CN110492001A - A kind of organic photodetector and preparation method thereof based on spin coating heating process - Google Patents
A kind of organic photodetector and preparation method thereof based on spin coating heating process Download PDFInfo
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- CN110492001A CN110492001A CN201910803577.9A CN201910803577A CN110492001A CN 110492001 A CN110492001 A CN 110492001A CN 201910803577 A CN201910803577 A CN 201910803577A CN 110492001 A CN110492001 A CN 110492001A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention discloses a kind of organic photodetectors based on spin coating heating process, including the substrate set gradually from top to bottom, conductive cathode, electron transfer layer, photoactive layer, hole transmission layer and metal anode, the photoactive layer after electron donor material and electron acceptor material mixture through spin coating heating process by being made, and the invention also discloses the preparation methods of the photodetector.The present invention is by placing heating sheet around spin coating instrument turntable, the influence of the cold airflow and environment that generate due to turntable high speed rotation can be neutralized, so that the quality of forming film of device greatly promotes, this also can reduce the roughness of active layer surface, the film of formation is more evenly, it is easy the production of large area, optimizes the contact between electron transfer layer and active layer, the final overall performance for promoting device.
Description
Technical field
The present invention relates to organic semiconductor thin-film photodetector technical fields, more particularly to one kind to be based on spin coating heater
Organic photodetector of skill and preparation method thereof.
Background technique
Organic photodetector is using with the sensor that can be realized photoelectric conversion made of photoelectric material.
Traditional optical detector is made of inorganic semiconductor material, and complex manufacturing technology is at high cost, and is unsuitable for making large area device
Part.It is light since organic material has efficient photaesthesia, it inexpensive, the features such as processing performance is excellent, is easier to prepare small size,
Low-power consumption, inexpensive sensitive detection parts can make up for it equipment valuableness generally existing in inorganic optical detector, complex process etc.
Defect.Miscellaneous organic semiconducting materials also provide very big may be selected for the development and innovation of organic photodetector part
Property, synthesize the new material with corresponding photoelectric characteristic as needed.Therefore organic photodetector will be empty with bigger research
Between and commercial value, such as in astronomy, environmental monitoring, light splitting and medicine detector device etc..
In transoid device, when spin coating active layer, uses P3HT:IEICO-4F as active layer, then solvent anneal to be formed
Active layer film.But during spin coating active layer solution, due to by weather, revolving speed influenced so that film exists
Quality of forming film is very poor in relative temperature and the biggish environment of humidity, and surface topography roughness is high.This not only will affect active layer
Internal carrier transport and separation, can also to possess biggish interface contact resistance between electron transfer layer and active layer,
This will reduce the electron transport ability of electron transfer layer.Therefore, how research with a kind of spin coating proceeding of optimization prepares height
Quality, uniform active layer film, is one of emphasis and difficult point of current organic photodetector area research.
Summary of the invention
It is an object of the invention to: a kind of organic photodetector based on spin coating heating process and its preparation side are provided
Method can reduce the influence of the cold airflow and the clammy air of surrounding that are generated due to turntable high speed rotation, keep the active layer to be formed thin
Film is more smooth, to reduce the defect of active layer, improves device performance, while it is good by spin-coating film to solve active layer
The low problem of product rate, and then improve the whole yields of device.
The technical solution adopted by the invention is as follows:
To achieve the above object, the present invention provides a kind of organic photodetector based on spin coating heating process, including light
Active layer, the photoactive layer after electron donor material and electron acceptor material mixture through spin coating heating process by being made；
Preferably, the electron donor material is P3HT, electron acceptor material IEICO-4F.
Preferably, the concentration of the P3HT and IEICO-4F mixed solution is the quality of 30mg/mL, P3HT and IEICO-4F
Than for 1:1.
Preferably, the photoactive layer with a thickness of 50~300nm.
Preferably, the photodetector includes the substrate set gradually from top to bottom, conductive cathode, electron-transport
Layer, photoactive layer, hole transmission layer and metal anode.
