CN105336859A - Organic micromolecule thin film electrical bistable device and manufacturing method thereof - Google Patents
Organic micromolecule thin film electrical bistable device and manufacturing method thereof Download PDFInfo
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- CN105336859A CN105336859A CN201510629158.XA CN201510629158A CN105336859A CN 105336859 A CN105336859 A CN 105336859A CN 201510629158 A CN201510629158 A CN 201510629158A CN 105336859 A CN105336859 A CN 105336859A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
- H10K10/50—Bistable switching devices
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- H—ELECTRICITY
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- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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Abstract
The invention relates to an organic micromolecule thin film electrical bistable device and a manufacturing method thereof. The organic micromolecule thin film electrical bistable device comprises an electrode layer, a functional layer, a conductive layer and a substrate which are arranged from the top to the bottom in turn. The substrate, the conductive layer, the functional layer and the electrode layer are connected in turn. The conductive layer is a thin film of polymethyl methacrylate, and the functional layer is the thin film of tris[2-phenylpyridine-C2,N]iridium(III); or the conductive layer is silicon dioxide through vacuum evaporation, and the functional layer is the thin film of tris[2-phenylpyridine-C2,N]iridium(III). According to the organic micromolecule thin film electrical bistable device and the manufacturing method thereof, the conductive state of the device can be regulated by applying external bias voltage, difference effects of device current can be presented under the same voltage, and the maximum current difference of the sample device can be 104 times; meanwhile, cycle testing of "write-in, reading, erasing and reading" is performed on the device by applying periodic voltage pulse signals so that reuse capacity of the device can be tested, and relatively high switch ratio of the sample device is maintained in the cycle testing.
Description
Technical field
The present invention relates to organic optoelectronic technical field, is a kind of organic molecule thin-film electro bistable device and preparation method thereof specifically.Be espespecially conductive layer with polymer, based on organic molecule thin-film electro bistable device and preparation method thereof.
Background technology
Electric bi-stable is the fundamental characteristics of semiconductor memory component, and its principal phenomena is: device there will be two kinds of different conduction states under identical applied voltage.Specifically, when applying voltage on the functional layer film both sides of device, along with the change of voltage, the conductive characteristic of device also changes thereupon.When applied voltage is removed, the conduction state occurring to change can keep for a long time.And applying reverse voltage can make again the conduction state of device reduce, difference the is corresponding write of memory element, reading and erase process.
In recent years, along with information technology is to low carbonization, low cost, portable, high power capacity and respond future development fast, be that the memory technology of medium reaches Development limitation gradually with inorganic semiconductor, and as memory device prepared by functional layer, there is the advantages such as cost is low, technique is simple, pliability is good, structure is changeable, device size is little based on organic material and become the memory having application prospect most, regain the concern of academia, and achieved and develop rapidly.
At present, organic molecule film is prepared simply and effect stability due to it, obtains everybody concern.Utilize the physicochemical characteristics of different organic molecules, annealed process produces phenomenon of phase separation, at interface meeting defectiveness, makes device have charge storage, can produce stable device, have good application prospect in organic field of storage.
Summary of the invention
For the defect existed in prior art, the object of the present invention is to provide a kind of organic molecule thin-film electro bistable device and preparation method thereof, device can regulate its conduction state by applying bias, under same voltage, device current has different effects, and the difference between current of samples devices is maximum reaches 10
4doubly; Meanwhile, by applying periodic voltage pulse signal device carried out to the loop test of " write, read, erasing, to read ", reuse ability with what check device, samples devices maintains larger on-off ratio in loop test.
For reaching above object, the technical scheme that the present invention takes is:
A kind of organic molecule thin-film electro bistable device, it is characterized in that, comprising: the electrode layer 4 from top to bottom set gradually, functional layer 3, conductive layer 2, substrate 1, substrate, conductive layer, functional layer, electrode layer are connected in turn;
The film of conductive layer to be 2 be polymethyl methacrylate, its solvent is ethyl acetate, and functional layer 3 is films that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide;
Or:
The silicon dioxide of conductive layer to be 2 be vacuum evaporation, functional layer 3 is films that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide.
