electrostatic induction, including array mould
Preparation and processing, the preparation of quantum dot reaction solution and coating, the placement of electrostatic induction pole plate and the electrostatic induction shaping of plate.
The schematic device of electrostatic induction shaping as shown in Fig. 2 including array mould plate 1, upper flat plate 2, poor solvent layers 3,
Quantum dot precursor layer 4, cushion block 5 and lower flat board 6;Nothing of the mini column array structure placed face down of array mould plate 1 in upper flat plate 2
On solution face, upper flat plate 2 is coated with the surface that the surface of poor solvent and lower flat board 6 be coated with precursor solution and inwardly placed,
Cushion block 5 is placed between two plates, makes to leave the air gap between upper and lower flat board;Upper flat plate 2 is coated with the surface of poor solvent and formed not
Good solvent layer, the surface that lower flat board 6 is coated with precursor solution forms quantum dot precursor layer.
The mini column array structure on the surface of the array mould plate obtained by photoetching and etching includes cylindrical-array and square column battle array
Any one in row, and central shaft distance range between microtrabeculae is 0.5-15 μm;Fig. 3 is two isometric axis of cylindrical-array template
Mapping, the diameter range of cylindrical-array is 0.1-10 μm, and cylinder height scope is 1-100 μm;Fig. 4 is the two of square column array mould plate
Isogonism axonometric drawing, the bottom surface side size range of square column array is 0.1-10 μm, and square column altitude range is 1-100 μm.
Embodiment 1
The present embodiment provides a kind of graphical quantum dot film preparation method based on electrostatic induction, comprises the following steps:
(1)The preparation and processing of array mould plate:The rectangle red copper that a block size is 50mm × 100mm, thickness is 2mm is chosen to put down
Plate, one Surface Machining of red copper flat board is gone out required micro-pillar array graphic structure, be used as electrostatic using photoetching and etching technics
The array mould plate of Induction Process;Gained micro-pillar array is processed for cylindrical-array, a diameter of 2 μm of micro- bottom cylindrical face of cylindrical-array,
Micro- cylinder height scope is that central shaft distance is 5 μm between 4 μm, the adjacent microtrabeculae of array mold;In the non-structured surface of array mold
Adhesive electrode and wire, connect DC power anode.
(2)The preparation of quantum dot reaction solution:Quantum dot reaction solution includes quantum dot precursor solution and poor solvent;
Perovskite quantum dot is chosen as quanta point material, 0.0371g PbCl are first weighed2、0.0984g PbBr2、0.018g
(mol ratio is Cs to CsCl and 0.0454g CsBr:Pb:Cl:Br=1:1:1:2) it is dissolved in 10mL DMF and adds 1mL
Oleic acid and 0.5mL oleyl amines;Because PbCl2With CsCl compared with indissoluble solution, therefore add 3mL dimethyl sulfoxide (DMSO)s (DMSO) hydrotropy;Will be mixed
Liquid stirring and dissolving 10min is closed, precursor solution is made;Selection toluene is poor solvent;All operating process are in normal temperature and pressure
It is lower to carry out, it is not necessary to protective gas.
(3)The coating of quantum dot reaction solution:The rectangle height that selection size is 50mm × 100mm, thickness is 2mm, which mixes, leads
Electric silicon chip is used as upper flat plate;Upper flat plate is fixed on spin coater, quantum dot precursor solution is extracted by upper flat plate with syringe
Surface is filled, and is opened spin coater with 800r/min rotating speed spin coating 20s, is obtained the precursor layer that thickness is 80 μm;Chi is chosen again
Lower flat board is fixed on spin coater, with note by the ITO electro-conductive glass that very little is 50mm × 100mm, thickness is 2mm as lower flat board
Emitter extracts poor solvent toluene and fills lower planar surface, opens spin coater with 800r/min rotating speed spin coating 20s, obtains thickness
Spend the poor solvent layer for 80 μm;Lower flat board is removed, in lower flat board without solution surface adhesive electrode and wire, direct current is connected to
The negative pole in source.
