CN106058046B - A kind of organometallic complex p-n junction nanometer crystal preparation method - Google Patents
A kind of organometallic complex p-n junction nanometer crystal preparation method Download PDFInfo
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- CN106058046B CN106058046B CN201610644074.8A CN201610644074A CN106058046B CN 106058046 B CN106058046 B CN 106058046B CN 201610644074 A CN201610644074 A CN 201610644074A CN 106058046 B CN106058046 B CN 106058046B
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- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
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Abstract
Organometallic complex p-n junction nanometer crystal preparation method of the invention, comprising the following specific steps depositing a layer thickness in substrate with the method for vacuum evaporation is 50-2000nm through the amorphous film layer of formula organometallic complex；Obtained above-mentioned film layer is placed upwards, on clean glass sheet cover layer, and is placed it in teat glass, normalizing is sintered 8-24min under 300-400 DEG C of air environment；Stop heating, be cooled to room temperature, control heating condition is different, and the organometallic complex that different structure can be obtained is nanocrystalline；It is passed through organic solvent tetrahydrofuran and hydrogen gas mixture 10min in the nanocrystalline sample preparation pipe of organometallic complex, p-n metal complex crystal can be obtained.By above-mentioned, the present invention shows as p-type and n-type semiconductor wire characteristic under different conformations, while can be used for the fields such as organic semiconductor luminescent device, organic field effect tube, solar battery.
Description
Technical field
The present invention relates to organic semiconductor luminescent device, organic UV detector, area of solar cell, the present invention is to close
In a kind of tool there are two types of the eutectic and its doping method of the hexa-coordinate metal complex of isomers, prepared by vacuum evaporation organic
Metal complex amorphous membrance, then by normalized treatment, the nanocrystalline side of the organometallic complex of different proportion doping is made
Method.
Background technique
Organic semiconductor (organic semiconductor) is the organic material with characteristic of semiconductor, and people are universal
Think, the characteristic of semiconductor of organic matter is derived from conjugated pi structure big present in its molecule, the π track with low energy
(HOMO) regard valence band as, the π * track (LUMO) with high-energy regards conduction band as, and two interorbital energy differences are band gap.Have mostly
Machine semiconductor band gap is 1.5ev-3.0ev, is in ideal visible-range.
Organic semiconducting materials are many kinds of, are broadly divided into polymer, two class of oligomer.Oligomer is broadly divided into gold again
Belong to chelate (Alq3, Gaq3, Znq2 etc.), rubrene, metal phthalocyanine (ZnPc etc.), Oligopoly thiophene (T4 etc.) and other materials
Material.Since organic semiconducting materials have environmental-friendly, cheap, preparation is simple, and the advantages that can prepare flexible device,
Organic semiconducting materials have broad application prospects.(J. Physics:Condensed Matter, 2005,17,
6271-6283, Paramagnetic defect centres in crystalline Alq3; Advanced
Functional Materials, 2003, 13, 108-112, Preparation and characterization of
Blue-luminescent tris (8-hydroxyquinaline) aluminum (Alq3)) still, due to organic semiconductor
The carrier mobility of material is low, largely limits its application, so, the method for generalling use doping changes it
Property processing.Carrier concentration and mobility can be not only greatly improved by doping, the luminescent color of device can also be changed.Example
Such as, the devices such as organic light emission or solar battery can improve the luminous quantum efficiency of device by doping；In organic light emission
Devices field can also change emission wavelength by doping.(Advanced Functional Materials, 2006,16,
1985-1991, Photoluminescence and electroluminescence from tris (8-
hydroxyquinoline)aluminum nanowires prepared by adsorbent-assisted physical
vapor deposition；Advanced Functional Materials, 2006,16,819-823,
Crystallization of amorphous tris(8-hydroxyquinoline)aluminum nanoparticles
and transformation to nanowires; Advanced Materials, 2008, 20, 2747-2750,
Alq3 nanorods:Promising building blocks for optical devices.)
Organic layer in the devices all uses amorphous film layer mostly, but there are a large amount of impurity and lacks in amorphous film layer
It falls into, is largely affected by the mobility of carrier, in order to reduce the influence of magazine and defect to there is several layers of middle carrier transports,
Amorphous film layer can be replaced using organic semi-conductor crystal structure.This is because the homogeneity of crystal and the spy of stable structure
Property, there is excellent carrier transport efficiency and thermal stability, the performance of device can be promoted.