On the basis of technique scheme, described substrate 1 is the glass substrate with electric conducting material, and described electric conducting material is tin indium oxide.
On the basis of technique scheme, the material of described electrode layer 4 is low-work-function material.
On the basis of technique scheme, when " film of conductive layer to be 2 be polymethyl methacrylate, its solvent is ethyl acetate; functional layer 3 is films that three (2-phenylpyridine-C2; N) close iridium (III), and its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate 1 is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, the ITO in substrate 1, as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: spin coating polymethyl methacrylate forms conductive layer 2 on the base 1, and its solvent is ethyl acetate, and concentration is 30 ~ 50mg/ml; Spin coating degree of turning is 500 ~ 1500r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 20 ~ 40min, and solvent is volatilized completely;
Step 3: in a nitrogen environment, spin coating three (2-phenylpyridine-C2 on conductive layer 2, N) close iridium (III) and form functional layer 3, its solvent is dimethyl formamide, concentration is 5mg/ml ~ 10mg/ml, spin coating degree of turning is 500 ~ 2000r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 10 ~ 30min, and solvent is volatilized completely, allows Ir (ppy) simultaneously
3crystallization better;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer 3, utilize mask plate, evaporation low-work-function material forms electrode layer 4, and thickness is 120nm ~ 200nm.
On the basis of technique scheme, when " film of conductive layer to be 2 be polymethyl methacrylate, its solvent is ethyl acetate; functional layer 3 is films that three (2-phenylpyridine-C2; N) close iridium (III), and its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate 1 is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, the ITO in substrate 1, as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: spin coating polymethyl methacrylate forms conductive layer 2 on the base 1, and its solvent is ethyl acetate, and concentration is 30 ~ 50mg/ml; Spin coating degree of turning is 500 ~ 1500r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 20 ~ 40min, and solvent is volatilized completely;
Step 3: use vacuum evaporation Ir (ppy)
3method, make its thickness reach 40 ~ 80nm, the temperature of vacuum evaporation is 180 DEG C ~ 260 DEG C;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer 3, utilize mask plate, evaporation low-work-function material forms electrode layer 4, and thickness is 120nm ~ 200nm.
On the basis of technique scheme, when " silicon dioxide of conductive layer to be 2 be vacuum evaporation, functional layer 3 is films that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate 1 is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, the ITO in substrate 1, as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: vacuum evaporation silicon dioxide forms conductive layer 2 on the base 1, and vacuum evaporation is 10 at air pressure
-4carry out under the vacuum condition of Pa, vacuum evaporation thickness is 20 ~ 60nm;
Step 3: in a nitrogen environment, spin coating three (2-phenylpyridine-C2 on conductive layer 2, N) close iridium (III) and form functional layer 3, its solvent is dimethyl formamide, concentration is 5mg/ml ~ 10mg/ml, spin coating degree of turning is 500 ~ 2000r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 10 ~ 30min, and solvent is volatilized completely, allows Ir (ppy) simultaneously
3crystallization better;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer 3, utilize mask plate, evaporation low-work-function material forms electrode layer 4, and thickness is 120nm ~ 200nm.
On the basis of technique scheme, when " silicon dioxide of conductive layer to be 2 be vacuum evaporation, functional layer 3 is films that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate 1 is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, the ITO in substrate 1, as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: vacuum evaporation silicon dioxide forms conductive layer 2 on the base 1, and vacuum evaporation is 10 at air pressure
-4carry out under the vacuum condition of Pa, vacuum evaporation thickness is 20 ~ 60nm;
Step 3: use vacuum evaporation Ir (ppy)
3method, make its thickness reach 40 ~ 80nm, the temperature of vacuum evaporation is 180 DEG C ~ 260 DEG C;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer 3, utilize mask plate, evaporation low-work-function material forms electrode layer 4, and thickness is 120nm ~ 200nm.
