CN105789486B - A kind of selective orientated deposition method of organic film - Google Patents
A kind of selective orientated deposition method of organic film Download PDFInfo
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- H—ELECTRICITY
- 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
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/125—Deposition of organic active material using liquid deposition, e.g. spin coating using electrolytic deposition e.g. in-situ electropolymerisation
Abstract
The invention discloses the selective orientated deposition method of organic film, comprise the following steps：The film crystal tube drive circuit of AMOLED substrates is connected in series in the electrolytic cell circuit of electrochemical deposition；The break-make electricity condition in electrolytic cell circuit, simultaneous electrochemical work station output electro-deposition signal are controlled by film crystal tube drive circuit；Deposition obtains organic film on the corresponding pixel electrode in the electrolytic cell circuit of "on" position.The present invention passes through the adjusting of control circuit and the replacement of electrolyte, can orientated deposition red, green, blue light-emitting film successively, multicolour pattern is prepared, a kind of colorization technology simply, economic that provides is prepared for the pixel of Organic Light Emitting Diode (OLED).
Description
Technical field
The present invention relates to field of photovoltaic materials, the selective orientated deposition method of more particularly to a kind of organic film.
Background technology
The full color of display be examine display commercially whether competitive important symbol.Using it is red,
It is to use most colorization patterns at present that green, blue (RGB) luminescent material, which independently shines, which needs to make RGB hairs respectively
Sub-pixels, Patternized technique is more complicated, and larger specific gravity (50%) is occupied in the cost of manufacture of device.It is most common at present
The technology of preparing of organic film is metal mask evaporation, and the organic small molecule material that it is suitable for easily distil, this method is profit
With precision metal mask plate and CCD pixel technique of counterpoint, in high vacuum conditions, be deposited respectively red-green-blue luminescent layer from
And realize patterning, which has been widely used in the preparation of Organic Light Emitting Diode (OLED) display screen,
But its used equipment is complicated, of high cost, waste of material is serious, in addition, metal shadow mask lithographic technique is directly affected and shown
The screen resolution and image quality of screen, are limited by metal etch technology, and the patterning precision of mask evaporation technology is general
Tens microns to several microns of level is can only achieve, and high-resolution metal mask plate thickness is all very thin, makes it in big ruler
It is difficult exactitude position in very little display screen.Therefore in OLED moves towards high-resolution and large-sized industrialization process, metal mask
Technology is faced with harsher dimension of picture precision and positioning accuracy request.The inkjet printing technology developed in recent years is to prepare figure
The very potential method of case pixel, the technology are that micro solution (several picoliters) is ejected into RGB by printing head
The characteristics of realizing that three-color light-emitting patterns in pixel hole, macromolecule and the processing of some small soluble molecules liquid can be given full play to, it is right
Substrate does not have selectivity substantially, easy to operate, saves material, is a kind of energy-saving and environment-friendly colorization film technique.But ink-jet
Printing also has a problem urgently to be resolved hurrily --- printing precision problem, and for inkjet printing, ink droplet is smaller to be more difficult to accurately
Ground drips to Pixel surface, and experiment shows, when drop diameter is less than 10 microns, is dropped onto it is difficult to break through air drag on substrate.
The content of the invention
In order to overcome the disadvantages mentioned above of the prior art and deficiency, it is an object of the invention to provide a kind of choosing of organic film
Selecting property orientated deposition method, electropolymerization thin film deposition position controllable precise, patterning easy to implement, technique is simple, can room temperature it is normal
Operated under the conditions of pressure, is of low cost.