Nanocrystal is the polycrystalline on nano-scale, and crystal is in the size of nanometer scale, sound, light, electricity, thermal and magnetic etc.
Performance can change.Nanocrystal is divided into 3-D nano, structure, two-dimensional nanostructure, one-dimensional nano structure and zero-dimension nano knot
Structure, wherein one-dimensional nano structure is received significant attention because of its bright prospects in nano-device application.General inorganic material
The preparation method of material is not suitable for organic material, and the preparation method of organic monodimension nanometer material mainly has: physical vapor transport,
Template and solwution method.
Monodimension nanometer material has unique photoelectric property, can be used for organic field effect tube device (OFET), has
Machine light emitting semiconductor device (OLED), the fields such as organic solar batteries (OPV).
Summary of the invention
The invention mainly solves the technical problem of providing a kind of organometallic complex p-n junction nanometer crystal preparation method,
Different proportion is obtained using annealing and adulterates through formula structure and face-type structural nanocrystalline, what is obtained is nanocrystalline for rodlike knot
Structure shows as p-type and n-type semiconductor wire characteristic under different conformations, while the nanocrystalline organic semiconductor that can be used for is sent out
The fields such as optical device, organic field effect tube, solar battery.
In order to solve the above technical problems, one technical scheme adopted by the invention is that: provide a kind of organic metal cooperation
Object p-n junction nanometer crystal preparation method, comprising the following specific steps
Comprising the following specific steps
Step 1: depositing a layer thickness in substrate with the method for vacuum evaporation is 50-2000nm through formula organometallic ligand
Close the amorphous film layer of object；
Step 2: obtained above-mentioned film layer being placed upwards, on clean glass sheet cover layer, and places it on glass
In glass test tube, normalizing is sintered 8-24min under 300-400 DEG C of air environment；
Step 3: stopping heating, be cooled to room temperature, control heating condition is different, and the organic metal of different structure can be obtained
Complex is nanocrystalline；
Step 4: being passed through organic solvent tetrahydrofuran in the nanocrystalline sample preparation pipe of organometallic complex and hydrogen is mixed
Gas 10min is closed, p-n metal complex crystal can be obtained.
In a preferred embodiment of the present invention, the vacuum evaporation uses the vacuum pressure of 10-2-10-5Pa.
In a preferred embodiment of the present invention, it includes p-type and n-type semiconductor that the organometallic complex is nanocrystalline
The nanometer rods of doping.
In a preferred embodiment of the present invention, it is club shaped structure that the organometallic complex is nanocrystalline, and diameter is
0.2-1 μm, 2-60 μm of length.
In a preferred embodiment of the present invention, it is formed by the way that the organometallic complex is nanocrystalline in substrate surface
Efficent electronic transmission and electronics transfer layer.
The beneficial effects of the present invention are: a kind of organometallic complex p-n junction nanometer crystal preparation method of the invention, passes through
Simple doping method forms organic semiconductor eutectics and organic semiconductor pn-junction, obtains different proportion through formula using annealing
Structure and face-type structural doping it is nanocrystalline, what is obtained is nanocrystalline for club shaped structure, shows as p-type and n under different conformations
Type semiconductor lead characteristic, while this nanocrystalline can be used for organic semiconductor luminescent device, organic field effect tube, solar energy
The fields such as battery.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing, in which:
Fig. 1 is Alq3Organic semiconductor p-n junction fluorescence microscope picture；
Fig. 2 is Alq3Organic semiconductor eutectic fluorescence microscope picture；
Fig. 3 is the Alq adulterated through formula structure and face-type structural3Nanocrystalline PL spectrogram；
Fig. 4 is the organic electroluminescence device schematic diagram based on PN junction；
Fig. 5 is the organic field effect tube schematic diagram based on PN junction；
Fig. 6 is the solar cell device schematic diagram based on PN junction.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The embodiment of the present invention includes:
A kind of organometallic complex p-n junction nanometer crystal preparation method, comprising the following specific steps
Step 1: depositing a layer thickness in substrate with the method for vacuum evaporation is 50-2000nm through formula organometallic ligand
Close the amorphous film layer of object；
Step 2: obtained above-mentioned film layer being placed upwards, on clean glass sheet cover layer, and places it on glass
In glass test tube, normalizing is sintered 8-24min under 300-400 DEG C of air environment；
Step 3: stopping heating, be cooled to room temperature, control heating condition is different, and the organic metal of different structure can be obtained
Complex is nanocrystalline；
Step 4: being passed through organic solvent tetrahydrofuran in the nanocrystalline sample preparation pipe of organometallic complex and hydrogen is mixed
Gas 10min is closed, p-n metal complex crystal can be obtained.
