CN113744767A - Method for preparing titanium dioxide film with grating structure by using DVD (digital video disk) optical disk, film prepared by method and application of film - Google Patents
Method for preparing titanium dioxide film with grating structure by using DVD (digital video disk) optical disk, film prepared by method and application of film Download PDFInfo
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- CN113744767A CN113744767A CN202111013985.8A CN202111013985A CN113744767A CN 113744767 A CN113744767 A CN 113744767A CN 202111013985 A CN202111013985 A CN 202111013985A CN 113744767 A CN113744767 A CN 113744767A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 15
- 230000003287 optical effect Effects 0.000 title claims description 12
- 239000011521 glass Substances 0.000 claims abstract description 49
- 238000001035 drying Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 17
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 17
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 17
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004528 spin coating Methods 0.000 claims abstract description 11
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 57
- 239000000203 mixture Substances 0.000 claims description 22
- 239000010410 layer Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229920000515 polycarbonate Polymers 0.000 claims description 10
- 239000004417 polycarbonate Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000000059 patterning Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000007872 degassing Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000011241 protective layer Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- MFYSUUPKMDJYPF-UHFFFAOYSA-N 2-[(4-methyl-2-nitrophenyl)diazenyl]-3-oxo-n-phenylbutanamide Chemical compound C=1C=CC=CC=1NC(=O)C(C(=O)C)N=NC1=CC=C(C)C=C1[N+]([O-])=O MFYSUUPKMDJYPF-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Images
Classifications
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
- G11B7/252—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers
- G11B7/253—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers of substrates
- G11B7/2533—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers of substrates comprising resins
- G11B7/2534—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers of substrates comprising resins polycarbonates [PC]
Abstract
The invention belongs to the technical field of semiconductor films, and discloses a method for preparing a titanium dioxide film with a grating structure by using a DVD (digital video disk) and a film prepared by the method and application of the film. Stirring and mixing absolute ethyl alcohol, triethanolamine, tetrabutyl titanate and deionized water to prepare a precursor solution, spin-coating the precursor solution on clean transparent conductive glass, then attaching a pre-prepared polydimethylsiloxane film on the transparent conductive glass with a wet film, applying 150 pascal pressure, and annealing in a drying oven; after cooling to room temperature, uncovering the polydimethylsiloxane film attached to the transparent conductive glass, then putting the transparent conductive glass into a muffle furnace for annealing at 550 ℃ for 2 hours to obtain the TiO film with the grating structure2A film of (2). The method is simple to operate, short in preparation time and high in repeatability, and can be used as the anode of the solar cell in the field of solar cells without being carried out under a special vacuum environment condition.
Description
Technical Field
The invention belongs to the technical field of semiconductor films, and particularly relates to a method for preparing a titanium dioxide film with a grating structure by using a DVD (digital video disk) and a film prepared by the method and application of the film.
Background
With the development of the solar cell field, the photoelectric conversion efficiency of films prepared by some traditional transparent conductive film materials can not meet the requirements of people on energy. At present, researchers are dedicated to changing the structure of the surface of the film or preparing a multilayer composite transparent conductive film for improving the efficiency of the solar cell. Wherein, changing the structure of the film refers to preparing a micro-nano structure on the surface of the film. Up to now, there have been a pyramid structure, a grating structure, a honeycomb structure, and the like. These structures can reduce the surface of light reflection and improve the transmittance of the film. At present, several commonly used methods for preparing a micro-nano structure on the surface of a film mainly comprise an electron beam etching method, a plasma etching method, a nano-imprinting method, an electrochemical deposition method and the like. However, most of the methods have the problems of complicated preparation process, long preparation time period and high manufacturing cost, and some methods require expensive instruments and chemicals, some methods also require addition of toxic and harmful chemical reagents, some methods also require harsh environmental conditions, and the like. In addition, controllability is not easy to guarantee when the transparent conductive film structure is prepared by adopting the methods, and the appearance and the size of the obtained product are not uniform.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention mainly aims to provide a method for preparing a titanium dioxide film with a grating structure by using a DVD optical disk; the method is simple, low in cost and high in repeatability, and special gas is not needed to be used as an environmental medium.
The invention also aims to provide a titanium dioxide film prepared by the method.
