CN114551110A - Cut carbon nanotube @ TiO2Nanotube array heterostructure and preparation method and device thereof - Google Patents
Cut carbon nanotube @ TiO2Nanotube array heterostructure and preparation method and device thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a cut-off carbon nano tube @ TiO2Nanotube array heterostructure, preparation method and device thereof, and TiO regulated by controlling reaction conditions2Nanotube array structure and length/diameter size and proportion of carbon nanotubes; carbon nano tube @ TiO with different filling densities formed by electrophoresis method2A nanotube array heterostructure; the obtained heterostructures with the series of structural differences are prepared into brand new photovoltaic devices under two conditions of no electrolyte and the presence of the electrolyte. Average photocurrent density from pure TiO216 muA/cm of nanotube array2Increasing the concentration to 20-23 muA/cm2(ii) a The device exhibits an efficiency of 0.01% to 2%. The device has simple manufacturing method, low cost and no pollution, is a novel structure for effectively utilizing sunlight, and widens TiO2And the application of the carbon nano tube in the photovoltaic field.
Description
Technical Field
The invention relates to a material and a construction method of a photovoltaic device, in particular to a cut carbon nano tube filled TiO2A heterostructure of a nanotube array, a preparation method thereof, a brand new photovoltaic device and a construction method thereof.
Background
Solar energy has been widely noticed by people as a novel energy source, TiO2As a semiconductor material, it has a suitable forbidden band width, low cost and good chemical stability, and has been widely used in solar cells. TiO based on titanium substrate growth2The nanotube array has high orientation, can provide a good path for electron transfer, has simple manufacturing method, avoids the complicated process of organic synthesis, and provides possibility for large-scale roll-to-roll production. The TiO existing at present2Nanocrystalline chemical cells, in which the photosensitizer component requires complex organic synthesis and is expensive, have limited their development.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for cutting off carbon nano tube @ TiO2A preparation method of a nanotube array heterostructure is provided, and the nanotube array heterostructure is used for a brand new photovoltaic device.
The technical scheme of the invention is as follows:
cut-off carbon nano tube @ TiO2The preparation method of the nanotube array heterostructure comprises the following steps: (1) anodic oxidation of TiO on metallic titanium substrates2A nanotube array; (2) heating and stirring the carbon nano tube in the mixed acid solution, and cutting off; (3) to prepare a TiO-loaded catalyst2The metal titanium substrate of the nanotube array is a positive electrode, the platinum foil is a negative electrode, and the carbon nanotubes are filled into TiO by an electrophoresis method2Nanotube array formed on a metallic titanium substrateBroken carbon nanotube @ TiO2Nanotube array heterostructures.
The preparation method comprises the step of forming TiO on a metal titanium substrate by anodic oxidation2The nanotube array is at room temperature, and the volume ratio of the electrolyte is as follows: 95% of diethylene glycol, 2% of hydrofluoric acid solution and 3% of deionized water, the voltage is 20V-55V, and the oxidation time is 0.5-24 h.
According to the preparation method, the diameter of the used carbon nano tube is 8-15 nm, and the length of the carbon nano tube is 0.5-2 mu m; cutting carbon nanotube with mixed acid and concentrating with H2SO4And concentrated HNO3The volume ratio of (A) to (B) is 7: 3-1: 1, the temperature is 70-80 ℃, and the treatment time is 5-12 h.
The preparation method comprises the step of preparing the TiO-loaded suspension in the cut carbon nanotube suspension2The metal titanium substrate of the nanotube array is a positive electrode, the platinum foil is a negative electrode, electrophoresis is carried out under the voltage of 10-30V, and at the moment, the carbon nanotubes with negative electricity groups after oxidation cutting enter the TiO under the action of an external electric field2Nanotube array, direction and duration of constantly alternating voltage during electrophoresis: the forward direction lasts for 5-30 min, the reverse direction lasts for 5-30 min, and the steps are repeated for 10-30 times to form the carbon nano tube @ TiO with different filling densities2Nanotube array heterostructures.
