CN110783472B - LED containing PMOT PPV/ZnO Cu/ZnO Al heterojunction and preparation method thereof - Google Patents
LED containing PMOT PPV/ZnO Cu/ZnO Al heterojunction and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of an LED containing a PMOT/ZnO/Cu/ZnO/Al heterojunction, which is characterized by comprising the steps of growing a ZnO Cu/ZnO Al heterojunction on an ITO substrate, spin-coating a mixed solution of PMOT and PPV on the surface of a ZnO Cu polycrystal layer of the ZnO Cu/ZnO Al heterojunction for heat treatment, and finally plating a Ti electrode on the surface of the ZnO Cu polycrystal layer to obtain the LED; the ZnO/Cu/ZnO/Al heterojunction is grown on the ITO substrate, and comprises the steps of firstly growing a ZnO/Al polycrystal layer on the ITO substrate, then putting the ZnO/Al polycrystal layer into a mixed solution of zinc acetate and copper nitrate, growing a ZnO/Cu polycrystal layer on the surface of the ZnO/Al polycrystal layer, and finally obtaining the ZnO/Cu/ZnO/Al heterojunction on the ITO substrate. The invention realizes 490nm main luminous peak through spectrum modulation based on semiconductor energy band engineering, and can provide more excellent photo-biological effect. The preparation method has simple and safe process and low price of used equipment and raw materials, and is suitable for industrialized large-scale preparation.
Description
Technical Field
The invention belongs to the field of electronic materials and preparation thereof, and particularly relates to an LED containing a PMOT PPV/ZnO Cu/ZnO Al heterojunction and a preparation method thereof.
Background
The LED is a semiconductor light emitting diode, has the characteristics of energy conservation, environmental protection, long service life, small volume and the like, and can be widely applied to the fields of various indications, display, decoration, backlight sources, common illumination, urban night scenes and the like. Semiconductor ZnO nanowires have been successfully assembled into different types of nanodevices such as nanowire field effect transistors, nanowire lasers, nanowire sensors and nanowire LEDs. However, some conventional devices have unstable light emitting performance and high operating voltage. The research on the ultraviolet LED based on the ZnO nano-rod is not very successful, and the electroluminescence is basically in the visible light wave band. The main luminescence peak of the commercial gallium nitride white light LED is positioned at 450nm, and the value of the photobiological effect beneficial to the human body is limited. In addition to producing visible ultraviolet light, it can also affect biological physiological functions, such as interfering with a person's body temperature, blood pressure, heart rate, brain waves or causing drowsiness, irritability, or even depression.
Disclosure of Invention
Aiming at the defects and the defects of the prior preparation technology, the invention provides an LED containing a PMOT PPV/ZnO Cu/ZnO Al heterojunction and a preparation method thereof, and solves the technical problem that the main luminous peak of the commercial gallium nitride white LED at the present stage is located at 450nm, so that the photobiological effect value beneficial to the human body is very limited.
In order to solve the problems, the invention adopts the technical scheme that:
a preparation method of an LED containing a PMOT/ZnO/Cu/ZnO/Al heterojunction comprises the steps of growing a ZnO Cu/ZnO/Al heterojunction on an ITO substrate, spin-coating a mixed solution of the PMOT and the PPV on the surface of a ZnO Cu polycrystal layer of the ZnO Cu/ZnO/Al heterojunction for heat treatment, and finally plating a Ti electrode on the surface of the ZnO Cu polycrystal layer;
the ZnO/Cu/ZnO/Al heterojunction is grown on the ITO substrate, and comprises the steps of firstly growing a ZnO/Al polycrystal layer on the ITO substrate, then putting the ZnO/Al polycrystal layer into a mixed solution of zinc acetate and copper nitrate, growing a ZnO/Cu polycrystal layer on the surface of the ZnO/Al polycrystal layer, and finally obtaining the ZnO/Cu/ZnO/Al heterojunction on the ITO substrate.
Furthermore, the molar ratio of ZnO to Al in the ZnO to Al polycrystal layer is (95-100): 2-5.
