CN113395011B - Array interweaving type friction nano generator and preparation method thereof - Google Patents

Array interweaving type friction nano generator and preparation method thereof Download PDF

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CN113395011B
CN113395011B CN202110016906.2A CN202110016906A CN113395011B CN 113395011 B CN113395011 B CN 113395011B CN 202110016906 A CN202110016906 A CN 202110016906A CN 113395011 B CN113395011 B CN 113395011B
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吴璠
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Huzhou University
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Abstract

The invention discloses an array interweaving type friction nanometerThe invention relates to a generator and a preparation method thereof, in particular to a nano friction generating set formed by directly mutually superposing a p-type semiconductor CuO nano array and an n-type semiconductor ZnO nano array and a preparation method thereof. When the CuO nano array and the plane ZnO film are used to form the nano friction power generation device, the current density of the deviceJ sc Is 0.23 uA/cm2(ii) a When the nano friction power generation device is formed by the plane CuO film and the ZnO nano array, the current density of the deviceJ sc Is 0.48 uA/cm2(ii) a Compared with the two devices, the current density of the nano friction power generation device formed by the CuO nano array and the ZnO nano arrayJ sc Up to 8 uA/cm2. Therefore, the p-type semiconductor CuO nano array and the n-type semiconductor ZnO nano array are directly overlapped with each other, so that the interface area of the CuO and the ZnO is greatly increased, the friction between the CuO and the ZnO is more sufficient, and the concentration of generated electron holes is richer.

Description

Array interweaving type friction nano generator and preparation method thereof
Technical Field
The invention relates to the field of nano semiconductor materials and new energy, in particular to novel power generation equipment and a preparation method thereof.
Background
Energy and environmental problems are two most urgent problems to be solved in the current human face, and low-carbon economy is the hottest topic at present. Since the first zinc oxide piezoelectric nano-generator was proposed in 2006, nano-generators that convert mechanical energy into electrical energy with minimum energy were produced worldwide [ Science, 312, 5771, 2006 ]. When the object and the object rub against each other, one side is negatively charged and the other side is positively charged, and the friction electrification is caused by the friction between different materials. Triboelectrification is one of the most common phenomena in nature, and is a contact-induced charging effect, but is neglected because of difficult collection and utilization. If can with the triboelectricity application in the self-generating equipment, will certainly bring more facilities for people's life. The friction nano-generator has application prospects in various fields such as wearable electronic devices, internet of things, environment, infrastructure, medical treatment and the like as a brand-new energy technology [ Materials Letters 280, 128568, 2020 ].
At present, a pyramid structure, a micropore-nanoparticle composite structure and the like are prepared on a friction concave-convex surface of a friction nano generator by means of photoetching and other methods, the preparation process is complex, the cost is high, and the contact surface is limited [ Advanced Function Materials, 29, 1901638, 2019 ]. In addition, the friction interfaces are solid-solid interfaces and are easy to wear.
Disclosure of Invention
The technical problem to be solved by the invention is to overcomeThe friction nanometer power generation device is formed by directly mutually overlapping a p-type semiconductor CuO nanometer array and an n-type semiconductor ZnO nanometer array, and has the advantages of simple preparation method and strong process repeatability. In the device, nanorods in a p-type semiconductor CuO nano array and nanorods in an n-type semiconductor ZnO nano array are fully interwoven, a friction interface is greatly enhanced, and I injected into the interwoven arrays-/I3 -On one hand, the electrolyte lubricates the interface friction and slows down the interface loss; on the other hand, the self-powered organic electroluminescent device is beneficial to the separation of electron holes, the obtained electron holes are separated under the action of an electric field built in a micro-region of a p-n junction, the holes are collected by the p-type semiconductor CuO nano-rods, and the electrons are collected by the n-type semiconductor ZnO nano-rods, so that self-power supply is completed.