Among the above, the vacuum evaporation uses the vacuum pressure of 10-2-10-5Pa；The organometallic complex is received
Meter Jing includes the nanometer rods of p-type and n-type semiconductor doping, and the nanocrystalline organometallic complex is club shaped structure, diameter
It is 0.2-1 μm, 2-60 μm of length.
Wherein, nanocrystalline by the organometallic complex, using the metal complex nano bar-shape structure, in base
Bottom surface forms efficent electronic transmission and electronics transfer layer, realizes the preparation of high efficiency organic electroluminescence device；Utilize the metal
Complex nano bar-shape structure, substrate surface formed efficent electronic transmission and electronics transfer layer by the nano wire prepare it is organic too
Positive energy battery obtains incident photon-to-electron conversion efficiency with high.
The present invention relates to the eutectics and its doping method of a kind of metal complex with isomers, in report before
In, metal organic complex is modified by ligand modified method mostly.And this method obtains difference using annealing
Ratio is adulterated nanocrystalline through formula structure and face-type structural.This method obtains nanocrystalline for club shaped structure, in different conformations
Under show as p-type and n-type semiconductor wire characteristic.The preparation method that the present invention relates to organic semiconductor crystalline substances as adulterating PN junction, together
When this nanocrystalline can be used for the fields such as organic semiconductor luminescent device, organic field effect tube, solar battery.
The organic semiconductor eutectic that it is an object of the invention to be adulterated by organic semiconductor.Another mesh of the invention
Be to be formed through two kinds of isomers of formula structure and face-type structural form organic semiconductor pn-junction.To achieve the goals above,
It is proposed by the present invention the preparation method comprises the following steps: by vacuum evaporation, then be heat-treated the method for (annealing) to prepare organometallic ligand
It is nanocrystalline to close object, by changing heat treatment temperature and time, is adulterated to control to obtain different proportion through formula structure and face-type structural
Organometallic complex it is nanocrystalline.
This is nanocrystalline can to form on quartz glass, ito glass and silicon wafer and receives micron film, and the thicknesses of layers of formation exists
Between 200-5000nm, it can be used as preparing and assembling organic light emitting semiconductor device.
The method of the present invention can be used for preparing Alq3And its derivative, Ir (ppy) 3And its derivative, Gaq3And its derivative
Equal metal organic complexes.
Embodiment 1: preparation Alq3Organic semiconductor eutectic
1. preparation is through formula Alq3Amorphous membrance
Using quartz glass as substrate, with the method for vacuum evaporation by solid Alq3Solid material heats (225 ± 10 DEG C) liters
China, it is 1000nm through formula Alq that a layer thickness is deposited in substrate3Amorphous film layer, vacuum degree 10-2-10-5Pa.
2. preparing Alq3Organic semiconductor eutectic
Obtained above-mentioned film layer is placed upwards, thereon with the covering of multi-disc clean glass sheet, is placed in teat glass,
Normalizing is sintered 14min under 390 DEG C of air environment.Stop heating, takes out, be cooled to room temperature from furnace, fluorescent microscopy images
Proof is obtaining Alq3Organic semiconductor eutectic.