(4)The placement of electrostatic induction pole plate:Array mould plate micro-structural placed face down is used in upper flat plate without on solution face
Non-conductive fixture, which clamps upper and lower flat board, makes the surface of its coating solution inwardly and horizontal parallel placement, and two fritters are placed between flat board
The sheet glass that 50 μm of thickness is used as cushion block so that the air gap that thickness range is 50 μm is left between pole plate.
(5)Electrostatic induction is molded:Array mould plate is connect into DC power anode, lower board joint DC power cathode opens electricity
Source carries out electrostatic induction, applies 250V voltages between pole plate, conduction time is 10min.Due to array mould plate microtrabeculae lower zone
Electric charge more concentrate, electrostatic force is bigger, is adsorbed to first below microtrabeculae when precursor layer deforms under electrostatic force,
Precipitation quantum dot is contacted with poor solvent layer, the quantum dot of generation is in array distribution.In deenergization after energization 10min, taking-up
Flat board is placed in the oven for baking 5min that temperature range is 80 DEG C, and poor solvent layer unnecessary on upper flat plate is dried, institute is left
The quantum dot array array structure needed.
Change quanta point material fluorescence color and aforesaid operations are repeated using respective array template, realizing has RGB array
Color membrane substrates preparation.
Embodiment 2
The present embodiment provides a kind of graphical quantum dot film preparation method based on electrostatic induction, comprises the following steps:
(1)The preparation and processing of array mould plate:The rectangle red copper that a block size is 50mm × 100mm, thickness is 2mm is chosen to put down
Plate, one Surface Machining of red copper flat board is gone out required micro-pillar array graphic structure, be used as electrostatic using photoetching and etching technics
The array mould plate of Induction Process;Processing gained micro-pillar array is square column array, and micro- square column bottom surface length of side of square column array is 0.1 μ
M, micro- square column is highly that central shaft distance is 0.5 μm between 1 μm, the adjacent microtrabeculae of array mold;In the non-structured surface of array mold
Adhesive electrode and wire, connect DC power anode.
(2)The preparation of quantum dot reaction solution:Quantum dot reaction solution includes quantum dot precursor solution and poor solvent;
Perovskite quantum dot is chosen as quanta point material, 0.0270g PbCl are first weighed2、0.0717g PbBr2、0.0131g
(mol ratio is Cs to CsCl and 0.0331g CsBr:Pb:Cl:Br=1:1:1:2) it is dissolved in 10mL DMF and adds 1mL
Oleic acid and 0.5mL oleyl amines;Because PbCl2With CsCl compared with indissoluble solution, therefore add 3mL dimethyl sulfoxide (DMSO)s (DMSO) hydrotropy;Will be mixed
Liquid stirring and dissolving 10min is closed, precursor solution is made;Selection toluene is poor solvent;All operating process are in normal temperature and pressure
It is lower to carry out, it is not necessary to protective gas.
(3)The coating of quantum dot reaction solution:The rectangle height that selection size is 50mm × 100mm, thickness is 2mm, which mixes, leads
Electric silicon chip is used as upper flat plate;Upper flat plate is fixed on spin coater, quantum dot precursor solution is extracted by upper flat plate with syringe
Surface is filled, and is opened spin coater with 1800r/min rotating speed spin coating 120s, is obtained the precursor layer that thickness is 1 μm;Chi is chosen again
Lower flat board is fixed on spin coater, with note by the ITO electro-conductive glass that very little is 50mm × 100mm, thickness is 2mm as lower flat board
Emitter extracts poor solvent toluene and fills lower planar surface, opens spin coater with 1800r/min rotating speed spin coating 120s, obtains
Thickness is 1 μm of poor solvent layer;Lower flat board is removed, in lower flat board without solution surface adhesive electrode and wire, direct current is connected to
The negative pole of power supply.
(4)The placement of electrostatic induction pole plate:Array mould plate micro-structural placed face down is used in upper flat plate without on solution face
Non-conductive fixture, which clamps upper and lower flat board, makes the surface of its coating solution inwardly and horizontal parallel placement, and two fritters are placed between flat board
The sheet glass that 10 μm of thickness is used as cushion block so that the air gap that thickness range is 10 μm is left between pole plate.