The cut carbon nanotube @ TiO prepared by any one of the methods2Nanotube array heterostructures.
The cut carbon nano tube @ TiO2The photovoltaic device prepared by the nanotube array heterostructure is prepared by cutting off the carbon nanotube @ TiO2The metallic titanium substrate of the nanotube array heterostructure is arranged in the sealed insulation groove and covered with the counter electrode.
The photovoltaic device is characterized in that a cut carbon nanotube aqueous solution is taken and spin-coated on transparent conductive glass to form a cut carbon nanotube film, and the cut carbon nanotube film is dried and then used as a counter electrode.
The photovoltaic device is prepared by cutting off the carbon nano tube @ TiO2Placing the metallic titanium substrate of the nanotube array heterostructure in the sealed insulation groove, and then electrolyzing appropriate amounts of iodine electrolyte, iron electrolyte, cobalt electrolyte and copper electrolyteElectrolyte or chalcogenide electrolyte is injected into the groove from the edge and covers the counter electrode.
The iodine electrolyte of the photovoltaic device is as follows: 0.5M lithium iodide, 0.05M iodine and 0.5M 4-tert-butylpyridine, the solvent being acetonitrile.
The photovoltaic device is characterized in that the iron electrolyte is as follows: 0.2M potassium ferricyanide and 0.2M potassium ferrocyanide, the solvent being water.
The cut carbon nano tube @ TiO2The photovoltaic device prepared by the nanotube array heterostructure has the advantages that the carbon nanotube after oxidation cutting has certain band gap width and TiO2Formation of appropriate energy level matching while carbon nanotubes are the darkest material in the world can improve TiO2Absorbing light, so that in the photovoltaic device, the carbon nano tube is used as a photosensitizer to prepare the cut carbon nano tube @ TiO2The nanotube array photoanode takes transparent conductive glass with carbon nanotubes as a counter electrode to construct a brand new titanium-carbon photovoltaic device, and the performance tests are respectively carried out under the two conditions of no electrolyte and the presence of electrolyte, so that the efficiency of the obtained device is 0.01% -2%.
Without an electrolyte, the electrons conduct only through direct contact of the two materials; when added to an electrolyte, the conduction of electrons is mainly through two pathways: (1) direct contact electron conduction: the carbon nano tube is used as a photosensitizer, absorbs light energy electrons to jump to a conduction band, and is transferred to TiO through direct contact of the two materials2. (2) Indirect contact electron conduction. After addition of a suitable amount of electrolyte, the device efficiency is improved compared to that without electrolyte, which is comparable to carbon nanotubes and TiO2The contact point between the two is related, the electrolyte is used as a bridge to realize the transportation of electrons and holes, the carbon nano tube is excited by illumination, the electrons jump to a conduction band, the oxidation state electrolyte receives the electrons to be changed into a reduction state, and the electrons are transferred to TiO2Then changing into oxidation state again, taking iodine electrolyte as an example, the specific process is as follows:
(cut-MWCNTs)+hν→(cut-MWCNTs)* (1)
(cut-MWCNTs)*→(cut-MWCNTs)++e- (cb) (2)
I3 -+2e-(cb)→3I- (3)
TiO2+3I-→(TiO2)-+I3 - (4)
the invention has the following beneficial effects:
1. the carbon nano tube is cheap and easy to obtain, and oxygen-containing functional groups can be introduced to the surface of the carbon nano tube through mixed acid treatment, so that the band gap width of the carbon nano tube is changed, the band gap can be adjusted, and the purpose of adjusting the band gap with TiO is achieved2Proper energy level matching, and in addition, the mixed acid treatment cuts off the carbon nanotubes, and the short carbon nanotubes can be mixed with TiO2More fully bound, this provides us with a potential photosensitizer. 2. The cut carbon nano tube @ TiO is prepared by a simple electrophoresis method2Nanotube array heterostructures, comparable to pure TiO2Nanotube arrays have better photocurrent response.