Organic molecule thin-film electro bistable device of the present invention and preparation method thereof, device can regulate its conduction state by applying bias, and under same voltage, device current has different effects, and the difference between current of samples devices is maximum reaches 10
4doubly; Meanwhile, by applying periodic voltage pulse signal device carried out to the loop test of " write, read, erasing, to read ", reuse ability with what check device, samples devices maintains larger on-off ratio in loop test.
Accompanying drawing explanation
The present invention has following accompanying drawing:
Fig. 1 structure chart of the present invention;
The i-v curve of Fig. 2 device 1 of the present invention;
The i-v curve of Fig. 3 device 2 of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
As shown in Figure 1, organic molecule thin-film electro bistable device of the present invention, comprising: the electrode layer 4 from top to bottom set gradually, functional layer 3, conductive layer 2, substrate 1, and substrate, conductive layer, functional layer, electrode layer are connected in turn;
The film of conductive layer to be 2 be polymethyl methacrylate, its solvent is ethyl acetate, and functional layer 3 is films that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide; The dual stabilization part that this scheme is prepared is called device 1;
Or:
The silicon dioxide of conductive layer to be 2 be vacuum evaporation, functional layer 3 is films that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide; The dual stabilization part that this scheme is prepared is called device 2.
On the basis of technique scheme, described substrate 1 is the glass substrate with electric conducting material, and described electric conducting material is tin indium oxide (ITO).
On the basis of technique scheme, the material of described electrode layer 4 is low-work-function material, comprises and is not limited to silver, aluminium, lithium, calcium.Aluminium is preferred.
Organic molecule thin-film electro bistable device of the present invention, the preparation process of device 1 is:
Step 1: substrate 1 is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, the ITO in substrate 1, as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min, preferred 15min in UV ozone environment;
Step 2: spin coating polymethyl methacrylate (PMMA) forms conductive layer 2 on the base 1, its solvent is ethyl acetate, and concentration is 30 ~ 50mg/ml, preferred 50mg/ml; Spin coating degree of turning is 500 ~ 1500r/min, and preferred rotating speed is 1000r/min; Rotational time is 40 ~ 60S, and the preferred time is 40S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, preferably 100 DEG C; Annealing time is 20 ~ 40min, preferred 40min, and solvent is volatilized completely;
Step 3: in a nitrogen environment, on conductive layer 2, iridium (III) (Ir (ppy) is closed in spin coating three (2-phenylpyridine-C2, N)
3) forming functional layer 3, its solvent is dimethyl formamide, and concentration is 5mg/ml ~ 10mg/ml (experimental point is 5mg/ml), and spin coating degree of turning is 500 ~ 2000r/min, and preferred rotating speed is 1000r/min; Rotational time is 40 ~ 60S, and the preferred time is 40S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, preferably 100 DEG C; Annealing time is 10 ~ 30min, preferred 20min; Solvent is volatilized completely, allows Ir (ppy) simultaneously
3crystallization better;
The spin coating process of step 3 completes in glove box;
This step also can use vacuum evaporation Ir (ppy)
3method, make its thickness reach 40 ~ 80nm, preferred 60nm, the temperature of vacuum evaporation is 180 DEG C ~ 260 DEG C, and preferable temperature is 256 DEG C;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer 3, utilize mask plate, evaporation low-work-function material formed electrode layer 4, experimental selection be aluminium, thickness is 120nm ~ 200nm, and preferred thickness is 180nm.
The electrostrictive polymer bistable device that above-mentioned making obtains, decreases operating process, owing to adopting vacuum spin coating, improves film forming, improves element manufacturing efficiency, have a good application prospect.