Preferably, the substrate is made using transparent polymer material, and the transparent polymer material uses polyethylene, gathers
Methyl methacrylate, polycarbonate, polyurethanes, polyimides, vinyl chloride-vinyl acetate resin and polyacrylic acid it is one or more；
The material of the conductive cathode is ITO；The electron transport layer materials are ZnO sol gel solution, with a thickness of 30nm；The sky
It is MoO that layer material is transmitted in cave3, with a thickness of 15nm；The metal anode material is one of Ag, Al and Au or a variety of, thickness
For 100nm.
Preferably, the ZnO sol gel solution is made of zinc acetate and ethanol amine, and the weight of the zinc acetate accounts for 60%
~80%, surplus is ethanol amine.
The present invention also provides a kind of preparation method of organic photodetector based on spin coating heating process, feature exists
In, including following preparation step:
(1) substrate being made of substrate and conductive cathode is cleaned, with being dried with nitrogen after cleaning；
(2) configured ZnO mixed solution is spin-coated to conductive cathode surface, and the substrate after spin coating is subjected to thermal annealing
Processing, the temperature of thermal annealing are 150 DEG C, and time 15min obtains electron transfer layer；
(3) blend solution that spin coating is made of electron donor material and electron acceptor material on the electron transport layer, simultaneously
It is heated in spin coating process, photoactive layer is made；
It (4) is 3 × 10 in vacuum degree3Under the conditions of Pa, MoO is deposited on photoactive layer surface3, hole transmission layer is prepared；
(5) evaporation metal anode on the hole transport layer, is packaged to obtain photodetector later.
Preferably, the heating method in the step (3) are as follows: it is 5cm that a radius is placed around the turntable of spin coating instrument
Cylindrical type heating sheet, so that turntable is in cylindrical center position, heated during spin coating, make the active layer of spin coating in heat source
Under the influence of can be uniform, regularly adhere on the electron transport layer.
Preferably, the heating and temperature control in the step (3) is at 20 DEG C~55 DEG C
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
1. the present invention is heated by introducing in spin coating proceeding, so that the active layer of spin coating can be equal under the influence of heat source
Even, regularly adhere to reduces IEICO-4F on the electron transport layer divides in active layer because of the effect of temperature and humidity
The problem of brought quality of forming film difference is precipitated in uneven and material on cloth, and it is low by spin-coating film yields to solve active layer
Problem, and then improve the whole yields of device.
2. the present invention is heated by introducing in spin coating proceeding, solution can be made in spin-coating film under the influence of heat source
In the process solvent can volatilization more evenly, make active layer inner molecular structure more orderly, solve since acceptor material is assembled
Untight problem is contacted, so that donor and receptor are more equally distributed in active layer, the work formed after annealing can be made
Property layer film it is more fine and close smooth, optimize the contact between active layer and electron transfer layer, reduce the contact resistance between interface, mention
High photoelectric current reduces dark current, improves device performance.
3. the present invention can optimize the pattern of active layer, make the active layer film to be formed more by spin coating heating process
It is smooth, to reduce the defect of active layer, the recombination probability of carrier is reduced, while increasing the dissociation of exciton, improves photoelectric current,
And the production of large area may be implemented.
Detailed description of the invention
Examples of the present invention will be described by way of reference to the accompanying drawings, in which:
Fig. 1 is the structural schematic diagram of photodetector of the present invention；
Fig. 2 is the structural schematic diagram of spin coating heating device of the invention.
In the figure, it is marked as 1- substrate, 2- conductive cathode, 3- electron transfer layer, 4- photoactive layer, 5- hole transmission layer, 6-
Metal anode.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Reference examples
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；In transparent conductive cathode ITO surface spin coating ZnO precursor solution, and carry out thermal anneal process (150
DEG C, 15min) electron transfer layer is prepared, P3HT:IEICO-4F (1:1,30mg/ are prepared using spin-coating method on the electron transport layer
Ml hole transmission layer MoO is deposited on photoactive layer surface in) photoactive layer (800rpm, 30s)3(15nm)；On the hole transport layer
Evaporation metal anode A g (100nm).