3. Based on cutting off carbon nano tube @ TiO2The nanotube array heterostructure can be used for preparing a brand-new photovoltaic device, and compared with the traditional photovoltaic device, the photovoltaic device has lower cost and a simple manufacturing method. The method is a brand new attempt and provides reference value for the application of the carbon nano tube in the titanium-carbon photovoltaic device.
Drawings
FIG. 1 is pure TiO2A Field Emission Scanning Electron Microscopy (FESEM) pattern (a) and an X-ray diffraction (XRD) pattern (b) of the nanotube array;
FIG. 2 is a Transmission Electron Microscope (TEM) image of pristine carbon nanotubes (a) and cut carbon nanotubes (b);
FIG. 3 is a cut carbon nanotube @ TiO2A Field Emission Scanning Electron Microscope (FESEM) image of the nanotube array heterostructure;
FIG. 4 shows pure TiO2Nanotube array, cut carbon nanotubes @ TiO2A photocurrent response graph of the nanotube array heterostructure;
FIG. 5 is a diagram showing the structure of a photovoltaic device, 1 transparent conductive glass, 2 cut carbon nanotube film, 3 electrolyte, 4 cut carbon nanotube, 5TiO2Nanotube array, 6TiO2A barrier layer, 7 a metallic titanium substrate;
fig. 6 is a graph of current density-voltage (J-V) characteristics of a photovoltaic device without electrolyte (example one) and with the addition of an iron-based electrolyte (example three).
Detailed Description
The present invention will be described in detail with reference to specific examples.
The first embodiment is as follows:
grinding a metal titanium substrate (pure titanium foil) by using sand paper, cleaning and polishing, and storing in deionized water for later use. Platinum foil was used as the counter electrode. The electrolyte solution is 95% diethylene glycol, 2% hydrofluoric acid solution and 3% deionized water by volume. Anodizing at 55V at room temperature for 1h to form TiO on the metallic titanium substrate2Nanotube array, as shown in FIG. 5, TiO is formed on a metallic titanium substrate 7 by anodic oxidation2Nanotube array 5 on TiO at the same time2TiO is formed at the bottom of the nanotube array2A barrier layer 6. Bringing the film with TiO2The metallic titanium substrate of the nanotube array was sequentially rinsed in isopropanol and deionized water to remove electrolytes, dried in a fume hood, and then the dried sample was annealed at 530 ℃ for 3h in an air atmosphere to obtain a crystal structure. FIG. 1 is pure TiO2Field Emission Scanning Electron Microscopy (FESEM) and X-ray diffraction (XRD) patterns (a, b) of nanotube arrays, TiO2Is in an ordered tubular array structure and takes an anatase crystal form after annealing.
Suspending 100mg of carbon nanotubes in 30mL of concentrated H2SO4Stirring for 30min at room temperature, and then adding 18mL of concentrated HNO3And heating and stirring at 70-80 ℃ for 8 h. The cut carbon nanotubes were collected by centrifugation, washed repeatedly with deionized water until the pH reached neutrality, and then freeze-dried to obtain cut carbon nanotube solid powder. FIG. 2 is a Transmission Electron Microscope (TEM) image of pristine carbon nanotubes (FIG. a) and cut carbon nanotubes (FIG. b). The cut carbon nanotubes were dispersed in deionized water and sonicated to produce a uniform suspension. To prepare a well-prepared film with TiO2The metal titanium substrate of the nanotube array is used as the anode, the platinum foil is used as the cathode, 10V voltage is applied to cut off the carbon nanotube suspension, the forward direction lasts for 5min, then the electrode direction is changed, and the reverse direction lasts for 5minRepeating for 10 times (i.e. repeating for 10 times to apply forward and reverse voltage for 5min) for 5min, and filling the carbon nanotubes in the solution into TiO under the action of the electric field2Cutting off the carbon nanotube @ TiO formed in the tube and in the gap of the nanotube array2Nanotube array heterostructure, FIG. 3 cut carbon nanotubes @ TiO2The Field Emission Scanning Electron Microscope (FESEM) of the heterostructure of nanotube array shows that part of the carbon nanotubes enter into TiO2And in the gap. FIG. 4 shows pure TiO2Nanotube array, cut carbon nanotube @ TiO2Photocurrent response diagram of nanotube array heterostructure, and pure TiO2In contrast, carbon nanotubes are comparable to TiO2The combination of (a) and (b) results in an improved photogenerated charge separation efficiency.