In order to achieve the purpose, the invention adopts the following technical scheme:
an array interweaving friction nano-generator comprises a glass substrate, an FTO layer, a CuO nanorod array, a ZnO nanorod array and an I-/I3 -An electrolyte; the FTO layer is plated on the glass substrate to serve as an electrode, the CuO nanorod array vertically grows on the FTO layer, the CuO nanorod array is a hole collecting part, the ZnO nanorod array vertically grows on the FTO layer, the ZnO nanorod array is an electron collecting part, and meanwhile, the CuO nanorod array and the ZnO nanorod serve as friction electrification parts.
The thickness of the FTO layer is 50-200 nm.
The length of the CuO nanorod array is 300-600 nm, the diameter of the CuO nanorod array is 30-90 nm, and the number density of the CuO nanorods is 3-6' 102Number of ormm2The length of the ZnO nanorod array is 300-600 nm, the diameter of the ZnO nanorod array is 20-50 nm, and the number density of the ZnO nanorods is 3-6' 102Is/aremm2。
The preparation method of the array interweaving type friction nano generator comprises the following steps:
(1) obtaining clean FTO conductive glass for later use;
(2) growing a CuO nano array and a ZnO nano array on FTO conductive glass by using a hydrothermal reaction method;
(3) the FTO conductive glass base for growing the CuO nano array and the FTO conductive glass base for growing the ZnO nano array are oppositely superposed;
(4) by capillary action-/I3 -The electrolyte penetrates into the interlaced CuO and ZnO nano array.
The process of growing the CuO nano array on the FTO conductive glass by using the hydrothermal reaction method in the step (2) comprises the following steps:
(1) dissolving copper acetate in absolute ethyl alcohol, and stirring the obtained mixture at room temperature to obtain a blue clear solution;
(2) spin-coating the blue clear solution obtained in the step (1) on the treated FTO conductive glass, and then placing the FTO conductive glass on a heating table to obtain a uniform copper acetate film;
(3) calcining the copper acetate film obtained in the step (2) in a muffle furnace to obtain a CuO compact seed crystal layer film covering the FTO conductive substrate;
(4) and (4) placing the CuO compact seed crystal layer film on the FTO conductive substrate in the step (3) into an aqueous solution consisting of copper nitrate and hexamethylenetetramine, sealing, and reacting in an oven to obtain the CuO nanorod array.
The process of growing the ZnO nano array on the FTO conductive glass by using the hydrothermal reaction method in the step (2) comprises the following steps:
(1) dissolving zinc acetate in water, stirring to dissolve, adding anhydrous ethanol and glacial acetic acid, and stirring at room temperature to obtain colorless clear transparent solution;
(2) spin-coating the colorless clear solution obtained in the step (1) on the treated FTO conductive glass, and then placing the FTO conductive glass on a heating table for annealing to obtain a uniform zinc acetate film;
(3) calcining the zinc acetate film obtained in the step (2) in a muffle furnace to obtain a ZnO dense seed crystal layer film covering the FTO conductive substrate;
(4) and (4) placing the ZnO dense seed crystal layer film on the FTO conductive substrate in the step (3) into an aqueous solution consisting of copper nitrate and hexamethylenetetramine, sealing, and reacting in an oven to obtain the ZuO nanorod array.
The specific steps of the step (4) are as follows: will I2LiI, 4-tert-butylpyridine and tetrabutylammonium iodide are dissolved in acetonitrile to prepare I-/I3 -An electrolyte; by capillary action-/I3 -And the electrolyte permeates into the interlaced CuO and ZnO nano array to complete the nano friction power generation device.
The beneficial effects of the invention are as follows:
(1) the invention directly and mutually superposes the p-type semiconductor CuO nano array and the n-type semiconductor ZnO nano array to complete the nano friction power generation device, has low requirement on equipment, is suitable for large-scale application, and has great application value in the fields of energy devices and the like.