The purpose of the present invention is achieved through the following technical solutions：
A kind of selective orientated deposition method of organic film, comprises the following steps：
(1) using m pixel electrode of AMOLED substrates as working electrode, the thin film transistor (TFT) on AMOLED substrates is driven
Dynamic circuit connected in series is into the electrolytic cell circuit of electrochemical deposition；The electrolytic cell circuit of the electrochemical deposition includes electrochemical operation
Stand, reference electrode, working electrode, auxiliary electrode；m≥1；
The auxiliary electrode, working electrode are placed in electrolyte；The auxiliary electrode is electrically connected with electrochemical workstation；
M pixel electrode is connected with m driving unit of film crystal tube drive circuit respectively, film crystal tube drive circuit and electrification
Learn work station connection；The reference electrode is placed between auxiliary electrode, working electrode, and reference electrode connects with electrochemical workstation
Connect；
(2) the break-make electricity condition in electrolytic cell circuit, simultaneous electrochemical work station are controlled by film crystal tube drive circuit
Export electro-deposition signal；Deposition obtains organic film on the corresponding pixel electrode in the electrolytic cell circuit of "on" position.
The driving unit is made of a switching tube, a driving tube, a capacitance, the wherein source electrode of switching tube and drive
The grid connection of dynamic pipe, the source electrode of driving tube are connected with pixel electrode, the both ends grid with driving tube and the drain electrode respectively of capacitance
Connection；
The grid of the switching tube is connected with scan line, and drain electrode is connected with data cable；The drain electrode of the driving tube and power supply
Line connects；
The switching tube is used to address, and the driving tube is used for the color and grayscale for controlling luminescent device, the capacitance
For storing electric charge.
The AMOLED substrates are 1 × n array, n >=1.
The electrochemical workstation using cyclic voltammetry control electrodeposited film deposition process, pixel electrode relative to
The voltage range of reference electrode is 0~0.835 volt, and sweep speed is 50 mv s, and the scanning number of turns is 12 circles.
The method of the i-th row deposition of organic thin film on pixel electrode substrate is as follows：
AMOLED substrates are dipped into the electrolyte of jth kind electro-deposition monomer, to the scan line of n row pixel electrode connection
Apply positive grid voltage；Positive grid voltage is applied to the data cable of the i-th row pixel electrode connection, the data cable of other row pixel electrodes connection is applied
Add minus gate voltage；Electrochemical workstation inputs electro-deposition signal to the power cord that n row pixel electrode connects；
Wherein, 1≤i≤n；j≥1.
The organic film is any one in feux rouges film, blue light film, green light film.
The electrolytic solution is that the electro-deposition monomer that is dissolved in organic solvent and supporting electrolyte configuration form, electro-deposition
Monomer concentration is 10-5Mol/L~103Mol/L, the concentration of supporting electrolyte is 10-3Mol/L~102Mol/L.Institute
State in electro-deposition monomer precursor and contain electroactive group, such as carbazole, pyrroles, ethene, acetylene, thiophene, aniline, diphenylamines or triphen
Electrochemical Coupling reaction can occur under appropriate current potential or electric current for amine and its derivative etc., the group.Supporting electrolyte is more
For inorganic salts, it can be formed by the independent assortment for commonly using anion and cation, wherein the anion of supporting electrolyte can be high
Chloranion, tetrafluoroborate ion, hexafluorophosphoricacid acid ions, hexafluoroarsenate radical ion；The cation of supporting electrolyte is
Potassium ion, lithium ion, tetramethyl ammonium, tetraethyl ammonium ion, tetra-n-butyl ammonium ion.Organic solvent is N, N- dimethyl second
One kind in acid amides, n,N-Dimethylformamide, acetonitrile, chloroform, dichloromethane, propene carbonate, three fluoboric acid ether
Or its combination.
The principle of the present invention is：
In active-matrix light emitting diode (AMOLED), each sub-pixel is corresponding with by thin film transistor (TFT) TFT groups
Into drive circuit, the drive circuit play the role of one regulation and control loop current size, you can using the switch as circuit.Cause
Drive circuit in AMOLED substrates is combined by this with electrochemical deposition technique, utilizes the switching function control of TFT drive circuits
The break-make electricity condition of system pixel electrode carrys out the generation of coordination electrode reaction or prohibits, can be optionally in corresponding pixel
Orientated deposition light-emitting film.Using the TFT drive circuits control trizonal pixel electrode of red, green, blue in three kinds of RGB
Break-make electricity condition in dyestuff, you can the sub-pixel of three kinds of colors of RGB is prepared respectively, so as to fulfill the colorization of pixel.