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=1.2 × 10 of device-6A/
cm2, photoelectric current (Jph)=2.8 × 10-3A/cm2, specific detecivity (D*)=2.57 × 1011Jones。
Embodiment 1
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, then thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (20 DEG C) preparation P3HT:IEICO- of spin-coating method
Anode buffer layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；In
Evaporation metal anode A g (100nm) on anode buffer layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=1.5 × 10 of device-6A/
cm2, photoelectric current (Jph)=3.4 × 10-3A/cm2, specific detecivity (D*)=4.3 × 1011Jones。
Embodiment 2
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, and carries out thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (25 DEG C) preparation P3HT:IEICO- of spin-coating method
Anode buffer layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；In
Evaporation metal anode A g (100nm) on anode buffer layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=1.33 × 10 of device-6A/
cm2, photoelectric current (Jph)=1.6 × 10-3A/cm2, specific detecivity (D*)=1.77 × 1011Jones。
Embodiment 3
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, and carries out thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (30 DEG C) preparation P3HT:IEICO- of spin-coating method
Hole transmission layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；In
Evaporation metal anode A g (100nm) on hole transmission layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=1.3 × 10 of device-6A/
cm2, photoelectric current (Jph)=6.2 × 10-3A/cm2, specific detecivity (D*)=3.5 × 1011Jones。
Embodiment 4
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, and carries out thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (35 DEG C) preparation P3HT:IEICO- of spin-coating method
Hole transmission layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；In
Evaporation metal anode A g (100nm) on hole transmission layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=0.9 × 10 of device-6A/
cm2, photoelectric current (Jph)=8.4 × 10-3A/cm2, specific detecivity (D*)=7.96 × 1011Jones。
Embodiment 5
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, and carries out thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (40 DEG C) preparation P3HT:IEICO- of spin-coating method
Hole transmission layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；In
Evaporation metal anode A g (100nm) on anode buffer layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=1.22 × 10 of device-6A/
cm2, photoelectric current (Jph)=9.3 × 10-3A/cm2, specific detecivity (D*)=9.64 × 1011Jones。
Embodiment 6
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, and carries out thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (45 DEG C) preparation P3HT:IEICO- of spin-coating method
Layer hole transmission layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；
Evaporation metal anode A g (100nm) on the hole transport layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=1.16 × 10 of device-7A/
cm2, photoelectric current (Jph)=3.03 × 10-2A/cm2, specific detecivity (D*)=1.1 × 1012Jones。
Embodiment 7
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, and carries out thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (50 DEG C) preparation P3HT:IEICO- of spin-coating method
Hole transmission layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；In
Evaporation metal anode A g (100nm) on hole transmission layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=7.3 × 10 of device-5A/cm,
Photoelectric current (Jph)=2.24 × 10-3A/cm2, specific detecivity (D*)=3.45 × 1011Jones。
Embodiment 8
The substrate as composed by transparent substrates and transparent conductive cathode ITO to surface roughness less than 1nm cleans,
With being dried with nitrogen after cleaning；ZnO precursor solution is prepared in transparent conductive cathode ITO surface spin coating, and carries out thermal anneal process
(150 DEG C, 15min) prepare electron transfer layer, on the electron transport layer using heating (55 DEG C) preparation P3HT:IEICO- of spin-coating method
Hole transmission layer MoO is deposited on photoactive layer surface in 4F (1:1,30mg/ml) photoactive layer (800rpm, 30s)3(15nm)；In
Evaporation metal anode A g (100nm) on hole transmission layer.