(2) According to the invention, the p-type semiconductor CuO nano array and the n-type semiconductor ZnO nano array are directly overlapped with each other, so that the interface area of CuO and ZnO is greatly increased, the friction between CuO and ZnO is more sufficient, and the concentration of generated electron holes is richer. When the CuO nano array and the planar ZnO film are used for forming the nano friction power generation device, the current density Jsc of the device is 0.23 uA/cm2(ii) a When the nano friction power generation device is formed by the plane CuO film and the ZnO nano array, the current density Jsc of the device is 0.48 uA/cm2(ii) a Compared with the two devices, when the CuO nano array and the ZnO nano array are used for forming the nano friction power generation device, the current density Jsc of the nano friction power generation device is up to 8 uA/cm2。
(3) The innovation points of the invention are as follows:
(a) the CuO/ZnO nano friction power generation device is prepared for the first time; (b) the CuO nano array and the ZnO nano array are applied to a nano friction power generation device for the first time; (c) the performance of the nano friction power generation device formed by the CuO nano array and the ZnO nano array is greatly enhanced compared with that of a planar film device.
Drawings
FIG. 1 is a schematic structural diagram of an array interweaving type friction nano-generator according to the present invention;
the numerical designations in the drawings illustrate the following: (1) FTO conductive glass as anode, (2) CuO nanorod array, (3) ZnO nanorod array, and (4) I-/I3 -Electrolyte and cathode made of (5) FTO conductive glass
FIG. 2 is SEM characterization results of CuO nanorod arrays of example 1 of the present invention;
FIG. 3 is the SEM characterization result of ZuO nanorod array of example 1 of the present invention;
fig. 4 is a result of current-time performance characterization of the friction nanogenerators of examples 1 to 2 of the invention and comparative examples 1 to 2.
Detailed Description
Comparative example 1: CuO nano array/ZnO nano film power generation device
(1-1) ultrasonically cleaning the FTO conductive glass by acetone, isopropanol and ultrapure water, drying, and then treating for 30 minutes by ultraviolet ozone to obtain clean FTO conductive glass for later use;
(1-2) dissolving 0.10 g of copper acetate in 5 ml of absolute ethanol, and stirring the resulting mixture at room temperature for 2 hours to obtain a blue clear solution;
(1-3) spin-coating the blue clear solution obtained in the step (1-2) on the treated FTO conductive glass at the rotating speed of 2000 rpm/min, then placing the FTO conductive glass on a heating table, and annealing the FTO conductive glass at the temperature of 100 ℃ for 1 minute, wherein the process is repeated for four times to obtain a uniform copper acetate film;
(1-4) calcining the copper acetate film obtained in the step (1-3) in a muffle furnace at 250 ℃ for 60 minutes to obtain a CuO dense seed crystal layer film covering the FTO conductive substrate,
(1-5) placing the CuO compact seed crystal layer film on the FTO conductive substrate in the step (1-4) into an aqueous solution consisting of 0.25 mol/L copper nitrate and 0.25 mol/L hexamethylenetetramine, sealing, and reacting in a 90 ℃ oven for 2 hours to obtain a CuO nanorod array;
(1-6) dissolving 0.327 g of zinc acetate in 2 g of water, stirring to dissolve, adding 8 ml of absolute ethanol and 200 microliters of glacial acetic acid, and stirring at room temperature to obtain a colorless clear transparent solution;
(1-7) spin-coating the colorless clear solution obtained in the step (1-6) on the treated FTO conductive glass at the rotating speed of 2000 rpm/min, then placing the FTO conductive glass on a heating table, and annealing the FTO conductive glass at the temperature of 100 ℃ for 1 minute, wherein the process is repeated for four times to obtain a uniform zinc acetate film;
and (1-8) calcining the zinc acetate film obtained in the step (1-7) in a muffle furnace at 350 ℃ for 30 minutes to obtain a ZnO dense layer film covering the FTO conductive substrate.
(1-9) 50 mmol of I20.5 mol of LiI, 0.5 mol of 4-tert-butylpyridine and 0.6 mol of tetrabutylammonium iodide were dissolved in 1L of acetonitrile to prepare I-/I3 -And (3) an electrolyte.