(5)Electrostatic induction is molded:Array mould plate is connect into DC power anode, lower board joint DC power cathode opens electricity
Source carries out electrostatic induction, applies 50V voltages between pole plate, conduction time is 1min.Due to array mould plate microtrabeculae lower zone
Electric charge is more concentrated, and electrostatic force is bigger, is adsorbed to first below microtrabeculae when precursor layer deforms under electrostatic force, with
Poor solvent layer contact separates out quantum dot, and the quantum dot of generation is in array distribution.Deenergization after energization 1min, takes out upper flat plate
The oven for baking 1min that temperature range is 60 DEG C is placed in, poor solvent layer unnecessary on upper flat plate is dried, needed for leaving
Quantum dot array array structure.
Change quanta point material fluorescence color and aforesaid operations are repeated using respective array template, realizing has RGB array
Color membrane substrates preparation.
Embodiment 3
The present embodiment provides a kind of graphical quantum dot film preparation method based on electrostatic induction, comprises the following steps:
(1)The preparation and processing of array mould plate:The rectangle red copper that a block size is 50mm × 100mm, thickness is 2mm is chosen to put down
Plate, one Surface Machining of red copper flat board is gone out required micro-pillar array graphic structure, be used as electrostatic using photoetching and etching technics
The array mould plate of Induction Process;Gained micro-pillar array is processed for cylindrical-array, a diameter of 10 μm of micro- bottom cylindrical face of cylindrical-array,
Micro- square column is highly that central shaft distance is 15 μm between 100 μm, the adjacent microtrabeculae of array mold;Glued in the non-structured surface of array mold
Electrode and wire are pasted, DC power anode is connected.
(2)The preparation of quantum dot reaction solution:Quantum dot reaction solution includes quantum dot precursor solution and poor solvent;
Perovskite quantum dot is chosen as quanta point material, 0.0811g PbCl are first weighed2、0.2152g PbBr2、0.0394g
(mol ratio is Cs to CsCl and 0.0993g CsBr:Pb:Cl:Br=1:1:1:2) it is dissolved in 10mL DMF and adds 1mL
Oleic acid and 0.5mL oleyl amines;Because PbCl2With CsCl compared with indissoluble solution, therefore add 3mL dimethyl sulfoxide (DMSO)s (DMSO) hydrotropy;Will be mixed
Liquid stirring and dissolving 10min is closed, precursor solution is made;Selection toluene is poor solvent;All operating process are in normal temperature and pressure
It is lower to carry out, it is not necessary to protective gas.
(3)The coating of quantum dot reaction solution:The rectangle height that selection size is 50mm × 100mm, thickness is 2mm, which mixes, leads
Electric silicon chip is used as upper flat plate;Upper flat plate is fixed on spin coater, quantum dot precursor solution is extracted by upper flat plate with syringe
Surface is filled, and is opened spin coater with 600r/min rotating speed spin coating 10s, is obtained the precursor layer that thickness is 100 μm;Chi is chosen again
Lower flat board is fixed on spin coater, with note by the ITO electro-conductive glass that very little is 50mm × 100mm, thickness is 2mm as lower flat board
Emitter extracts poor solvent toluene and fills lower planar surface, opens spin coater with 600r/min rotating speed spin coating 10s, obtains thickness
Spend the poor solvent layer for 100 μm;Lower flat board is removed, in lower flat board without solution surface adhesive electrode and wire, direct current is connected to
The negative pole of power supply.
(4)The placement of electrostatic induction pole plate:Array mould plate micro-structural placed face down is used in upper flat plate without on solution face
Non-conductive fixture, which clamps upper and lower flat board, makes the surface of its coating solution inwardly and horizontal parallel placement, and two fritters are placed between flat board
The sheet glass that 1000 μm of thickness is used as cushion block so that the air gap that thickness range is 1000 μm is left between pole plate.
(5)Electrostatic induction is molded:Array mould plate is connect into DC power anode, lower board joint DC power cathode opens electricity
Source carries out electrostatic induction, applies 500V voltages between pole plate, conduction time is 30min.Due to array mould plate microtrabeculae lower zone
Electric charge more concentrate, electrostatic force is bigger, is adsorbed to first below microtrabeculae when precursor layer deforms under electrostatic force,
Precipitation quantum dot is contacted with poor solvent layer, the quantum dot of generation is in array distribution.In deenergization after energization 30min, taking-up
Flat board is placed in the oven for baking 10min that temperature range is 120 DEG C, and poor solvent layer unnecessary on upper flat plate is dried, left
Required quantum dot array array structure.
