CN111952462A - Ultraviolet and visible light detector based on covalent organic framework material and preparation method thereof - Google Patents
Ultraviolet and visible light detector based on covalent organic framework material and preparation method thereof Download PDFInfo
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- H10K30/60—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation in which radiation controls flow of current through the devices, e.g. photoresistors
- H10K30/65—Light-sensitive field-effect devices, e.g. phototransistors
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- H—ELECTRICITY
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Abstract
The invention belongs to the technical field of photoelectric detectors, and particularly relates to an ultraviolet and visible light detector based on a covalent organic framework material and a preparation method thereof. The method comprises the following steps: firstly, preparing a transistor device with a semiconductor channel exposed outside; then, depositing a layer of photosensitive covalent organic framework material on the semiconductor channel; and finally, placing the device in a liquid environment to obtain the high-performance ultraviolet and visible light detector. The invention takes a photosensitive covalent organic framework material as a light energy absorption material, can accumulate a large amount of charges by a liquid-solid interface under the assistance of liquid, and changes the doping state and the conductivity of a semiconductor channel, thereby converting a light signal into an electric signal. The invention has simple process, can realize the detection of ultraviolet and visible light (254 nm-760 nm), has high responsivity, short response time and good stability, and has wide application prospect in the fields of information, communication, artificial intelligence and the like.
Description
Technical Field
The invention belongs to the technical field of photoelectric detectors, and particularly relates to a liquid-solid interface enhanced ultraviolet and visible light detector based on a covalent organic framework material and a preparation method thereof.
Background
The photoelectric signal conversion technology is one of the hot spots of modern information technology, and has important applications in optical communication, optical detection, video imaging and night detection. The photoelectric detectors are also mature with the development of modern technologies, and the common photoelectric detectors mainly have several photoelectric conversion principles such as photovoltaic, photothermal, photoconduction, gratings and the like. Among these principles, the grating type photodetector receives a great deal of attention due to its high responsivity. However, due to the limitation of the working principle of the grating type photodetector, it is difficult to simultaneously realize high responsivity and high response speed, which limits the practical application thereof.
Covalent organic framework materials are a class of porous crystalline organic materials with high conjugation and designability. The covalent organic framework material with the structure design can contain a large number of photosensitive groups to efficiently absorb light energy, and the extremely high specific surface area of the covalent organic framework material is also beneficial to realizing the accumulation of a large number of charges on a liquid-solid interface under the assistance of liquid, so that the extremely high photoelectric responsivity is achieved. Meanwhile, the movement of particles in the liquid and the conjugated planar structure of the covalent organic framework material are also beneficial to the rapid charge and discharge of accumulated charges, and the rapid conversion of photoelectric signals is realized. Therefore, the covalent organic framework material under the liquid-solid interface enhancement effect is used as the photosensitive layer of the grating type photoelectric detector, so that high responsivity and high response speed can be effectively realized, and the application value of the photoelectric detector in actual production and life is expected to be further improved.
Disclosure of Invention
The invention aims to provide an ultraviolet and visible light detector based on a covalent organic framework material and having high responsivity, high response speed and wide detection wave band and a preparation method thereof.
The invention combines the covalent organic frame material and the transistor device, fully utilizes the advantages of higher photosensitivity and large specific surface area of the covalent organic frame material and the charge capturing capability of a liquid-solid interface to construct a grating layer with large surface and high charge capacity, and realizes high and fast photoelectric detection on the broadband of 254 nm-650 nm.
The invention provides a preparation method of an ultraviolet and visible light detector based on a covalent organic framework material, which comprises the following specific steps:
(1) preparing a transistor device with a semiconductor channel exposed outside; comprises an insulating substrate, a patterned electrode, and a semiconductor channel;
(2) depositing a photosensitive covalent organic framework material on a semiconductor channel of the transistor device obtained in the step (1) to obtain the transistor device with the surface of the semiconductor channel uniformly distributed with the covalent organic framework material;
(3) putting the device obtained in the step (2) into liquid to work, and measuring current change under the illumination condition; and obtaining the corresponding illumination intensity by calibrating the corresponding relation between the current change and the illumination intensity.
In the present invention, the insulating substrate of the transistor device is selected from the group consisting of silicon dioxide, glass, mica, silicon wafers with dielectric layers, and insulating polymers (e.g., polyethylene terephthalate, polyimide, polydimethylsiloxane).
In the invention, the preparation method of the patterned electrode is thermal evaporation, magnetron sputtering or screen printing, and the electrode material is selected from metals (such as gold, silver, copper, titanium, aluminum and chromium), conductive silicides, conductive polymers or conductive carbon materials.
In the present invention, the semiconductor channel material of the transistor device is selected from an elemental semiconductor, a compound semiconductor or a doped semiconductor, such as silicon, germanium, graphene, carbon nanotube, zinc oxide, indium oxide, and a transition metal chalcogenide.