(1-10) oppositely superposing the CuO nano array obtained in the step (1-5) and the ZnO dense layer film obtained in the step (1-8) and infiltrating I by utilizing capillary action-/I3 -And (4) electrolyte to complete the nano friction power generation device.
Comparative example 2: ZnO nano array/CuO nano film power generation device
(2-1) ultrasonically cleaning the FTO conductive glass by acetone, isopropanol and ultrapure water, drying, and then treating for 30 minutes by ultraviolet ozone to obtain clean FTO conductive glass for later use;
(2-2) 0.10 g of copper acetate was dissolved in 5 ml of anhydrous ethanol, and the resulting mixture was stirred at room temperature for 2 hours to obtain a blue clear solution.
(2-3) spin-coating the blue clear solution obtained in the step (2-2) on the treated FTO conductive glass at the rotating speed of 2000 rpm/min, then placing the FTO conductive glass on a heating table, and annealing the FTO conductive glass at the temperature of 100 ℃ for 1 minute, wherein the process is repeated for four times to obtain a uniform copper acetate film;
(2-4) calcining the copper acetate film obtained in the step (2-3) in a muffle furnace at 250 ℃ for 60 minutes to obtain a CuO dense layer film covering the FTO conductive substrate,
(2-5) dissolving 0.327 g of zinc acetate in 2 g of water, stirring to dissolve, adding 8 ml of absolute ethanol and 200 microliters of glacial acetic acid, and stirring at room temperature to obtain a colorless clear transparent solution;
(2-6) spin-coating the colorless clear solution obtained in the step (2-6) on the treated FTO conductive glass at the rotating speed of 2000 rpm/min, then placing the FTO conductive glass on a heating table, and annealing the FTO conductive glass at the temperature of 100 ℃ for 1 minute, wherein the process is repeated for four times to obtain a uniform zinc acetate film;
and (2-7) calcining the zinc acetate film obtained in the step (2-7) in a muffle furnace at 350 ℃ for 30 minutes to obtain a ZnO dense layer film covering the FTO conductive substrate.
(2-8) placing the ZnO dense seed crystal layer film on the FTO conductive substrate in the step (2-4) in an aqueous solution consisting of 0.25 mol/L zinc nitrate and 0.25 mol/L hexamethylenetetramine, sealing, and reacting in an oven at 90 ℃ for 2 hours to obtain a ZnO nanorod array;
(2-9) 50 mmol of I20.5 mol of LiI, 0.5 mol of 4-tert-butylpyridine and 0.6 mol of tetrabutylammonium iodide were dissolved in 1L of acetonitrile to prepare I-/I3 -And (3) an electrolyte.
(2-10) oppositely superposing the ZnO nano array obtained in the step (2-8) and the CuO dense layer film obtained in the step (2-4) and infiltrating I by utilizing capillary action-/I3 -And (4) electrolyte to complete the nano friction power generation device.
Example 1: a CuO nano array/ZnO nano array power generation device.