Organic molecule thin-film electro bistable device of the present invention, the preparation process of device 2 is:
Step 1: substrate 1 is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, the ITO in substrate 1, as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min, preferred 15min in UV ozone environment;
Step 2: vacuum evaporation silicon dioxide forms conductive layer 2 on the base 1, and vacuum evaporation is 10 at air pressure
-4carry out under the vacuum condition of Pa, vacuum evaporation thickness is 20 ~ 60nm, preferred 40nm;
Step 3: in a nitrogen environment, on conductive layer 2, iridium (III) (Ir (ppy) is closed in spin coating three (2-phenylpyridine-C2, N)
3) forming functional layer 3, its solvent is dimethyl formamide, and concentration is 5mg/ml ~ 10mg/ml (experimental point is 5mg/ml), and spin coating degree of turning is 500 ~ 2000r/min, and preferred rotating speed is 1000r/min; Rotational time is 40 ~ 60S, and the preferred time is 40S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, preferably 100 DEG C; Annealing time is 10 ~ 30min, preferred 20min; Solvent is volatilized completely, allows Ir (ppy) simultaneously
3crystallization better;
The spin coating process of step 3 completes in glove box;
This step also can use vacuum evaporation Ir (ppy)
3method, make its thickness reach 40 ~ 80nm, preferred 60nm, the temperature of vacuum evaporation is 180 DEG C ~ 260 DEG C, and preferable temperature is 256 DEG C;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer 3, utilize mask plate, evaporation low-work-function material formed electrode layer 4, experimental selection be aluminium, thickness is 120nm ~ 200nm, and preferred thickness is 180nm.
The electrostrictive polymer bistable device that above-mentioned making obtains, decreases operating process, owing to adopting vacuum spin coating, improves film forming, improves element manufacturing efficiency, have a good application prospect.
As shown in Figure 2, the i-v curve of device 1.As can be seen from the figure device has obvious high low state, on-off ratio 10
3above, maximumly 10 are reached
4,the condition of memory storage can well be met.
As shown in Figure 3, the i-v curve of device 2.As can be seen from the figure device has obvious high low state, on-off ratio 10
2above, maximumly 10 are reached
3,the condition of memory storage can be met.
On the basis of technique scheme, the spin coating process of the organic molecule functional layer of step 3 completes in glove box.
The content be not described in detail in this specification belongs to the known prior art of professional and technical personnel in the field.
Claims (7)
1. an organic molecule thin-film electro bistable device, it is characterized in that, comprise: the electrode layer (4) from top to bottom set gradually, functional layer (3), conductive layer (2), substrate (1), substrate, conductive layer, functional layer, electrode layer are connected in turn;
Conductive layer is the film that (2) are polymethyl methacrylate, and its solvent is ethyl acetate, and functional layer (3) is the film that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide;
Or:
Conductive layer is the silicon dioxide that (2) are vacuum evaporation, and functional layer (3) is the film that three (2-phenylpyridine-C2, N) close iridium (III), and its solvent is dimethyl formamide.
2. organic molecule thin-film electro bistable device as claimed in claim 1, is characterized in that: described substrate (1) is the glass substrate with electric conducting material, and described electric conducting material is tin indium oxide.
3. organic molecule thin-film electro bistable device as claimed in claim 1, is characterized in that: the material of described electrode layer (4) is low-work-function material.
4. organic molecule thin-film electro bistable device as claimed in claim 1, it is characterized in that: when " conductive layer is the film that (2) are polymethyl methacrylate; its solvent is ethyl acetate; functional layer (3) is the film that three (2-phenylpyridine-C2; N) close iridium (III); its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate (1) is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, ITO in substrate (1), as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: form conductive layer (2) at the upper spin coating polymethyl methacrylate of substrate (1), its solvent is ethyl acetate, and concentration is 30 ~ 50mg/ml; Spin coating degree of turning is 500 ~ 1500r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 20 ~ 40min, and solvent is volatilized completely;
Step 3: in a nitrogen environment, at the upper spin coating three (2-phenylpyridine-C2 of conductive layer (2), N) close iridium (III) and form functional layer (3), its solvent is dimethyl formamide, concentration is 5mg/ml ~ 10mg/ml, spin coating degree of turning is 500 ~ 2000r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 10 ~ 30min, and solvent is volatilized completely, allows Ir (ppy) simultaneously
3crystallization better;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer (3), utilize mask plate, evaporation low-work-function material forms electrode layer (4), and thickness is 120nm ~ 200nm.