Embodiment 2: preparation Alq3Organic semiconductor p-n junction
1. preparation is through formula Alq3Amorphous membrance is as described for example 1；
2. preparing Alq3Organic semiconductor pn-junction
Obtained above-mentioned film layer is placed upwards, thereon with the covering of multi-disc clean glass sheet, is placed in teat glass,
Normalizing is sintered 15min under 380 DEG C of air environment.Stop heating, takes out, be cooled to room temperature from furnace, as depicted in figs. 1 and 2,
Fluorescent microscopy images proof is obtaining Alq3Organic semiconductor pn-junction.The light as shown in figure 3, the obtained PN junction of the present invention shines
Spectral peak position is located at 470 nanometers and 500 nanometers.
Embodiment 3: the nanocrystalline application in terms of for organic semiconductor luminescent device of organometallic complex
Device architecture are as follows: [ITO/ Alq3Organic semiconductor eutectic film/LiF/Al].
As shown in figure 4, ito glass successively to be used to detergent, acetone, deionized water, EtOH Sonicate 10min, in clean ring
It is toasted under border with infrared lamp, places into processing chamber and substrate ion is bombarded.Alq is prepared on ito glass surface3(1000nm) is organic
Semiconductor eutectics film (as described in Example 1), then use vacuum evaporation LiF(15nm) and Al(2000nm) as composite cathode.
Embodiment 4: organometallic complex is nanocrystalline to be used for organic field effect tube
Device architecture are as follows: [Si/ polyimide/Alq3Organic semiconductor eutectic film/Au].
As shown in figure 5, in one layer of polyimide (revolving speed 4000r/s) of silicon chip surface spin coating, heated baking, then prepare Alq3
(1000nm) organic semiconductor eutectic film (as described in Example 1) finally plates Au layers with mask method.
Embodiment 5: the nanocrystalline preparation for organic solar batteries of organometallic complex
Device architecture are as follows: [FTO/TiO2/ Alq3Organic semiconductor eutectic film/Ag].
As shown in fig. 6, ito glass successively to be used to detergent, acetone, deionized water, EtOH Sonicate 10min, in clean ring
It is toasted under border with infrared lamp, places into processing chamber and substrate ion is bombarded.The successively vacuum evaporation TiO2(20nm on ITO),
Alq3(250nm), then by Alq3It is prepared into eutectic film, then prepares hole transmission layer and vapor deposition Ag(100nm) film layer.
In conclusion a kind of organometallic complex p-n junction nanometer crystal preparation method of the invention, by simply adulterating
Method forms organic semiconductor eutectics and organic semiconductor pn-junction, obtains different proportion through formula structure and face formula using annealing
Structure doping it is nanocrystalline, what is obtained is nanocrystalline for club shaped structure, and p-type is shown as under different conformations and n-type semiconductor is led
Line characteristic, while nanocrystalline organic semiconductor luminescent device, organic field effect tube, the solar battery etc. of can be used for is led
Domain.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (4)
1. a kind of organometallic complex p-n junction nanometer crystal preparation method, which is characterized in that comprising the following specific steps
Step 1: depositing a layer thickness in substrate with the method for vacuum evaporation is 50-2000nm through formula organometallic complex
Amorphous film layer；
Step 2: obtained above-mentioned film layer being placed upwards, on clean glass sheet cover layer, and places it on glass examination
Guan Zhong, normalizing is sintered 8-24min under 300-400 DEG C of air environment；
Step 3: stopping heating, be cooled to room temperature, control heating condition is different, and the organic metal cooperation of different structure can be obtained
Object is nanocrystalline, wherein the nanocrystalline nanometer rods adulterated including p-type and n-type semiconductor of the organometallic complex,
Step 4: being passed through organic solvent tetrahydrofuran and hydrogen mixed gas in the nanocrystalline sample preparation pipe of organometallic complex
P-n metal complex crystal can be obtained in body 10min.
2. organometallic complex p-n junction nanometer crystal preparation method according to claim 1, which is characterized in that described
Vacuum evaporation uses the vacuum pressure of 10-2-10-5Pa.
3. organometallic complex p-n junction nanometer crystal preparation method according to claim 1, which is characterized in that described
Nanocrystalline organometallic complex is club shaped structure, and diameter is 0.2-1 μm, 2-60 μm of length.
4. organometallic complex p-n junction nanometer crystal preparation method according to claim 3, which is characterized in that pass through institute
The organometallic complex stated is nanocrystalline to form efficent electronic transmission and electronics transfer layer in substrate surface.
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