(3-1) ultrasonically cleaning the FTO conductive glass by acetone, isopropanol and ultrapure water, drying, and then treating for 30 minutes by ultraviolet ozone to obtain clean FTO conductive glass for later use;
(3-2) dissolving 0.10 g of copper acetate in 5 ml of absolute ethanol, and stirring the resulting mixture at room temperature for 2 hours to obtain a blue clear solution;
(3-3) spin-coating the blue clear solution obtained in the step (3-2) on the treated FTO conductive glass at the rotating speed of 2000 rpm/min, then placing the FTO conductive glass on a heating table, and annealing the FTO conductive glass at the temperature of 100 ℃ for 1 minute, wherein the process is repeated for four times to obtain a uniform copper acetate film;
(3-4) calcining the copper acetate film obtained in the step (3-3) in a muffle furnace at 250 ℃ for 60 minutes to obtain a CuO dense seed crystal layer film covering the FTO conductive substrate,
(3-5) placing the CuO compact seed crystal layer film on the FTO conductive substrate in the step (3-4) into an aqueous solution consisting of 0.25 mol/L copper nitrate and 0.25 mol/L hexamethylenetetramine, sealing, and reacting in a 90 ℃ oven for 2 hours to obtain a CuO nanorod array;
(3-6) dissolving 0.327 g of zinc acetate in 2 g of water, stirring to dissolve, adding 8 ml of absolute ethanol and 200 microliters of glacial acetic acid, and stirring at room temperature to obtain a colorless clear transparent solution;
(3-7) spin-coating the colorless clear solution obtained in the step (3-6) on the treated FTO conductive glass at the rotating speed of 2000 rpm/min, then placing the FTO conductive glass on a heating table, and annealing at the temperature of 100 ℃ for 1 minute, wherein the process is repeated for four times to obtain a uniform zinc acetate film;
and (3-8) calcining the zinc acetate film obtained in the step (3-7) in a muffle furnace at 350 ℃ for 30 minutes to obtain a ZnO dense layer film covering the FTO conductive substrate.
(3-9) placing the ZnO dense seed crystal layer film on the FTO conductive substrate in the step (3-8) in an aqueous solution consisting of 0.25 mol/L zinc nitrate and 0.25 mol/L hexamethylenetetramine, sealing, and reacting in an oven at 90 ℃ for 2 hours to obtain a ZnO nanorod array;
(3-10) adding 50 mmol of I20.5 mol of LiI, 0.5 mol of 4-tert-butylpyridine and 0.6 mol of tetrabutylammonium iodide were dissolved in 1L of acetonitrile to prepare I-/I3 -And (3) an electrolyte.
(3-11) oppositely superposing the CuO nano array obtained in the step (3-5) and the ZnO nano array obtained in the step (3-9) and infiltrating I by utilizing capillary action-/I3 -And (4) electrolyte to complete the nano friction power generation device.
Example 2: a CuO nano array/ZnO nano array power generation device.
(4-1) preparation of a CuO nanorod array: the same procedure as in example 1 was repeated, except that the reaction time in step (3-5) was 4 hours.
(4-2) preparation of ZnO nanorod array: the same procedure as in example 1 was repeated, except that the reaction time in steps (3-9) was 4 hours.
(4-3) oppositely superposing the CuO nano array obtained in the step (4-1) and the ZnO nano array obtained in the step (4-2) and infiltrating I by utilizing capillary action-/I3 -And (4) electrolyte to complete the nano friction power generation device.
Characterization of the batteries
In comparative example 1, when a nano friction power generation device was formed using a CuO nano array and a planar ZnO film, the current density of the device wasJ sc Is 0.23 uA/cm2(ii) a In comparative example 2, when a nano friction power generation device was formed using a planar CuO film and a ZnO nano array, the current density of the device wasJ sc Is 0.48 uA/cm2(ii) a Compared with the two devices, in example 1, when the current density of the nano friction power generation device is formed by the CuO nano array and the ZnO nano array with the reaction time of 2h respectivelyJ sc Can reach 4 uA/cm2. In example 2, when the current density of the nano friction power generation device was formed using the CuO nanoarray and the ZnO nanoarray each having a reaction time of 4 hoursJ sc Can reach 8 uA/cm2. Therefore, the p-type semiconductor CuO nano array and the n-type semiconductor ZnO nano array are directly overlapped with each other, so that the interface area of the CuO and the ZnO is greatly increased, the friction between the CuO and the ZnO is more sufficient, and the concentration of generated electron holes is richer.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and those skilled in the art can make various corresponding changes and modifications according to the present invention without departing from the spirit and the essence of the present invention, but these corresponding changes and modifications should fall within the protection scope of the appended claims.