In the present invention, the covalent organic framework material is selected from the group consisting of a boronic acid-based covalent organic framework material, an imine-based covalent organic framework material, and a triazine-based covalent organic framework material. The photosensitive covalent organic framework material needs to be subjected to structural design, and a structural unit contains a photosensitive functional group with the absorption wavelength of 254 nm-760 nm, and the photosensitive functional group comprises a conjugated condensed ring or a heterocyclic group, such as porphyrin, phthalocyanine, pyrene, triazine, anthracene and the like.
In the invention, the deposition method of the covalent organic framework material is a solvothermal method, an ionothermal method, a microwave-assisted method or a supercritical solvothermal method.
In the present invention, the covalent organic framework material is deposited to a thickness of 10 nm to 10 μm.
In the invention, the liquid comprises one or more of N-pentane, petroleum ether, hexane, cyclohexane, isooctane, trifluoroacetic acid, heptane, carbon tetrachloride, benzene, toluene, xylene, trimethylbenzene, chlorobenzene, dichlorobenzene, diethyl ether, isobutanol, N-butanol, propanol, ethanol, methanol, dichloromethane, chloroform, ethyl acetate, tetrahydrofuran, dioxane, acetone, pyridine, acetonitrile, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide, acetic acid, formic acid and water which are mixed in any proportion.
The method for detecting the illumination intensity comprises the steps of connecting the device to a circuit with an external voltage, placing the device in an illumination environment, measuring the change of current between electrodes, and calculating the corresponding illumination intensity by utilizing the corresponding relation between the calibrated current change and the illumination intensity.
In the invention, the wavelength range of the illumination condition is 254 nm-760 nm, and the illumination intensity is 0.1 microwatt per square centimeter-10 watts per square centimeter.
Compared with the traditional photoelectric detector, the invention has the advantages that: the high-photosensitivity covalent organic framework material is used as a light signal receiving layer, a semiconductor with adjustable and controllable conductivity is used as a signal transduction medium to construct a transistor device structure, and meanwhile, the liquid-solid interface in a liquid environment is utilized to enhance the charge capturing capability, so that the responsivity and the response speed of the photoelectric detector are greatly improved, and the broadband photoelectric detection of 254 nm-650 nm is realized. The transistor photoelectric detector has the advantages of high responsivity, high response speed, easiness in miniaturization, wide detection wave band and the like, and the photoelectric detector prepared by the invention has wide application prospect in the fields of information and communication.
Drawings
FIG. 1 is a schematic diagram of a photodetector device of the present invention.
FIG. 2 is a scanning electron micrograph of the surface of a semiconductor channel having a covalent organic framework material uniformly distributed therein according to example 1.
Fig. 3 is a schematic structural view of a photodetector device in embodiment 1.
Fig. 4 is a photoelectric response curve obtained in example 1.
FIG. 5 is a graph showing the change of the light responsivity with the light intensity obtained in example 1.
Detailed Description
The present invention will be further described with reference to the following embodiments and the accompanying drawings, and a schematic structural diagram of a photodetector device according to the present invention is shown in fig. 1. The following embodiments are merely illustrative of the present invention and do not limit the scope of the present invention.
Example 1
Firstly, single-layer graphene is grown on a copper foil with the thickness of 25 microns by using a chemical vapor deposition method, and the graphene is transferred to SiO (silicon dioxide) which is prepared with patterned Cr/Au (5/40 nanometers) source and drain electrodes by a thermal evaporation technology in advance by using an electrochemical stripping method2And obtaining the graphene field effect device on the Si substrate. Then, a layer of photosensitive covalent organic framework material grows in situ on the surface of the graphene film, the covalent organic framework material is prepared by reacting 0.12 mol/L of terephthalaldehyde and 0.06 mol/L of 1,3,6, 8-tetra- (p-aminophenyl) -pyrene in a n-butyl alcohol solvent under the catalysis of 0.1 ml of acetic acid at 80 ℃ for 12 hours by adopting a supercritical carbon dioxide auxiliary method, a high-crystallinity columnar covalent organic framework material with uniform growth is obtained, the columnar covalent organic framework material is respectively washed clean by acetone, ethanol and distilled water, and then is dried by blowing under high-purity nitrogen, and the appearance of the surface of the material is shown in figure 2. Connecting the obtained device to a circuit with an external voltage of 50 millivolts, placing the device in pure water to work, measuring current change under illumination conditions, and calibrating corresponding illumination power to obtain the high-performance ultraviolet and visible light broadband photoelectric detector, wherein the structural schematic diagram of the device is shown in FIG. 3, and the device is blue-violet with a wavelength of 405 nanometersThe photoelectric response curve under light irradiation is shown in fig. 4, and the light response current curve with the light intensity is shown in fig. 5.