The invention also aims to provide application of the titanium dioxide film.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a titanium dioxide film with a grating structure by utilizing a DVD optical disk comprises the following steps:
(1) removing the protective layer above the polycarbonate disc layer of the unrecorded DVD disc, washing with absolute ethyl alcohol in an ultrasonic cleaning machine, and drying for later use; mixing the following components in a mass ratio of 10: 1, mixing and stirring uniformly the Dow Corning 184 and the curing agent, casting the mixture on a polycarbonate disc layer of a DVD optical disc, degassing the mixture in a vacuum drying oven at the temperature of between 60 and 80 ℃, and curing the mixture for 1.5 to 2 hours; then stripping the polydimethylsiloxane film with the grating pattern from the DVD optical disk;
(2) dropwise adding absolute ethyl alcohol, triethanolamine and tetrabutyl titanate into a beaker in sequence, and fully stirring for 15-30 minutes; then, deionized water is dripped into the mixed solution, and the mixed solution is fully stirred for 15-30 minutes to obtain TiO2Sol; the volume ratio of the absolute ethyl alcohol to the triethanolamine to the tetrabutyl titanate to the deionized water is 12: 1: 3: 1;
(3) 80-120 mu L of TiO obtained in the step (2)2Dropwise adding the sol onto clean transparent conductive glass, and spin-coating the transparent conductive glass at the speed of 1000-1500 revolutions per minute;
(4) after the spin coating is finished, immediately attaching the polydimethylsiloxane film with the grating patterning obtained in the step (1) to the coating film coated with TiO2Applying 150 pascal pressure on transparent conductive glass of the sol; then drying the mixture in a drying oven at the temperature of between 60 and 80 ℃ for 1.5 to 2 hours, and naturally cooling the mixture to room temperature;
(5) uncovering the polydimethylsiloxane film with the grating pattern attached to the transparent conductive glass, and putting the transparent conductive glass into a muffle furnace for annealing at 450-550 ℃ for 2-3 hours to obtain the titanium dioxide film with the grating structure.
And (3) putting the clean transparent conductive glass in an ultrasonic cleaning machine, respectively washing the transparent conductive glass with deionized water, acetone and absolute ethyl alcohol for 30 minutes to remove impurities on the surface of the transparent conductive glass, and drying after cleaning to obtain the clean transparent conductive glass.
The titanium dioxide film with the grating structure is prepared by the method.
The titanium dioxide film with the grating structure is applied to the field of solar cells as the anode of the solar cells.
Compared with the prior art, the invention has the following advantages and effects:
(1) the method has the advantages of simple process operation, short sample preparation time, high repeatability and no need of introducing harsh vacuum environment conditions such as special gas and the like; the required equipment is simple, the cost is low, and the mass production can be directly realized.
(2) The TiO2 film prepared by the invention can be applied to the field of solar cells, and the TiO2 film with the grating structure can improve the lighting effect of the solar cells and is beneficial to charge extraction, thereby improving the efficiency of the solar cells.
Drawings
FIG. 1 is a diagram showing the preparation of TiO with a grating structure2Flow chart of the film.
FIG. 2 is a diagram showing the preparation of TiO with a grating structure according to example 12The structure of the film is shown schematically.
FIGS. 3 and 4 are views for preparing TiO with a grating structure according to example 12Surface secondary electron microstructure photographs of the films.
FIG. 5 shows a TiO with a grating structure2Reflectance spectrum profile of the film.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The raw materials used in the following examples are all commercially available or self-made.
Example 1
1. The protective layer above the polycarbonate disc layer of the unrecorded DVD disc was removed, then washed with absolute ethanol in an ultrasonic washer, and after drying, dow corning 184 was mixed with a base: curing agent 10: 1 mass ratio, then casting the mixture on a polycarbonate disc layer of a DVD optical disc, degassing the mixture in a vacuum drying oven at 60 ℃ and curing the mixture for 2 hours; the polydimethylsiloxane film with the grating pattern was then peeled off from the DVD disk.
2. And (3) putting the transparent conductive glass into an ultrasonic cleaning machine, respectively washing the transparent conductive glass with deionized water, acetone and absolute ethyl alcohol for 30 minutes to remove impurities on the surface of the transparent conductive glass, and drying after cleaning to obtain clean transparent conductive glass.