Compared with prior art, the present invention has the following advantages and beneficial effect：
(1) present device is simple, can carry out at normal temperatures and pressures；Raw material is saved very much, can once complete light-emissive polymer
The synthesis of thing and accurate deposition；Easily realize the preparation of large area light emitting film.
(2) electropolymerization thin film deposition position controllable precise of the invention, patterning easy to implement.Film property (pattern,
Thickness etc.) can be by polymerizing condition conveniently regulating and controlling.
(3) glow color that film can be easily adjusted by varying light emitting molecule of the invention, carries for total colouring
For platform.
Brief description of the drawings
Fig. 1 is the electrolytic cell circuit connection diagram of the electrochemical deposition of the embodiment of the present invention.
Fig. 2 is the circuit diagram of the AMOLED substrates of the embodiment of the present invention.
Fig. 3 is the structure diagram of the thin film transistor (TFT) of the embodiment of the present invention.
Fig. 4 (a) is the output curve diagram of the thin film transistor (TFT) of the embodiment of the present invention；Fig. 4 (b) is the embodiment of the present invention
Thin film transistor (TFT) transfer characteristic curve figure.
Fig. 5 is the electro-deposition voltage signal that the power cord Vdd terminal being connected with pixel electrode of the embodiment of the present invention applies
Oscillogram.
Fig. 6 (a), Fig. 6 (b), Fig. 6 (c) are respectively electro-deposition monomer under thin film transistor (TFT) TFT control conditions under positive grid voltage
OCNzC (red), OCBzC (yellowish green), OCPC (indigo plant) 200 microns * 200 microns gold (Au) Nanoparticle Modified pixel electrode
On cyclic voltammetry curve；Fig. 6 (d) is that electro-deposition monomer OCNzC (red) exists under thin film transistor (TFT) TFT control conditions under minus gate voltage
Cyclic voltammetry curve on the pixel electrode of 200 microns * 200 microns of Au Nanoparticle Modifieds.
Fig. 7 (a), Fig. 7 (b), Fig. 7 (c) are respectively the OCNzC (red), OCBzC (yellowish green), OCPC deposited on pixel electrode
The fluorescence spectrum of (indigo plant) film.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
The selective orientated deposition method of the organic film of the AMOLED of the present embodiment, comprises the following steps：
(1) using the pixel electrode on AMOLED substrates as working electrode, the thin film transistor (TFT) driving on AMOLED substrates
Circuit connected in series is into the electrolytic cell circuit of electrochemical deposition：
Realize electrolytic cell circuit such as Fig. 1 institutes of the selective orientated deposition method of the organic film of the AMOLED of the present embodiment
Show, electrolytic cell circuit include electrochemical workstation 1, ampere meter 2, voltmeter 3, auxiliary electrode 5, reference electrode 4, electrolyte 6,
AMOLED substrates 7；The auxiliary electrode 5, AMOLED substrates 7 are placed in electrolyte 6；The auxiliary electrode 5 and electrochemical operation
Stand 1 connection；The reference electrode 4 is placed between auxiliary electrode 5, AMOLED substrates 7, and reference electrode 4 connects with electrochemical workstation 1
Connect.
The circuit diagram of the AMOLED substrates of the present embodiment is as shown in Fig. 2, AMOLED substrates include 3 in 1 × 3 array distribution
A pixel electrode and film crystal tube drive circuit, the film crystal tube drive circuit include 3 driving units 11~13, often
A driving unit is by a switching tube, a driving tube, a capacitance composition.By taking driving unit 13 as an example, by a switch
Pipe T1, a driving tube T2, a capacitance C composition, wherein the source electrode of switch transistor T 1 is connected with the grid of driving tube T2, driving tube
The source electrode of T2 is connected with pixel electrode, the both ends grid with driving tube T2, the drain electrode connection respectively of capacitance C；The switch transistor T 1
For addressing, the driving tube T2 is used for the color and grayscale for controlling luminescent device, and the capacitance C is used to store electric charge.Drive
The drain electrode of the switching tube of moving cell 11~13 respectively with data cable Vdata1, Vdata2, Vdata3 connection, driving unit 11~13
The grid of switching tube be connected with scan line Vsel1；The drain electrode of the driving tube of driving unit 11~13 with power cord Vdd1
Connection.