5. organic molecule thin-film electro bistable device as claimed in claim 1, it is characterized in that: when " conductive layer is the film that (2) are polymethyl methacrylate; its solvent is ethyl acetate; functional layer (3) is the film that three (2-phenylpyridine-C2; N) close iridium (III); its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate (1) is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, ITO in substrate (1), as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: form conductive layer (2) at the upper spin coating polymethyl methacrylate of substrate (1), its solvent is ethyl acetate, and concentration is 30 ~ 50mg/ml; Spin coating degree of turning is 500 ~ 1500r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 20 ~ 40min, and solvent is volatilized completely;
Step 3: use vacuum evaporation Ir (ppy)
3method, make its thickness reach 40 ~ 80nm, the temperature of vacuum evaporation is 180 DEG C ~ 260 DEG C;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer (3), utilize mask plate, evaporation low-work-function material forms electrode layer (4), and thickness is 120nm ~ 200nm.
6. organic molecule thin-film electro bistable device as claimed in claim 1, it is characterized in that: when " conductive layer is the silicon dioxide that (2) are vacuum evaporation; functional layer (3) is the film that three (2-phenylpyridine-C2; N) close iridium (III); its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate (1) is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, ITO in substrate (1), as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: form conductive layer (2) at the upper vacuum evaporation silicon dioxide of substrate (1), vacuum evaporation is 10 at air pressure
-4carry out under the vacuum condition of Pa, vacuum evaporation thickness is 20 ~ 60nm;
Step 3: in a nitrogen environment, at the upper spin coating three (2-phenylpyridine-C2 of conductive layer (2), N) close iridium (III) and form functional layer (3), its solvent is dimethyl formamide, concentration is 5mg/ml ~ 10mg/ml, spin coating degree of turning is 500 ~ 2000r/min, and rotational time is 40 ~ 60S; After treating that spin coating is complete, need carry out annealing in process, annealing temperature is 80 ~ 120 DEG C, and annealing time is 10 ~ 30min, and solvent is volatilized completely, allows Ir (ppy) simultaneously
3crystallization better;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer (3), utilize mask plate, evaporation low-work-function material forms electrode layer (4), and thickness is 120nm ~ 200nm.
7. organic molecule thin-film electro bistable device as claimed in claim 1, it is characterized in that: when " conductive layer is the silicon dioxide that (2) are vacuum evaporation; functional layer (3) is the film that three (2-phenylpyridine-C2; N) close iridium (III); its solvent is dimethyl formamide ", preparation process is:
Step 1: substrate (1) is successively put into acetone, ethanol cleans, and respectively carry out the ultrasonic cleaning of 30 minutes, ITO in substrate (1), as anode electrode, then after nitrogen fluidized drying, processes 10 ~ 20min in UV ozone environment;
Step 2: form conductive layer (2) at the upper vacuum evaporation silicon dioxide of substrate (1), vacuum evaporation is 10 at air pressure
-4carry out under the vacuum condition of Pa, vacuum evaporation thickness is 20 ~ 60nm;
Step 3: use vacuum evaporation Ir (ppy)
3method, make its thickness reach 40 ~ 80nm, the temperature of vacuum evaporation is 180 DEG C ~ 260 DEG C;
Step 4: be 10 in vacuum degree
-4under Pa environment, in functional layer (3), utilize mask plate, evaporation low-work-function material forms electrode layer (4), and thickness is 120nm ~ 200nm.
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WO2020151711A1 (en) * | 2019-01-21 | 2020-07-30 | 京东方科技集团股份有限公司 | Display unit, display substrate, driving method thereof and display device |
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