Constructing a device: the metallic titanium substrate 7 is oxidized anodically to form TiO2Nanotube array 5 with TiO formed at the bottom of the array2A barrier layer 6, the array being combined with the cut carbon nanotubes 4 to form cut carbon nanotubes @ TiO2A nanotube array heterostructure; 1mL of 0.002g/mL cutting carbon nanotube aqueous solution is taken to be spin-coated on transparent conductive glass 1 at the rotating speed of 500 revolutions/second to form a cutting carbon nanotube film 2 which is used as a counter electrode after being dried; cutting the prepared carbon nano tube @ TiO2The metallic titanium substrate 7 of the nanotube array heterostructure is placed in a sealing insulation groove with the depth of 0.5mm, a counter electrode is covered, the two electrodes are staggered with each other, a small part of lead-out two-pole lead wires are reserved, a clamp is used for clamping and sealing, and then the current density-voltage (J-V) characteristic test of a device is carried out under the AM 1.5G solar illumination.
Example two:
and grinding the metal titanium substrate (pure titanium foil) by using sand paper, cleaning and polishing the metal titanium substrate, and storing the metal titanium substrate in deionized water for later use. A platinum foil was used as the counter electrode. The electrolyte solution is 95% diethylene glycol, 2% hydrofluoric acid solution and 3% deionized water by volume. Anodizing at 55V at room temperature for 2h to form TiO on the metallic titanium substrate2An array of nanotubes. Bringing the film with TiO2The metallic titanium substrate of the nanotube array was sequentially rinsed in isopropanol and deionized water to remove the electrolyte, dried in a fume hood, and the dried sample was then placed in an air atmosphere 53Annealing at 0 deg.C for 3h to obtain the crystal structure.
Suspending 100mg of carbon nanotubes in 30mL of concentrated H2SO4Stirring for 30min at room temperature, and then adding 18mL of concentrated HNO3Heating and stirring at 70-80 ℃ for 10 h. The cut carbon nanotubes were collected by centrifugation, washed repeatedly with deionized water until the pH reached neutrality, and then freeze-dried to obtain cut carbon nanotube solid powder. The cut carbon nanotubes were dispersed in deionized water and sonicated to produce a uniform suspension. To prepare a prepared film with TiO2Applying 20V voltage to the metal titanium substrate of the nanotube array as the positive electrode and the platinum foil as the negative electrode, maintaining the positive direction for 20min, changing the electrode direction, maintaining the reverse direction for 5min, repeating the steps for 20 times, and filling the carbon nanotubes in the solution into TiO under the action of the electric field2Cutting off the carbon nanotube @ TiO formed in the tube and in the gap of the nanotube array2Nanotube array heterostructures.
Constructing a device: the metallic titanium substrate 7 is oxidized anodically to form TiO2Nanotube array 5 with TiO formed at the bottom of the array2A barrier layer 6, the array being combined with the cut carbon nanotubes 4 to form cut carbon nanotubes @ TiO2A nanotube array heterostructure; 1mL of 0.002g/mL cut carbon nanotube aqueous solution is taken to be spin-coated on transparent conductive glass 1 at the rotating speed of 500 r/s to form a cut carbon nanotube film 2, and the cut carbon nanotube film is used as a counter electrode after being dried; cutting the prepared carbon nano tube @ TiO2A metallic titanium substrate 7 of a nanotube array heterostructure is placed in a sealed insulation groove with the depth of 0.5mm, a counter electrode is covered, the two electrodes are staggered with each other, a small part of lead-out bipolar lead is reserved, a clamp is used for clamping and sealing, a proper amount (not exceeding the height of the heterostructure) of iodine electrolyte is injected from the edge, the electrolyte is acetonitrile solution of 0.5M lithium iodide, 0.05M iodine and 0.5M 4-tert-butylpyridine, and then the current density-voltage (J-V) characteristic test of a device is carried out under AM 1.5G solar illumination.