The structure of the thin film transistor (TFT) of the present embodiment as shown in figure 3, provided by Guangzhou New Vision Photoelectric Technology Co., Ltd.,
Transistor is the etching barrier layer structure based on indium gallium zinc oxide (IGZO) semiconductor, including substrate of glass 81, Mo grids 82,
SiNx, SiOx insulating layer 83, IGZO semiconductor layers 84, SiOx etching barrier layers 85, DL1000 passivation layers 86, Mo source electrodes 87, Mo
Drain electrode 88.
Fig. 4 (a) and Fig. 4 (b) is respectively curve of output and the transfer for the thin film transistor (TFT) that breadth length ratio is 30 microns/10 microns
Characteristic curve, the threshold voltage of thin film transistor (TFT) are -0.01 volt, saturation mobility for 15.48 square centimeters/(weber).
Electrochemical deposition experiment is completed on Shanghai Chen Hua company CHI760D electrochemical workstations.We are lied prostrate using circulation
Peace method controls the deposition process of electrodeposited film, and the waveform such as Fig. 5 for the voltage signal that cyclic voltammetric applies shows.Cyclic voltammetry
Scan each time all with deoxidation-reduction of film, be more advantageous to film and go to adulterate, so that beneficial to obtaining high-luminous-efficiency
Film.
(2) the break-make electricity condition in electrolytic cell circuit, simultaneous electrochemical work station are controlled by film crystal tube drive circuit
Export electro-deposition signal；Deposition obtains organic film on the corresponding pixel electrode in the electrolytic cell circuit of "on" position：
The present embodiment is using feux rouges OCNzC, green-yellow light OCBzC, blue light OCPC molecules as electro-deposition monomer, its molecular structure is such as
It is shown below respectively：
Molecular structure mainly includes two parts：1) centre of luminescence：Mainly using fluorenes as basic construction unit, plus proper proportion
Electron acceptor naphtho- thiadiazoles, diazosulfide and spiro fluorene, adjust glow color；2) electric activity center：Carbazole group, and
It is connected by the flexible alkyl chains of suitable length with the centre of luminescence.
Electro-deposition monomer feux rouges OCNzC, green-yellow light OCBzC, blue light OCPC are dissolved in volume ratio as 2 respectively:3 acetonitrile
With in the mixed solution of dichloromethane, concentration is 0.5 mg/ml.Supporting electrolyte is tetrabutyl ammonium hexafluorophosphate, and concentration is
0.1 mol/L.Luminophor used in the present invention is slightly soluble in acetonitrile, in order to increase the concentration of compound, adds dichloromethane
Alkane increases the solubility of luminophor.
By first, second, third row, deposition is upper red respectively, and yellowish green, the process of blue film is as follows：
1st row (feux rouges):Using 3 pixel electrodes of AMOLED substrates as working electrode, feux rouges electro-deposition monomer is placed in
In the electrolyte of molecule (OCNzC), apply positive grid voltage, the second external connection constant voltage power supply to Vsel1 using the first external connection constant voltage power supply
Apply positive grid voltage to Vdata1, the 3rd external connection constant voltage power supply applies minus gate voltage to Vdata2, Vdata3, and electrochemical workstation is given
Vdd1 inputs electro-deposition signal.