Claims (7)

1. An array interweaving friction nanometer generator is characterized in that: comprises a glass substrate, an FTO layer, a CuO nanorod array, a ZnO nanorod array and a first electrode-/I3 -An electrolyte; the FTO layer is plated on the glass substrate to be used as an electrode,the CuO nanorod array vertically grows on one FTO layer, is a hole collecting part, the ZnO nanorod array vertically grows on the other FTO layer, is an electron collecting part, and simultaneously serves as a friction electrification part together with the CuO nanorod array and the ZnO nanorod;
the FTO conductive glass substrate for growing the CuO nano array and the other FTO conductive glass substrate for growing the ZnO nano array are oppositely superposed, and I-/I3 -The electrolyte permeates into the interlaced CuO and ZnO nano-arrays.
2. An array interlaced triboelectric nanogenerator according to claim 1, wherein: the thickness of the FTO layer is 50-200 nm.
3. An array interlaced triboelectric nanogenerator according to claim 1, wherein: the length of the CuO nanorod array is 300-600 nm, the diameter of the CuO nanorod array is 30-90 nm, and the number density of the CuO nanorods is 3-6' 102Is/aremm2The length of the ZnO nanorod array is 300-600 nm, the diameter of the ZnO nanorod array is 20-50 nm, and the number density of the ZnO nanorods is 3-6' 102Is/aremm2。
4. A method for preparing an array interweaving type friction nano-generator according to claim 1, which is characterized by comprising the following steps:
(1) obtaining clean FTO conductive glass for later use;
(2) growing a CuO nano array and a ZnO nano array on FTO conductive glass by using a hydrothermal reaction method;
(3) superposing one FTO conductive glass substrate for growing the CuO nano array and the other FTO conductive glass substrate for growing the ZnO nano array in an opposite direction;
(4) by capillary action of the liquid I-/I3 -The electrolyte penetrates into the interlaced CuO and ZnO nano array.
5. The method for preparing an array interweaving type friction nanogenerator according to claim 4, wherein the process for growing the CuO nanoarray on the FTO conductive glass by using the hydrothermal reaction method in the step (2) comprises the following steps:
(1) dissolving copper acetate in absolute ethyl alcohol, and stirring the obtained mixture at room temperature to obtain a blue clear solution;
(2) spin-coating the blue clear solution obtained in the step (1) on the treated FTO conductive glass, and then placing the FTO conductive glass on a heating table to obtain a uniform copper acetate film;
(3) calcining the copper acetate film obtained in the step (2) in a muffle furnace to obtain a CuO compact seed crystal layer film covering the FTO conductive substrate;
(4) and (4) placing the CuO compact seed crystal layer film on the FTO conductive substrate in the step (3) into an aqueous solution consisting of copper nitrate and hexamethylenetetramine, sealing, and reacting in an oven to obtain the CuO nanorod array.
6. The method for preparing an array interweaving friction nanometer generator according to claim 4, wherein the process of growing the ZnO nanometer array on the FTO conductive glass by using the hydrothermal reaction method in the step (2) comprises the following steps:
(1) dissolving zinc acetate in water, stirring to dissolve, adding anhydrous ethanol and glacial acetic acid, and stirring at room temperature to obtain colorless clear transparent solution;
(2) spin-coating the colorless clear solution obtained in the step (1) on the treated FTO conductive glass, and then placing the FTO conductive glass on a heating table for annealing to obtain a uniform zinc acetate film;
(3) calcining the zinc acetate film obtained in the step (2) in a muffle furnace to obtain a ZnO dense seed crystal layer film covering the FTO conductive substrate;
(4) and (4) placing the ZnO dense seed crystal layer film on the FTO conductive substrate in the step (3) into an aqueous solution consisting of copper nitrate and hexamethylenetetramine, sealing, and reacting in an oven to obtain the ZuO nanorod array.
7. The method for preparing an array interweaving friction nanometer generator according to claim 4, wherein the specific steps of the step (4) are as follows: will I2LiI, 4-tert-butylpyridine and tetrabutylammonium iodide are dissolved in acetonitrile to prepare I-/I3 -An electrolyte; by capillary action-/I3 -And the electrolyte permeates into the interlaced CuO and ZnO nano array to complete the nano friction power generation device.
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