Under standard test condition: AM 1.5,100mW/cm2, measure the dark current (Jd)=9.25 × 10 of device-5A/
cm2, photoelectric current (Jph)=4.03 × 10-4A/cm2, specific detecivity (D*)=1.27 × 108Jones。
The photoelectric detector performance parameter of the present invention of table 1
As can be seen from Table 1: the organic photodetector for preparing active layer by heating spin-coating method is heated compared to not
Process, density of photocurrent becomes larger, and dark current reduces, it is seen that by being heated during spin coating, so that rotation
The active layer of painting can be uniform under the influence of heat source, regularly adheres on the electron transport layer, reduce IEICO-4F because
The effect of temperature and humidity and be distributed in active layer upper uneven and material be precipitated brought by quality of forming film difference problem, favorably
It is produced in large area, and shows that device performance is optimal when heating temperature is 45 DEG C by experiment repeatedly.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment, or some or all of the technical features are equal
Replacement；And these are modified or replaceed, the model for technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses, should all cover within the scope of the claims and the description of the invention.
Claims (10)
1. a kind of organic photodetector based on spin coating heating process, including photoactive layer, which is characterized in that the photolytic activity
Layer after electron donor material and electron acceptor material mixture through spin coating heating process by being made.
2. a kind of organic photodetector based on spin coating heating process according to claim 1, which is characterized in that described
Electron donor material is P3HT, electron acceptor material IEICO-4F.
3. a kind of organic photodetector based on spin coating heating process according to claim 2, which is characterized in that described
The concentration of P3HT and IEICO-4F mixed solution is that the mass ratio of 30mg/mL, P3HT and IEICO-4F are 1:1.
4. a kind of organic photodetector based on spin coating heating process according to claim 1, which is characterized in that described
Photoactive layer with a thickness of 50~300nm.
5. a kind of organic photodetector based on spin coating heating process according to any one of claims 1 to 4, feature
It is, the photodetector includes the substrate set gradually from top to bottom, conductive cathode, electron transfer layer, photoactive layer,
Hole transmission layer and metal anode.
6. a kind of organic photodetector based on spin coating heating process according to claim 5, which is characterized in that described
Substrate is made using transparent polymer material, and the transparent polymer material uses polyethylene, polymethyl methacrylate, poly- carbon
Acid esters, polyurethanes, polyimides, vinyl chloride-vinyl acetate resin and polyacrylic acid it is one or more；The material of the conductive cathode
For ITO；The electron transport layer materials are ZnO sol gel solution, with a thickness of 30nm；The hole transport layer material is
MoO3, with a thickness of 15nm；The metal anode material is one of Ag, Al and Au or a variety of, with a thickness of 100nm.
7. a kind of organic photodetector based on spin coating heating process according to claim 6, which is characterized in that described
ZnO sol gel solution is made of zinc acetate and ethanol amine, and the weight of the zinc acetate accounts for 60%~80%, and surplus is ethyl alcohol
Amine.
8. the preparation of described in any item a kind of organic photodetectors based on spin coating heating process according to claim 1~7
Method, which is characterized in that including following preparation step:
(1) substrate being made of substrate and conductive cathode is cleaned, with being dried with nitrogen after cleaning；
(2) configured ZnO mixed solution is spin-coated to conductive cathode surface, and the substrate after spin coating is carried out at thermal annealing
Reason, the temperature of thermal annealing are 150 DEG C, and time 15min obtains electron transfer layer；
(3) blend solution that spin coating is made of electron donor material and electron acceptor material on the electron transport layer, while spin coating
It is heated in the process, photoactive layer is made；
It (4) is 3 × 10 in vacuum degree3Under the conditions of Pa, MoO is deposited on photoactive layer surface3, hole transmission layer is prepared；
(5) evaporation metal anode on the hole transport layer, is packaged to obtain photodetector later.
9. a kind of preparation method of organic photodetector based on spin coating heating process according to claim 8, special
Sign is, the heating method in the step (3) are as follows: the cylindrical type that a radius is 5cm is placed around the turntable of spin coating instrument
Heating sheet makes turntable be in cylindrical center position, heats during spin coating, makes the active layer of spin coating under the influence of heat source
Can be uniform, regularly adhere on the electron transport layer.
10. a kind of preparation method of organic photodetector based on spin coating heating process according to claim 8, special
Sign is that the heating and temperature control in the step (3) is at 20 DEG C~55 DEG C.
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