Example three:
and grinding the metal titanium substrate (pure titanium foil) by using sand paper, cleaning and polishing the metal titanium substrate, and storing the metal titanium substrate in deionized water for later use. Platinum foil was used as the counter electrode. The electrolyte solution is 95 percent diethylene glycol and 2 percent hydrogen by volumeFluoric acid solution, 3% deionized water. Anodizing at 55V for 4h at room temperature to form TiO on the metallic titanium substrate2An array of nanotubes. Bringing the film with TiO2The metallic titanium substrate of the nanotube array was sequentially rinsed in isopropanol and deionized water to remove electrolytes, dried in a fume hood, and then the dried array was annealed at 530 ℃ for 3h in an air atmosphere to obtain a crystal structure.
Suspending 100mg of carbon nanotubes in 30mL of concentrated H2SO4Stirring for 30min at room temperature, and then adding 18mL of concentrated HNO3Heating and stirring at 70-80 ℃ for 12 h. And collecting the cut carbon nano tubes by centrifugation, repeatedly washing the carbon nano tubes by deionized water until the pH value reaches neutral, and freeze-drying the carbon nano tubes to obtain the cut carbon nano tube solid powder. The cut carbon nanotubes were dispersed in deionized water and sonicated to produce a uniform suspension. To prepare a prepared film with TiO2Applying 30V voltage to the metal titanium substrate of the nanotube array as the positive electrode and the platinum foil as the negative electrode, maintaining the positive direction for 30min, changing the electrode direction, maintaining the reverse direction for 10min, repeating for 30 times, and filling the carbon nanotubes in the solution into TiO under the action of the electric field2Cutting off the carbon nanotube @ TiO formed in the tube and in the gap of the nanotube array2A nanotube array heterostructure.
Constructing a device: the metallic titanium substrate 7 is oxidized anodically to form TiO2Nanotube array 5 with TiO formed at the bottom of the array2A barrier layer 6 formed by combining the array and the cut carbon nanotubes 4 to form cut carbon nanotubes @ TiO2A nanotube array heterostructure; 1mL of 0.002g/mL cut carbon nanotube aqueous solution is taken to be spin-coated on transparent conductive glass 1 at the rotating speed of 500 r/s to form a cut carbon nanotube film 2, and the cut carbon nanotube film is used as a counter electrode after being dried; cutting off the prepared carbon nano tube @ TiO2Placing metallic titanium substrate 7 of nanotube array heterostructure in 0.5mm deep sealed insulation groove, covering with counter electrode, staggering the two electrodes, reserving a small part to lead out two-pole lead, clamping and sealing with clamp, injecting appropriate amount (not more than heterostructure height) of iron system electrolyte from edge, the electrolyte is 0.2M potassium ferricyanide and 0.2M potassium ferrocyanide water solution, and then illuminating with AM 1.5G solar energyAnd carrying out a current density-voltage (J-V) characteristic test of the device. Fig. 6 is a graph of current density-voltage (J-V) characteristics of a photovoltaic device without electrolyte (example one) and with the addition of an iron-based electrolyte (example three).
Example four:
and grinding the metal titanium substrate (pure titanium foil) by using sand paper, cleaning and polishing the metal titanium substrate, and storing the metal titanium substrate in deionized water for later use. Platinum foil was used as the counter electrode. The electrolyte solution is 95% diethylene glycol, 2% hydrofluoric acid solution and 3% deionized water by volume. Anodizing at 55V at room temperature for 8h to form TiO on the metallic titanium substrate2An array of nanotubes. Oxidized with TiO2The metallic titanium substrate of the nanotube array was sequentially rinsed in isopropanol and deionized water to remove electrolytes, dried in a fume hood, and then the dried array was annealed at 530 ℃ for 3h in an air atmosphere to obtain a crystal structure.