Example 2
Firstly, single-layer graphene is grown on a copper foil with the thickness of 25 microns by using a chemical vapor deposition method, and the graphene is transferred to SiO (silicon dioxide) which is prepared with patterned Cr/Au (5/40 nanometers) source and drain electrodes by a thermal evaporation technology in advance by using an electrochemical stripping method2And obtaining the graphene field effect device on the Si substrate. Then, a layer of photosensitive covalent organic framework material grows on the surface of the graphene film in situ, the covalent organic framework material is prepared by reacting 0.24 mol/L of terephthalaldehyde and 0.12 mol/L of 1,3,6, 8-tetra- (p-aminophenyl) -pyrene in a n-butyl alcohol solvent at 0.1 ml of acetic acid at 80 ℃ for 12 hours by adopting a supercritical carbon dioxide auxiliary method for synthesis, the uniformly-grown high-crystallinity columnar covalent organic framework material is obtained, and is respectively washed clean by acetone, ethanol and distilled water, and then is dried under high-purity nitrogen. The obtained device is connected to a circuit with an external voltage of 50 millivolts, is placed in pure water to work, measures the current change under the illumination condition, and calibrates the corresponding illumination power, so that the high-performance ultraviolet and visible light broadband photoelectric detector can be obtained.
Example 3
Firstly, single-layer graphene is grown on a copper foil with the thickness of 25 microns by using a chemical vapor deposition method, and the graphene is transferred to SiO (silicon dioxide) which is prepared with patterned Cr/Au (5/40 nanometers) source and drain electrodes by a thermal evaporation technology in advance by using an electrochemical stripping method2And obtaining the graphene field effect device on the Si substrate. Then, a layer of photosensitive covalent organic framework material grows on the surface of the graphene film in situ, the covalent organic framework material is prepared by reacting 0.24 mol/L of terephthalaldehyde and 0.12 mol/L of 1,3,6, 8-tetra- (p-aminophenyl) -pyrene in a n-butyl alcohol solvent under the catalysis of 0.1 ml of acetic acid at 100 ℃ for 24 hours by adopting a supercritical carbon dioxide auxiliary method, the uniformly-grown high-crystallinity columnar covalent organic framework material is obtained, and is respectively washed clean by acetone, ethanol and distilled water, and then is dried under high-purity nitrogen. The resulting device is switched to an applied voltage of 50 mVAnd the circuit is arranged in pure water to work, measures the current change under the illumination condition, calibrates and calculates the corresponding illumination power, and then the high-performance ultraviolet and visible light broadband photoelectric detector can be obtained.
The ultraviolet and visible light broadband photodetectors prepared in examples 2 and 3 have the same morphology and performance as the ultraviolet and visible light broadband photodetector prepared in example 1.
The foregoing is merely an example of the present invention and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for preparing ultraviolet and visible light detectors based on covalent organic framework materials comprises the following specific steps:
(1) preparing a transistor device with a semiconductor channel exposed outside; comprises an insulating substrate, a patterned electrode, and a semiconductor channel;
(2) depositing a photosensitive covalent organic framework material on a semiconductor channel of the transistor device obtained in the step (1) to obtain the transistor device with the surface of the semiconductor channel uniformly distributed with the covalent organic framework material;
(3) putting the device obtained in the step (2) into liquid to work, and measuring current change under the illumination condition; and obtaining the corresponding illumination intensity by calibrating the corresponding relation between the current change and the illumination intensity.
2. The method according to claim 1, wherein the patterned electrode is prepared by thermal evaporation, magnetron sputtering or screen printing, and the electrode material is selected from metal, conductive silicide, conductive polymer, and conductive carbon material; the insulating substrate is selected from silicon dioxide, glass, mica, a silicon wafer with a dielectric layer and an insulating polymer, and the insulating polymer is polyethylene terephthalate, polyimide or polydimethylsiloxane; the semiconductor channel material is selected from an elemental semiconductor, a compound semiconductor or a doped semiconductor.
3. The method of claim 1, wherein the covalent organic framework material is selected from boronic acid-based covalent organic framework materials, imine-based covalent organic framework materials, triazine-based covalent organic framework materials; the covalent organic framework materials are structurally designed, and the structural units contain photosensitive functional groups with absorption wavelengths of 254 nm-760 nm, wherein the photosensitive functional groups are conjugated condensed rings or heterocyclic groups.
4. The method of claim 3, wherein the photoactive functional group is selected from the group consisting of porphyrins, phthalocyanines, pyrenes, triazines, anthracenes.
5. The method of claim 3, wherein the covalent organic framework material is deposited by a solvothermal method, an ionothermal method, a microwave-assisted method, or a supercritical solvothermal method.
6. The method of claim 3, wherein the covalent organic framework material is deposited to a thickness of 10 nm to 10 μm.
7. The method according to claim 1, wherein the liquid is selected from one or more of N-pentane, petroleum ether, hexane, cyclohexane, isooctane, trifluoroacetic acid, heptane, carbon tetrachloride, benzene, toluene, xylene, trimethylbenzene, chlorobenzene, dichlorobenzene, diethyl ether, isobutanol, N-butanol, propanol, ethanol, methanol, dichloromethane, chloroform, ethyl acetate, tetrahydrofuran, dioxane, acetone, pyridine, acetonitrile, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide, acetic acid, formic acid, and water.
8. The method according to claim 1, wherein the light irradiation conditions in the step (3) have a wavelength ranging from 254 nm to 760 nm and an irradiation intensity of 0.1 microwatts per square centimeter to 10 watts per square centimeter.
9. Ultraviolet and visible light detectors based on covalent organic framework materials obtained by the preparation process according to one of claims 1 to 8.
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