Furthermore, the molar ratio of ZnO to Cu in the ZnO to Cu polycrystal layer is (92-98): 4-6.
Furthermore, the mass ratio of PMOT to PPV in the mixed solution of PMOT and PPV is (30-40): 60-64).
Further, the growing of the ZnO: Cu/ZnO: Al heterojunction on the ITO substrate specifically comprises the following steps:
firstly, placing an ITO substrate into a magnetron sputtering vacuum chamber, introducing oxygen and argon by adopting a zinc target and an aluminum target, controlling the temperature of the ITO substrate to 300 ℃, carrying out co-sputtering for 30min under the power of 110W, then placing the ITO substrate into a mixed solution of zinc acetate and copper nitrate, growing a ZnO/Cu polycrystal layer on the surface of the ZnO/Al polycrystal layer, and finally obtaining a ZnO/Cu/Al heterojunction on the ITO substrate, wherein the molar ratio of ZnO to Al in the ZnO/Al polycrystal layer is 97:3, and the molar ratio of ZnO to Cu in the ZnO/Cu polycrystal layer is 95: 5.
Furthermore, the concentration of the zinc acetate is 0.04mol/L, and the concentration of the copper nitrate is 0.005 mol/L.
Further, before the mixed solution of PMOT and PPV is coated on the surface of a ZnO/Cu polycrystalline layer of the ZnO/Al heterojunction in a spinning mode, the method also comprises the step of carrying out plasma treatment on the ZnO/Cu/ZnO/Al heterojunction.
Further, the plasma treatment is to perform plasma treatment on the ZnO: Cu/ZnO: Al heterojunction for 2h by using a plasma generator with the power of 50 watts in an environment of 20pa oxygen and 20pa helium, and then perform plasma treatment on the ZnO: Cu/ZnO: Al heterojunction for 2h by using a plasma generator with the power of 50 watts in an environment of 50pa hydrogen and 20pa helium.
Further, the mixed solution of PMOT and PPV was spin-coated on the surface of a ZnO/Cu polycrystalline layer of a ZnO/Al heterojunction and then dried at 80 ℃ for 30 min.
The LED containing the PMOT PPV/ZnO Cu/ZnO Al heterojunction is prepared by the preparation method of the LED containing the PMOT PPV/ZnO Cu/ZnO Al heterojunction.
Compared with the prior art, the invention has the following beneficial technical effects:
the LED containing the PMOT PPV/ZnO Cu/ZnO Al heterojunction is designed and prepared, and the 490nm main light-emitting peak is realized through spectrum modulation based on semiconductor energy band engineering. Compared with the gallium nitride white light LED (the main luminous peak is located at 450nm) which is commercially used at present, the gallium nitride white light LED can provide photobiological effect which is more beneficial to human bodies.
The method for preparing the enhanced photobiological effect LED containing the PMOT, PPV, ZnO, Cu, ZnO and Al heterojunction is simple and safe in process, low in price of used equipment and raw materials, and suitable for industrial large-scale preparation.
Drawings
FIG. 1 shows the electroluminescence spectra of the examples at a voltage of 5V;
FIG. 2 is a current-voltage characteristic of various embodiments;
the invention is described in detail below with reference to the drawings and the detailed description.
Detailed Description
The optical biological effect means that the spectrum of the illuminating light source can influence the physiological functions of organisms besides generating visual ultraviolet, such as interfering the body temperature, blood pressure, heart rate and brain wave of a human or causing drowsiness, irritability and even depression. Research has proved that the beneficial photo-biological effect for human body is mainly focused on the sensitive peak position of photo-biological effect corresponding to the LED luminous peak near the lambda light wavelength of 490nm, which can improve the work efficiency, the sobriety degree, the attention, the vision and the reaction speed of human body.
According to the invention, the LED containing the PMOT PPV/ZnO Cu/ZnO Al heterojunction is prepared, and the enhanced photo-biological effect LED device is prepared through LED device structure design based on semiconductor energy band engineering, targeted doping and plasma treatment, wherein the light wavelength of a main light-emitting peak is about 490 nm.