Suspending 100mg of carbon nanotubes in 30mL of concentrated H2SO4Stirring for 30min at room temperature, and then adding 18mL of concentrated HNO3And heating and stirring at 70-80 ℃ for 8 h. And collecting the cut carbon nano tubes by centrifugation, repeatedly washing the carbon nano tubes by deionized water until the pH value reaches neutral, and freeze-drying the carbon nano tubes to obtain the cut carbon nano tube solid powder. The cut carbon nanotubes were dispersed in deionized water and sonicated to produce a uniform suspension. To prepare a prepared film with TiO2Applying 10V voltage to the metal titanium substrate of the nanotube array as the positive electrode and platinum foil as the negative electrode, maintaining the positive direction for 10min, changing the electrode direction, maintaining the reverse direction for 5min, repeating for 10 times, and filling the carbon nanotubes in the solution into TiO under the action of the electric field2Cutting off the carbon nanotube @ TiO formed in the tube and in the gap of the nanotube array2Nanotube array heterostructures.
Constructing a device: the metallic titanium substrate 7 is oxidized anodically to form TiO2Nanotube array 5 with TiO formed at the bottom of the array2A barrier layer 6, the array being combined with the cut carbon nanotubes 4 to form cut carbon nanotubes @ TiO2A nanotube array heterostructure; 1mL of 0.002g/mL cut carbon nanotube aqueous solution is taken to be spin-coated on the transparent conductive glass 1 at the rotating speed of 500 r/s to form the cut carbon nanotubeMembrane 2, dried to serve as a counter electrode; cutting the prepared carbon nano tube @ TiO2Placing metallic titanium substrate 7 of nanotube array heterostructure in a sealed insulation groove with a depth of 0.5mm, covering a counter electrode, staggering the two electrodes, reserving a small part to lead out two electrodes, clamping and sealing by a clamp, injecting proper amount (not exceeding the height of heterostructure) of cobalt electrolyte from the edge, wherein the electrolyte is 0.25M [ Co (II) (phen)3](PF6)2，0.05M[Co(II)(phen)3](PF6)30.3M 4-tert-butylpyridine, 0.1M lithium bis (trifluoromethanesulfonylimide) in acetonitrile, followed by testing of the current density-voltage (J-V) characteristics of the devices under AM 1.5G solar illumination.
Example five:
and grinding the metal titanium substrate (pure titanium foil) by using sand paper, cleaning and polishing the metal titanium substrate, and storing the metal titanium substrate in deionized water for later use. Platinum foil was used as the counter electrode. The electrolyte solution is 95% diethylene glycol, 2% hydrofluoric acid solution and 3% deionized water by volume. Anodizing at 55V at room temperature for 16h to form TiO on the metallic titanium substrate2An array of nanotubes. Oxidized with TiO2The metallic titanium substrate of the nanotube array was sequentially rinsed in isopropanol and deionized water to remove electrolytes, dried in a fume hood, and then the dried array was annealed at 530 ℃ for 3h in an air atmosphere to obtain a crystal structure.
Suspending 100mg of carbon nanotubes in 30mL of concentrated H2SO4Stirring for 30min at room temperature, and then adding 18mL of concentrated HNO3Heating and stirring at 70-80 ℃ for 10 h. And collecting the cut carbon nano tubes by centrifugation, repeatedly washing the carbon nano tubes by deionized water until the pH value reaches neutral, and freeze-drying the carbon nano tubes to obtain the cut carbon nano tube solid powder. The cut carbon nanotubes were dispersed in deionized water and sonicated to produce a uniform suspension. To prepare a prepared film with TiO2Applying 20V voltage to the metal titanium substrate of the nanotube array as the positive electrode and the platinum foil as the negative electrode, maintaining the positive direction for 20min, changing the electrode direction, maintaining the reverse direction for 10min, repeating the steps for 20 times, and filling the carbon nanotubes in the solution into TiO under the action of the electric field2The inside of the tube and the gap of the nanotube array form a cutBroken carbon nanotube @ TiO2Nanotube array heterostructures.