Electrolyte is the mixed solution of acetonitrile/dichloromethane (volume ratio 2/3) of 0.5 mg/ml OCNzC, is supported
Electrolyte is the tetrabutyl ammonium hexafluorophosphate of 0.1 mol/L, and the 1st external connection constant voltage power supply applies 10 volts of positive grid voltage to Vsel1,
Second external connection constant voltage power supply applies 10 volts of positive grid voltages to Vdata1, and the 3rd external connection constant voltage power supply applies -5 to Vdata2, Vdata3
Minus gate voltage is lied prostrate, electrochemical workstation is 0~0.835 volt of electro-deposition signal for reference electrode to Vdd1 the input phases., scanning speed
It is 12 circles to spend for 50 mv s, the scanning number of turns, and obtained cyclic voltammetry curve such as Fig. 6 (a) is shown, with the increasing of the scanning number of turns
Add, oxidation and reduction peak current increase successively, show the continuous growth of electrodeposited film, electrolytic cell circuit is conducting state, can
With depositing light-emitting film；1st external connection constant voltage power supply applies 10 volts of positive grid voltage to Vsel1, and the second external connection constant voltage power supply is given
Vdata1 applies -5 volt minus gate voltages, and the 3rd external connection constant voltage power supply applies -5 volt minus gate voltages, electrochemical operation to Vdata2, Vdata3
It is 0~0.835 volt of electro-deposition signal for reference electrode to stand to Vdd1 the input phases, sweep speed be 50 mv s, is scanned
The number of turns is 12 circles, and shown in obtained cyclic voltammetry curve such as Fig. 6 (d), curve electric current is almost 0, that is, electrolytic cell circuit is disconnected
Open state, grows without film.Prove that thin film transistor (TFT) TFT can be as the power on/off shape in a switch control electrolytic cell circuit
State, the generation of coordination electrode reaction is with prohibiting, you can with selective orientated deposition film.
2nd row (green-yellow light):Using AMOLED substrates as working electrode, green-yellow light electro-deposition monomer molecule is placed in
(OCBzC) in electrolyte, positive grid voltage is applied to Vsel1 using the first external connection constant voltage power supply, the second external connection constant voltage power supply is given
Vdata2 applies positive grid voltage, and the 3rd external connection constant voltage power supply applies minus gate voltage to Vdata1, Vdata3, and electrochemical workstation is to Vdd1
Input electro-deposition signal.Shown in OCBzC electro-deposition cyclic voltammetry curve such as Fig. 6 (b).
3rd row (blue light):Using AMOLED substrates as working electrode, the electricity of blue light electro-deposition monomer molecule (OCPC) is placed in
Solving in liquid, apply positive grid voltage to Vsel1 using the first external connection constant voltage power supply, the second external power supply applies positive grid voltage to Vdata3,
For 3rd external power supply to Vdata1, Vdata2 applies minus gate voltage, and electrochemical workstation inputs electro-deposition signal to Vdd1.OCPC is followed
Shown in ring volt-ampere curve such as 6 (c).
Polymerize obtain RGB light-emitting film it is luminous uniformly, illumination effect is preferable, and atomic force microscope tests to obtain
The results show film surface appearance be closelypacked fine particle, obtained film flatness is high, red, yellowish green, and indigo plant shines
The root mean square roughness of film is respectively 1.756 nanometers, 1.942 nanometers, 2.164 nanometers, and fluorescence property is preferable, suitable for Organic Electricity
Electroluminescence device.The fluorescence spectrum of red, yellowish green, blue light-emitting film is shown respectively such as Fig. 7 (a), Fig. 7 (b), Fig. 7 (c), corresponding
Transmitting peak position is respectively 637 nanometers (feux rouges), 560 nanometers (green-yellow lights), 425 nanometers (blue lights).
The process that organic light emitting diode device is prepared using the organic film of the present embodiment is as follows：
Electro-deposition light-emitting film after cleaning, when drying 24 is small under vacuum, temperature is 25 DEG C, obtains the thin of drying
Film, less than 3*10-4Under the vacuum condition of pa, cathode of the evaporated metal layer as organic light emitting diode device, evaporation fluorination
The thickness of caesium and aluminium is respectively 1 nanometer and 120 nanometers.Device architecture is ITO/Au/ light-emitting films/CsF/Al.Wherein deposit
Light-emitting film thickness is about 80 nanometers, and the thickness of Au is 1 nanometer.