3. Dropwise adding 12mL of absolute ethyl alcohol, 1mL of triethanolamine and 3mL of tetrabutyl titanate into a beaker in sequence, and fully stirring for 20 minutes; then, 1mL of deionized water is added into the mixed solution dropwise, and the mixed solution is fully stirred for 30 minutes to obtain stable, uniform, clear and transparent lightYellow TiO2And (3) sol.
4. Adding 100 μ L of TiO obtained in step 32And (3) dropwise adding the sol on the clean transparent conductive glass obtained in the step (2), and spin-coating the sol on the transparent conductive glass at the speed of 1000 revolutions per minute.
5. After the spin coating is finished, quickly attaching the polydimethylsiloxane film with the grating patterning obtained in the step 1 to the transparent conductive glass, and applying a pressure of 150 pascals; then the mixture is dried in a drying oven at 60 ℃ for 2 hours and naturally cooled to room temperature.
6. Lightly uncovering the polydimethylsiloxane film with the grating patterning attached to the transparent conductive glass, then putting the transparent conductive glass into a muffle furnace at 550 ℃, and annealing for 2 hours to obtain the TiO film with the grating structure2A film of (2).
The flow chart of the above steps is shown in fig. 1.
The prepared sample successfully replicated the structure of a DVD disc, as shown in fig. 3 and 4.
The structure of the obtained sample is shown in FIG. 2, and the TiO with the grating structure of the invention2The film is suitable for amorphous silicon solar cells, inorganic compound semiconductor thin film solar cells, organic thin film solar cells, perovskite solar cells and the like, and the light incidence direction 1 and the TiO ion incidence direction are sequentially from top to bottom2Layer 2, transparent conductive glass substrate 3.
Subjecting the embossed TiO to a treatment2Film and non-embossed TiO2The film was subjected to a reflectance test, and the results are shown in FIG. 5.
Example 2
1. The protective layer above the polycarbonate disc layer of the unrecorded DVD disc was removed, then washed with absolute ethanol in an ultrasonic washer, and after drying, dow corning 184 was mixed with a base: curing agent 10: 1 mass ratio, then casting the mixture on a polycarbonate disc layer of a DVD optical disc, degassing the mixture in a vacuum drying oven at 60 ℃ and curing the mixture for 2 hours; the polydimethylsiloxane film with the grating pattern was then peeled off from the DVD disk.
2. And (3) putting the transparent conductive glass into an ultrasonic cleaning machine, respectively washing the transparent conductive glass with deionized water, acetone and absolute ethyl alcohol for 30 minutes to remove impurities on the surface of the transparent conductive glass, and drying after cleaning to obtain clean transparent conductive glass.
3. 24mL of absolute ethyl alcohol, 2mL of triethanolamine and 6mL of tetrabutyl titanate are sequentially dripped into a beaker and fully stirred for 30 minutes; then 2mL of deionized water is dripped into the mixed solution and fully stirred for 30 minutes to obtain stable, uniform, clear and transparent faint yellow TiO2And (3) sol.
4. Adding 100 μ L of TiO obtained in step 32And (3) dropwise adding the sol on the clean transparent conductive glass obtained in the step (2), and spin-coating the sol on the transparent conductive glass at the speed of 1500 revolutions per minute.
5. After the spin coating is finished, quickly attaching the polydimethylsiloxane film with the grating patterning obtained in the step 1 to the transparent conductive glass, and applying a pressure of 150 pascals; then the mixture is dried in a drying oven at 70 ℃ for 1.5 hours and naturally cooled to room temperature.
6. Lightly uncovering the polydimethylsiloxane film with the grating patterning attached to the transparent conductive glass, then putting the transparent conductive glass into a muffle furnace at 500 ℃ for annealing for 2 hours to obtain the TiO film with the grating structure2A film of (2).
Example 3
1. The protective layer above the polycarbonate disc layer of the unrecorded DVD disc was removed, then washed with absolute ethanol in an ultrasonic washer, and after drying, dow corning 184 was mixed with a base: curing agent 10: 1 mass ratio, then casting the mixture on a polycarbonate disc layer of a DVD optical disc, degassing the mixture in a vacuum drying oven at 70 ℃ and curing the mixture for 1.5 hours; the polydimethylsiloxane film with the grating pattern was then peeled off from the DVD disk.