The preparation method comprises growing a ZnO Cu/ZnO Al heterojunction on an ITO substrate, spin-coating a mixed solution of PMOT and PPV on the surface of a ZnO Cu polycrystal layer of the ZnO Cu/ZnO Al heterojunction for heat treatment, and finally plating a Ti electrode on the surface of the ZnO Cu polycrystal layer; the ZnO/Cu/ZnO/Al heterojunction is grown on the ITO substrate, and comprises the steps of firstly growing a ZnO/Al polycrystal layer on the ITO substrate, then putting the ZnO/Al polycrystal layer into a mixed solution of zinc acetate and copper nitrate, growing a ZnO/Cu polycrystal layer on the surface of the ZnO/Al polycrystal layer, and finally obtaining the ZnO/Cu/ZnO/Al heterojunction on the ITO substrate. The molar ratio of ZnO to Al in the ZnO/Al polycrystalline layer is (95-100) to (2-5); the molar ratio of ZnO to Cu in the ZnO to Cu polycrystalline layer is (92-98) to (4-6); the mass ratio of PMOT to PPV in the mixed solution of PMOT and PPV is (30-40): 60-64).
The reagents of the present invention, such as ITO glass substrate, PMOT (poly 3 methoxythiophene), PPV (polyphenylacetylene), etc., were purchased from commercial standards, and the laboratory instruments were all commercially available.
The "ZnO — Cu polycrystalline layer" in the present invention means an aggregate of many oriented single crystals formed from ZnO grains doped with Cu; "ZnO: Al polycrystalline layer" means an assembly of a plurality of oriented single crystals formed from Al-doped ZnO grains; PPV denotes a PMOT material doped with PPV; wherein, a homojunction is formed between the ZnO/Cu polycrystal layer and the ZnO/Al polycrystal layer, and a heterojunction is formed between the PMOT/PPV layer and the ZnO/Cu polycrystal layer.
Heterojunction, an interface region formed by two different semiconductors contacting each other. The heterojunction can be divided into homotype heterojunction (P-P junction or N-N junction) and heterotype heterojunction (P-N or P-N) according to the conduction types of the two materials, and the multilayer heterojunction is called as heterostructure. The conditions for forming a heterojunction are typically that the two semiconductors have similar crystal structures, close atomic spacings, and coefficients of thermal expansion. Heterojunctions can be fabricated using techniques such as interfacial alloying, epitaxial growth, vacuum deposition, and the like. The heterojunction has excellent photoelectric characteristics which cannot be achieved by respective PN junctions of two semiconductors, so that the heterojunction is suitable for manufacturing ultrahigh-speed switching devices, solar cells, semiconductor lasers and the like.
The PMOT, PPV, ZnO, Cu, ZnO and Al heterojunction LEDs prepared in the examples were tested by conventional testing instruments, such as an Electroluminescent (EL) tester (off-line), an IV tester (on-line), a single tester, a ZL-4 Electroluminescent (EL) tester, or an IV tester.
In order to make the objects and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and examples and comparative examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Therefore, within the scope of the claims and their equivalents, the invention may be practiced otherwise than as specifically described below.
Example 1:
according to the technical scheme and with the accompanying drawings, the embodiment provides a preparation method of an LED containing a PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction, and the preparation method comprises the following steps:
step 1: putting an ITO substrate into a magnetron sputtering vacuum chamber, introducing 3pa oxygen and 2pa argon by adopting a 99.99 percent zinc target and a 99.9 percent aluminum target, controlling the substrate to be heated to 300 ℃, carrying out co-sputtering for 30min under 110W power, obtaining a ZnO-Al polycrystal layer on the ITO substrate, and taking out a sample. Wherein the molar ratio of ZnO to Al is 97: 3.
Step 2: preparing a mixed solution of zinc acetate and copper nitrate, wherein the concentrations of the zinc acetate and the copper nitrate are 0.04mol/L and 0.005mol/L respectively, then putting the ZnO and Al polycrystal layer into the mixed solution, heating to 95 ℃, taking out and drying after the ZnO and Al polycrystal layer grows for 5 hours, and obtaining a ZnO, Cu, ZnO and Al heterojunction on the ITO substrate. Wherein the molar ratio of ZnO to Cu is 95: 5.