Constructing a device: the metallic titanium substrate 7 is oxidized anodically to form TiO2Nanotube array 5 with TiO formed at the bottom of the array2Barrier layer 6 of TiO2The nanotube array 5 is combined with the cut carbon nanotube 4 to form a cut carbon nanotube @ TiO2A nanotube array heterostructure; 1mL of 0.002g/mL cut carbon nanotube aqueous solution is taken to be spin-coated on transparent conductive glass 1 at the rotating speed of 500 r/s to form a cut carbon nanotube film 2, and the cut carbon nanotube film is used as a counter electrode after being dried; cutting the prepared carbon nano tube @ TiO2Placing the metallic titanium substrate 7 of the nanotube array heterostructure in a sealed insulation groove with the depth of 0.5mm, covering the counter electrode, staggering the two electrodes, reserving a small part of lead-out two-pole lead wires, clamping and sealing by a clamp, injecting a proper amount (not exceeding the height of the heterostructure) of copper electrolyte from the edge, wherein the electrolyte is 0.2M copper complex redox medium (Cu)II/(CuI+CuII) 0.4, wherein CuIIIs [ Cu (phen) ]2](CF3SO3)2，CuIIIs [ Cu (phen) ]2](CF3SO3) 0.5M 4-tert-butylpyridine, 0.5M lithium perchlorate in methoxyacetonitrile, after which the current density-voltage (J-V) characteristics of the devices were tested under AM 1.5G solar illumination.
Example six:
grinding a metal titanium substrate (pure titanium foil) by using sand paper, cleaning and polishing, and storing in deionized water for later use. Platinum foil was used as the counter electrode. The electrolyte solution is 95% diethylene glycol, 2% hydrofluoric acid solution and 3% deionized water by volume. Anodizing at 55V at room temperature for 24h to form TiO on the metallic titanium substrate2An array of nanotubes. Oxidized with TiO2The metallic titanium substrate of the nanotube array was sequentially rinsed in isopropanol and deionized water to remove electrolytes, dried in a fume hood, and then the dried array was annealed at 530 ℃ for 3h in an air atmosphere to obtain a crystal structure.
Suspending 100mg of carbon nanotubes in 30mL of concentrated H2SO4Stirring at room temperature for 30min, then 18mL concentrated HNO was added3Heating and stirring at 70-80 ℃ for 12 h. And collecting the cut carbon nano tubes by centrifugation, repeatedly washing the carbon nano tubes by deionized water until the pH value reaches neutral, and freeze-drying the carbon nano tubes to obtain the cut carbon nano tube solid powder. The cut carbon nanotubes were dispersed in deionized water and sonicated to produce a uniform suspension. To prepare a prepared film with TiO2Applying 30V voltage to the metal titanium substrate of the nanotube array as the positive electrode and the platinum foil as the negative electrode, maintaining the positive direction for 30min, changing the electrode direction, maintaining the reverse direction for 5min, repeating for 30 times, and filling the carbon nanotubes in the solution into TiO under the action of the electric field2Cutting off the carbon nano tube @ TiO formed in the tube and in the gap of the nano tube array2Nanotube array heterostructures.
Constructing a device: the metallic titanium substrate 7 is oxidized anodically to form TiO2Nanotube array 5 with TiO formed at the bottom of the array2Barrier layer 6 of TiO2The nanotube array 5 is combined with the cut carbon nanotube 4 to form a cut carbon nanotube @ TiO2A nanotube array heterostructure; 1mL of 0.002g/mL cut carbon nanotube aqueous solution is taken to be spin-coated on transparent conductive glass 1 at the rotating speed of 500 r/s to form a cut carbon nanotube film 2, and the cut carbon nanotube film is used as a counter electrode after being dried; cutting the prepared carbon nano tube @ TiO2The metallic titanium substrate 7 of the nanotube array heterostructure is placed in a sealing insulation groove with the depth of 0.5mm, a counter electrode is covered, the two electrodes are mutually staggered, a small part of lead-out two-pole lead wires are reserved, a clamp is used for clamping and sealing, a proper amount (not exceeding the height of the heterostructure) of chalcogenide electrolyte is injected from the edge, the electrolyte is an aqueous solution of 3.38M sodium sulfate, 2M sulfur and 0.27M potassium chloride, and then the current density-voltage (J-V) characteristic test of the device is carried out under AM 1.5G solar illumination.