Change quanta point material fluorescence color and aforesaid operations are repeated using respective array template, realizing has RGB array
Color membrane substrates preparation.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, but the invention is not limited in this.For those skilled in the art, the essence of the present invention is not being departed from
In the case of refreshing and essence, various changes and modifications can be made therein, and these variations and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a kind of graphical quantum dot film preparation method based on electrostatic induction, it is characterised in that comprise the following steps:
(1)The preparation and processing of array mould plate:Figure needed for conducting plate Surface Machining is gone out using photoetching and etching technics
Mini column array structure, is used as the array mould plate of electrostatic induction process;
(2)The preparation and coating of quantum dot reaction solution:Configure the precursor solution and poor solvent of quantum dot;Presoma is molten
The upper surface that liquid is coated on lower flat board forms quantum dot precursor layer, then the lower surface that poor solvent is coated on into upper flat plate is formed
Poor solvent layer;
(3)The placement of electrostatic induction pole plate:By the mini column array structure placed face down of array mould plate in upper flat plate without solution
On face, the surface of upper and lower flat board coating solution is inwardly placed, places and is compressed and horizontal positioned after cushion block between two plates, made upper and lower
The air gap is left between flat board;
(4)Electrostatic induction is molded:Array mould plate is connect into DC power anode, lower board joint DC power cathode, turn on the power into
Row electrostatic induction;After electrostatic induction terminates, upper flat plate is placed in into oven cooking cycle dries unnecessary poor solvent layer, needed for leaving
Quantum dot array array structure, obtain quantum dot film.
2. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature exists
In step(1)In, the array mould plate is conductive plate, and material is any one in copper, iron and aluminium;The micro-pillar array
For any one in cylindrical-array and square column array;Central shaft distance range between the microtrabeculae is 0.5-15 μm.
3. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 2, its feature exists
In the diameter range of the cylindrical-array is 0.1-10 μm, and cylinder height scope is 1-100 μm;The bottom surface of the square column array
Side size range is 0.1-10 μm, and square column altitude range is 1-100 μm.
4. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature
It is, step(2)In, the quantum dot is perovskite quantum dot;The glow color of the quantum dot is any in red, green and blue
It is a kind of;The thickness range of the quantum dot precursor layer is 1-100 μm.
5. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature
It is, step(2)In, the quantum dot precursor solution is formulated as:Lead halide and caesium halide are dissolved in dimethylformamide
In, surfactant oleyl amine and oleic acid are added, stirring obtains quantum dot precursor solution after being completely dissolved;The quantum dot forerunner
In liquid solution, halogen includes one or more of Cl, Br and I, and the mol ratio of caesium, lead and halogen is 1:1:3, two
The volume ratio of NMF, oleic acid and oleyl amine is 20:2:1;The concentration of the quantum dot precursor solution is 0.01-0.03g/
mL。
6. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature
It is, step(2)In, the upper flat plate, lower flat board be ITO electro-conductive glass and it is high mix it is any one in conductive silicon chip
Kind;The method of the coating is any one in blade coating, spin coating and spraying.
7. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature
It is, step(2)In, any one of the poor solvent in toluene, dimethylbenzene, dichloromethane and chloroform;It is described not
The thickness range of good solvent layer is 1-100 μm.
8. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature
It is, step(3)In, the material of the cushion block includes glass;The thickness range of the air gap is 10 μm -1000 μm;Institute
The altitude range for stating cushion block is 10 μm -1000 μm.
9. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature
It is, step(4)In, the voltage range of the electrostatic induction process is 50-500V, and the time range of electrostatic induction is 1-
30min;The temperature of the baking is 60-120 DEG C, and the time of baking is 1-10min.
10. a kind of graphical quantum dot film preparation method based on electrostatic induction according to claim 1, its feature
It is, changes the fluorescence color of quantum dot, repeat step(3)With(4), prepare the color membrane substrates with RGB array.
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TWI642760B (en) * | 2018-01-04 | 2018-12-01 | 國立清華大學 | Perovskite quantum dot, preparation method thereof and quantum dot film including the same |
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