Using constant voltage source at the same time to the feux rouges prepared, green-yellow light, the anode of blue light organic emissive diode component
(ITO), cathode (Al) applies 7 volts of voltage, can be launched feux rouges, green-yellow light, the Organic Light Emitting Diode of blue light at the same time.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from the embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (2)
1. a kind of selective orientated deposition method of organic film, it is characterised in that comprise the following steps：
(1) using m pixel electrode of AMOLED substrates as working electrode, the thin film transistor (TFT) on AMOLED substrates is driven into electricity
Road is connected in series in the electrolytic cell circuit of electrochemical deposition；The electrolytic cell circuit of the electrochemical deposition include electrochemical workstation,
Reference electrode, working electrode, auxiliary electrode；m≥1；
The auxiliary electrode, working electrode are placed in electrolyte；The auxiliary electrode is connected with electrochemical workstation；M picture
Plain electrode is connected with m driving unit of film crystal tube drive circuit respectively, film crystal tube drive circuit and electrochemistry work
Make station connection；The reference electrode is placed between auxiliary electrode, working electrode, and reference electrode is connected with electrochemical workstation；
(2) the break-make electricity condition in electrolytic cell circuit, the output of simultaneous electrochemical work station are controlled by film crystal tube drive circuit
Electro-deposition signal；Deposition obtains organic film on the corresponding pixel electrode in the electrolytic cell circuit of "on" position；
The driving unit is made of a switching tube, a driving tube, a capacitance, wherein the source electrode and driving tube of switching tube
Grid connection, the source electrode of driving tube be connected with pixel electrode, the both ends grid with driving tube and the connection that drains respectively of capacitance；
The grid of the switching tube is connected with scan line, and drain electrode is connected with data cable；The drain electrode of the driving tube connects with power cord
Connect；
The switching tube is used to address, and the driving tube is used for the color and grayscale for controlling luminescent device, and the capacitance is used for
Store electric charge；
The AMOLED substrates are 1 × n array, n >=1；
The electrochemical workstation is using the deposition process of cyclic voltammetry control electrodeposited film, and pixel electrode is relative to reference
The voltage range of electrode is 0~0.835 volt, and sweep speed is 50 mv s, and the scanning number of turns is 12 circles；
The method of the i-th row deposition of organic thin film on pixel electrode substrate is as follows：
AMOLED substrates are dipped into the electrolyte of jth kind electro-deposition monomer, the scan line of n row pixel electrode connection is applied
Positive grid voltage；Positive grid voltage is applied to the data cable of the i-th row pixel electrode connection, the data cable of other row pixel electrodes connection, which applies, to be born
Grid voltage；Electrochemical workstation inputs electro-deposition signal to the power cord that n row pixel electrode connects；
Wherein, 1≤i≤n；j≥1.
2. the selective orientated deposition method of organic film according to claim 1, it is characterised in that the organic film
For any one in feux rouges film, blue light film, green light film.
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| CN106876593B (en) * | 2017-03-08 | 2019-05-14 | 中国工程物理研究院材料研究所 | A kind of preparation method of the organic film with array structure |
| CN107275521A (en) * | 2017-05-24 | 2017-10-20 | 华南理工大学 | A kind of preparation method and applications of high-resolution array organic film |
| CN108091776A (en) * | 2017-11-27 | 2018-05-29 | 华南理工大学 | Electrochemical deposition colorful film preparation method and device based on chip controls |
| WO2020136713A1 (en) * | 2018-12-25 | 2020-07-02 | シャープ株式会社 | Method for manufacturing light-emitting device |
| CN111403631A (en) * | 2020-03-30 | 2020-07-10 | 华南理工大学 | Micro-cavity structure top emitting device and preparation method thereof |
| CN112786821B (en) * | 2021-02-05 | 2022-11-18 | 华南理工大学 | Preparation method of OLED display screen |
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| CN104659066A (en) * | 2015-02-05 | 2015-05-27 | 京东方科技集团股份有限公司 | Display panel and manufacturing method thereof, as well as display device |
| CN105047131A (en) * | 2015-07-29 | 2015-11-11 | 深圳丹邦投资集团有限公司 | AMOLED pixel circuit control method |
| CN105182597A (en) * | 2015-10-10 | 2015-12-23 | 深圳市华星光电技术有限公司 | Manufacture method for COA type array substrate and manufacture method for color film substrate |
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