2. The transparent conductive glass is placed in an ultrasonic cleaning machine and washed with deionized water, acetone and absolute ethyl alcohol for 30 minutes respectively to remove impurities on the surface of the transparent conductive glass. And (5) drying after cleaning. Obtaining clean transparent conductive glass.
3. Will 12Dropwise adding 1mL of triethanolamine and 3mL of tetrabutyl titanate into a beaker in sequence, and fully stirring for 20 minutes; then, 1mL of deionized water is added into the mixed solution dropwise, and the mixed solution is fully stirred for 30 minutes to obtain stable, uniform, clear and transparent faint yellow TiO2And (3) sol.
4. 80 μ L of TiO obtained in step 32And (3) dropwise adding the sol on the clean transparent conductive glass obtained in the step (2), and spin-coating the sol on the transparent conductive glass at the speed of 1200 revolutions per minute.
5. After the spin coating is finished, quickly attaching the polydimethylsiloxane film with the grating patterning obtained in the step 1 to the transparent conductive glass, and applying a pressure of 150 pascals; then the mixture is dried in a drying oven at 80 ℃ for 1.5 hours and naturally cooled to room temperature.
6. Lightly uncovering the polydimethylsiloxane film with the grating patterning attached to the transparent conductive glass, then putting the transparent conductive glass into a muffle furnace at 500 ℃ for annealing for 3 hours to obtain the TiO film with the grating structure2A film of (2).
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. A method for preparing a titanium dioxide film with a grating structure by utilizing a DVD optical disk is characterized by comprising the following steps:
(1) removing the protective layer above the polycarbonate disc layer of the unrecorded DVD disc, washing with absolute ethyl alcohol in an ultrasonic cleaning machine, and drying for later use; mixing the following components in a mass ratio of 10: 1, mixing and stirring uniformly the Dow Corning 184 and the curing agent, casting the mixture on a polycarbonate disc layer of a DVD optical disc, degassing the mixture in a vacuum drying oven at the temperature of between 60 and 80 ℃, and curing the mixture for 1.5 to 2 hours; then stripping the polydimethylsiloxane film with the grating pattern from the DVD optical disk;
(2) dropwise adding absolute ethyl alcohol, triethanolamine and tetrabutyl titanate into a beaker in sequence, and fully stirring for 15-30 minutes; then, deionized water is dripped into the mixed solution, and the mixed solution is fully stirred for 15-30 minutes to obtain TiO2Sol; the volume ratio of the absolute ethyl alcohol to the triethanolamine to the tetrabutyl titanate to the deionized water is 12: 1: 3: 1;
(3) 80-120 mu L of TiO obtained in the step (2)2Dropwise adding the sol onto clean transparent conductive glass, and spin-coating the transparent conductive glass at the speed of 1000-1500 revolutions per minute;
(4) after the spin coating is finished, immediately attaching the polydimethylsiloxane film with the grating patterning obtained in the step (1) to the coating film coated with TiO2Applying 150 pascal pressure on transparent conductive glass of the sol; then drying the mixture in a drying oven at the temperature of between 60 and 80 ℃ for 1.5 to 2 hours, and naturally cooling the mixture to room temperature;
(5) uncovering the polydimethylsiloxane film with the grating pattern attached to the transparent conductive glass, and putting the transparent conductive glass into a muffle furnace for annealing at 450-550 ℃ for 2-3 hours to obtain the titanium dioxide film with the grating structure.
2. The method of claim 1, wherein: and (3) putting the clean transparent conductive glass in an ultrasonic cleaning machine, respectively washing the transparent conductive glass with deionized water, acetone and absolute ethyl alcohol for 30 minutes to remove impurities on the surface of the transparent conductive glass, and drying after cleaning to obtain the clean transparent conductive glass.
3. A titanium dioxide thin film having a grating structure produced by the method of claim 1 or 2.
4. The use of the titanium dioxide thin film with the grating structure according to claim 3 as an anode of a solar cell in the field of solar cells.
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Application publication date: 20211203 |