And step 3: PMOT (poly 3 methoxythiophene) with the purity of 99.9 percent is placed into chloroform and heated to 70 ℃ and then stirred for 30 minutes, PPV (polyphenylacetylene) with the purity of 99.9 percent is placed into toluene and heated to 50 ℃ and then stirred for 30 minutes, the PMOT and the PPV are mixed and heated to 50 ℃ and then stirred for reaction for 24 hours, and a PMOT and PPV mixed solution is obtained, wherein the mass ratio of the PMOT to the PPV is 38: 62.
And 4, step 4: the ZnO: Cu/ZnO: Al heterojunction was plasma treated with a 50 watt plasma generator for 2h in a 20pa oxygen and 20pa helium environment, and then plasma treated with a 50 watt plasma generator for 2h in a 50pa hydrogen and 20pa helium environment.
And 5: the PMOT and PPV mixed solution is uniformly coated on the surface of a ZnO/Cu polycrystalline layer of a ZnO/Al heterojunction in a spinning mode at the rotating speed of 2000rpm, and then the surface is dried for 30min at the temperature of 80 ℃, and the process is repeated for 8 times. Then put into a vacuum tube furnace at 10- 4pa at 120 ℃ for 3 h. And finally, plating a Ti electrode on the surface of the ZnO-Cu polycrystalline layer by magnetron sputtering to finish the manufacture of the enhanced photo-biological effect LED containing the PMOT-PPV/ZnO-Cu/ZnO-Al heterojunction. The detection result is shown in FIG. 1, and the main luminescence peak appears near 490nm, which shows that the photobiological effect beneficial to human body can be generated.
Example 2 (comparative):
the preparation method is the same as that of example 1, but step 2 is omitted, and the prepared device is a PMOT: PPV/ZnO: Al heterojunction. As can be seen from FIG. 1, the shift of the main emission peak from around 490nm to around 450nm indicates that it cannot have the photo-biological enhancement effect as in example 1 and the emission intensity is significantly weaker than that in example 1. As can be seen from fig. 2, the forward current is smaller, the reverse current is larger, the rectification ratio is lower, the rectification effect of the current-voltage characteristic is not as good as that of embodiment 1, and the electric injection efficiency is not as good as that of embodiment 1, because the band structure of the device of embodiment 2 is not as reasonable as that of embodiment 1.
Example 3 (comparative):
the preparation and testing were the same as in example 1, but step 4 was omitted. As can be seen from FIG. 1, the main peak of photo-biological effect at 490nm is significantly weaker than that of example 1, and the overall luminous intensity is also significantly weaker than that of example 1. As can be seen from FIG. 2, the forward current is smaller, the reverse current is larger, the rectification ratio is lower, the rectification effect of the current-voltage characteristic is not as good as that of example 1, and the electric injection efficiency is not as good as that of example 1 because the surface impurities of the LED of example 3 without plasma treatment of PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction are more than those of the LED of example 1 with plasma treatment of PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that the present invention can be practiced without departing from the spirit and scope of the appended claims.
Claims (10)
1. A preparation method of an LED containing a PMOT, PPV, ZnO, Cu, ZnO and Al heterojunction is characterized by comprising the steps of growing a ZnO, Cu/ZnO, Al homojunction on an ITO substrate, spin-coating a mixed solution of PMOT and PPV on the surface of a ZnO, Cu and Cu polycrystal layer of the ZnO, Cu/ZnO and Al homojunction, carrying out heat treatment, and finally plating a Ti electrode on the surface of the ZnO, Cu and polycrystal layer with a PMOT, PPV film layer to obtain the LED;
the ZnO/Cu/ZnO/Al homojunction is grown on the ITO substrate, and the ZnO/Al/Cu homojunction is finally obtained on the ITO substrate.