It will be appreciated that modifications and variations are possible to those skilled in the art in light of the above teachings, and it is intended to cover all such modifications and variations as fall within the scope of the appended claims.
Claims (10)
1. Cut-off carbon nano tube @ TiO2Preparation method of nanotube array heterostructureThe method is characterized in that: the method comprises the following steps: (1) anodic oxidation of TiO on metallic titanium substrates2A nanotube array; (2) heating and stirring the carbon nano tube in the mixed acid solution, and cutting off; (3) to prepare a TiO-loaded catalyst2The metal titanium substrate of the nanotube array is a positive electrode, the platinum foil is a negative electrode, and the carbon nanotubes are filled into TiO by an electrophoresis method2A nanotube array formed by cutting off carbon nanotubes (TiO) on a metallic titanium substrate2Nanotube array heterostructures.
2. The method of claim 1, wherein the anodic oxidation forms TiO on a metallic titanium substrate2The nanotube array is at room temperature, and the volume ratio of the electrolyte is as follows: 95% of diethylene glycol, 2% of hydrofluoric acid solution and 3% of deionized water, the voltage is 20V-55V, and the oxidation time is 0.5-24 h.
3. The method according to claim 1, wherein the carbon nanotubes used have a diameter of 8 to 15nm and a length of 0.5 to 2 μm; cutting carbon nanotube with mixed acid and concentrating with H2SO4And concentrated HNO3The volume ratio of (A) to (B) is 7: 3-1: 1, the temperature is 70-80 ℃, and the treatment time is 5-12 h.
4. The method of claim 1, wherein the TiO-loaded suspension is prepared in a chopped carbon nanotube suspension2The metal titanium substrate of the nanotube array is a positive electrode, the platinum foil is a negative electrode, electrophoresis is carried out under the voltage of 10-30V, and at the moment, the carbon nanotubes with negative electricity groups after oxidation cutting enter the TiO under the action of an external electric field2Nanotube array, direction and duration of constantly alternating voltage during electrophoresis: the forward direction lasts for 5-30 min, the reverse direction lasts for 5-30 min, and the steps are repeated for 10-30 times to form the carbon nano tube @ TiO with different filling densities2Nanotube array heterostructures.
5. Cut carbon nanotubes @ TiO obtainable by the process as claimed in any one of claims 1 to 42Nanotube array heterostructure。
6. The cut carbon nanotube @ TiO of claim 52The photovoltaic device prepared by the nanotube array heterostructure is characterized in that the prepared photovoltaic device with the cut carbon nanotube @ TiO2The metallic titanium substrate of the nanotube array heterostructure is arranged in the sealed insulating groove and covered with the counter electrode.
7. The photovoltaic device according to claim 6, wherein the cut carbon nanotube film is formed by spin-coating an aqueous solution of cut carbon nanotubes on a transparent conductive glass, and dried to be used as a counter electrode.
8. The photovoltaic device of claim 6, wherein the prepared tape with cut carbon nanotubes @ TiO is processed2The metallic titanium substrate of the nanotube array heterostructure is placed in the sealed insulation groove, then a proper amount of iodine electrolyte, iron electrolyte, cobalt electrolyte, copper electrolyte or sulfur electrolyte is injected into the groove from the edge, and the counter electrode is covered.
9. The photovoltaic device according to claim 8, wherein the iodine-based electrolyte is: 0.5M lithium iodide, 0.05M iodine and 0.5M 4-tert-butylpyridine, the solvent being acetonitrile.
10. The photovoltaic device according to claim 8, wherein the iron-based electrolyte is: 0.2M potassium ferricyanide and 0.2M potassium ferrocyanide, the solvent being water.
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