2. The method of claim 1, wherein the molar ratio of ZnO to Al in the ZnO to Al polycrystalline layer is (95-100): 2-5.
3. The method for preparing an LED containing a PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction as claimed in claim 1, wherein the molar ratio of ZnO to Cu in the ZnO: Cu polycrystalline layer is (92-98): 4-6).
4. The method for preparing the LED containing the PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction as claimed in claim 1, wherein the mass ratio of PMOT to PPV in the mixed solution of PMOT and PPV is (30-40): 60-64).
5. The method for preparing the LED containing the PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction as claimed in claim 1, wherein the growing of the ZnO: Cu/ZnO: Al homojunction on the ITO substrate specifically comprises:
firstly, placing an ITO substrate into a magnetron sputtering vacuum chamber, introducing oxygen and argon by adopting a zinc target and an aluminum target, controlling the temperature of the ITO substrate to 300 ℃, carrying out co-sputtering for 30min under the power of 110W, then placing the ITO substrate into a mixed solution of zinc acetate and copper nitrate, growing a ZnO/Cu polycrystal layer on the surface of the ZnO/Al polycrystal layer, and finally obtaining a ZnO/Cu/ZnO/Al homojunction on the ITO substrate, wherein the molar ratio of ZnO to Al in the ZnO/Al polycrystal layer is 97:3, and the molar ratio of ZnO to Cu in the ZnO/Cu polycrystal layer is 95: 5.
6. The method of claim 1, wherein the concentration of zinc acetate is 0.04mol/L and the concentration of copper nitrate is 0.005 mol/L.
7. The method for preparing the LED containing the PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction as claimed in claim 1, wherein the step of performing plasma treatment on the ZnO: Cu/ZnO: Al homojunction before spin-coating the mixed solution of PMOT and PPV on the surface of the ZnO: Cu/ZnO: Al homojunction ZnO: Cu polycrystal layer is further included.
8. The method for preparing the LED containing the PMOT PPV/ZnO Cu/ZnO Al heterojunction as claimed in claim 7, wherein the plasma treatment comprises the steps of firstly carrying out plasma treatment on the ZnO Cu/ZnO Al homojunction for 2 hours in an oxygen gas environment of 20pa and a helium gas environment of 20pa by using a plasma generator with the power of 50 watts, and then carrying out plasma treatment on the ZnO Cu/ZnO Al homojunction for 2 hours in a hydrogen gas environment of 50pa and a helium gas environment of 20pa by using a plasma generator with the power of 50 watts.
9. The method for preparing the LED containing the PMOT: PPV/ZnO: Cu/ZnO: Al heterojunction as claimed in claim 7, wherein the mixed solution of PMOT and PPV is spin-coated on the surface of a ZnO: Cu/ZnO: Al homojunction ZnO: Cu polycrystal layer and then dried for 30min at 80 ℃.
10. An LED containing a PMOT PPV/ZnO Cu/ZnO Al heterojunction is characterized in that the LED containing the PMOT PPV/ZnO Cu/ZnO Al heterojunction is prepared by the method for preparing the LED containing the PMOT PPV/ZnO Cu/ZnO Al heterojunction according to any one of claims 1-9.
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| US20160223269A1 (en) * | 2015-02-04 | 2016-08-04 | Outlast Technologies, LLC | Thermal management films containing phase change materials |
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Patent Citations (4)
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| TW392369B (en) * | 1998-03-11 | 2000-06-01 | Nat Science Council | Manufacturing method for high polymer light emitting diode capable of emitting nearly white light broadband spectrum |
| CN1933205A (en) * | 2005-08-12 | 2007-03-21 | 三星电子株式会社 | Single-crystal nitride-based semiconductor substrate and method of manufacturing high-quality nitride-based light emitting device by using the same |
| KR101170919B1 (en) * | 2011-06-30 | 2012-08-03 | 성균관대학교산학협력단 | Solar cell with enhanced energy efficiency by surface plasmon resonance effect |
| CN108841097A (en) * | 2013-02-15 | 2018-11-20 | 信越聚合物株式会社 | Electroconductive polymer dispersion liquid and conductive film |
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