LU501287B1 - METHOD FOR PREPARING POROUS TiO2 NANOCELLULOSE NETWORK COMPOSITE FILM THROUGH IN-SITU GROWTH - Google Patents
METHOD FOR PREPARING POROUS TiO2 NANOCELLULOSE NETWORK COMPOSITE FILM THROUGH IN-SITU GROWTH Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
- C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
Abstract
A method for preparing a porous TiO2 nanocellulose network composite film through in-situ growth, including the following steps: S1: incubating TiO2 at 450°C to 550°C for 2 h to 4 h, and cooling naturally; S2: subjecting a nanocellulose suspension to vacuum filtration and drying to obtain a nanocellulose film, and subjecting the nanocellulose film to magnetron sputtering in a magnetron sputtering device with the TiO2 obtained in S1 as a target; S3: after S2 is completed, replacing the target in the magnetron sputtering device with metallic titanium, and conducting magnetron sputtering once again to obtain a semi-finished composite film; and S4: subjecting the semi-finished composite film to anodic oxidation as an anode, washing an obtained sample with deionized water, and naturally drying the sample to obtain a finished product. The present disclosure can integrate a TiO2 material with nanocellulose, which improves the semiconductor material performance of a finished product.
Description
METHOD FOR PREPARING POROUS TiO2 NANOCELLULOSE NETWORK 17001887 COMPOSITE FILM THROUGH IN-SITU GROWTH
TECHNICAL FIELD The present disclosure relates to the field of semiconductor materials, and in particular to a method for preparing a porous TiO» nanocellulose network composite film through in-situ growth.
BACKGROUND With the development of modern industrial technologies, global environmental problems have become increasingly prominent, and more and more attention has been paid to the detection and treatment technologies for pollution components in the environment. Nano-titanium dioxide (TiO») has become one of the most popular semiconductor materials due to its advantages such as excellent photocatalytic activity, gas sensitivity, and no secondary pollution. In addition, with a large specific surface area (SSA) and a special surface morphology, porous irregular TiO» nanotubes are bound to improve photocatalytic activity and bring more possibilities. In particular, with the current rapid development of flexible devices, how to obtain flexible functional materials based on ensuring the characteristics of nano-TiO» materials is an urgent problem to be solved.
Nanocellulose itself has prominent biocompatibility, renewability, biodegradability, and mechanical performance, in which fibers are connected with each other in an interleaved manner and are easy to form a porous structure that facilitates the transmission of ions and electrons. Therefore, from the perspective of environmental protection and high-value utilization of renewable resources, it is an effective research direction to develop and use environment-friendly, renewable flexible functional composite film materials prepared with nanocellulose as a raw material.
However, a semiconductor material currently used for photocatalysis or sensitive performance analysis is processed on a substrate material by coating, and this method cannot make the catalytic material and the flexible substrate material tightly combined, which hinders the preparation and use of nano-TiO» materials.
SUMMARY The present disclosure is intended to provide a method for preparing a porous TiO; nanocellulose network composite film through in-situ growth. The present disclosure can integrate a TiO; material with nanocellulose, which improves the semiconductor material performance of a finished product.
To solve the above technical problem, the present disclosure provides the following technical solution: A method for preparing a porous TiO» nanocellulose network composite fm 2 through in-situ growth is provided, including the following steps: S1: incubating TiO; at 450°C to 550°C for 2 h to 4 h, and cooling naturally; S2: subjecting a nanocellulose suspension to vacuum filtration and drying to obtain a nanocellulose film, and subjecting the nanocellulose film to magnetron sputtering in a magnetron sputtering device with the TiO, obtained in S1 as a target; S3: after S2 is completed, replacing the target in the magnetron sputtering device with metallic titanium, and conducting magnetron sputtering once again to obtain a semi-finished composite film; and S4: connecting the semi-finished composite film as an anode to a positive pole of a power supply for an oxidation treatment, washing an obtained sample with deionized water, and naturally drying the sample to obtain a finished product.
For the method for preparing a porous TiO, nanocellulose network composite film through in-situ growth, in S2, the nanocellulose suspension may have a concentration of 0.05% to 0.3%.
For the method for preparing a porous TiO, nanocellulose network composite film through in-situ growth, when the TiO, is used as a target for magnetron sputtering, argon may be introduced as a working gas, and the magnetron sputtering may be conducted for 30 min to 2 h at a sputtering power of 150 W to 350 W.
For the method for preparing a porous TiO, nanocellulose network composite film through in-situ growth, in S3, argon may be introduced as a working gas, and the magnetron sputtering may be conducted for 90 s to 450 s at a sputtering power of 50 W to 100 W.
For the method for preparing a porous TiO, nanocellulose network composite film through in-situ growth, in S4, the semi-finished composite film may be connected as an anode to the positive pole of the power supply, a platinum electrode may be connected as a cathode to a negative pole, a distance between the two poles may be 2.0 cm to 3.0 cm, and an ethylene glycol (EG) solution with 0.5 wt% to 0.6 wt% ammonium fluoride and 20 wt% to 30 wt% deionized water may be used as an electrolyte; and at room temperature, the anode may be oxidized for 10 min to 60 min at 15 V to 30 V.
Compared with the prior art, in the present disclosure, titanium dioxide is first incubated in a high-temperature environment and then cooled, which can prevent the titanium dioxide as a target from cracking; the titanium dioxide target and the metallic titanium target are uniformly sputtered onto the nanocellulose film through magnetron sputtering; and a resulting product is subjected to anodic oxidation to obtain a finished product. In the present disclosure, a nanoporous structure is constructed through the crosslinking characteristics of nanocellulose and the in-situ growth of TiO; to simply and quickly prepare an integrated flexible composite film material, which not only improves the performance of the flexible composite film material asa 201287 semiconductor material, but also promotes the use of the composite film material in flexible wearable devices. The present disclosure can also be widely used in the field of environmental protection research.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a scanning electron microscopy (SEM) top view of the porous TiO» nanocellulose network composite film; FIG. 2 is an SEM side view of the porous TiO, nanocellulose network composite film; and FIG. 3 is an X-ray diffractometry (XRD) pattern of the porous TiO; nanocellulose network composite film.
DETAILED DESCRIPTION OF THE EMBODIMENTS The present disclosure will be further described below in conjunction with examples and accompanying drawings, but it should not be used as a basis for limiting the present disclosure.
Example 1: A method for preparing a porous TiO, nanocellulose network composite film through in-situ growth was provided, including the following steps: S1. A TiO; target with a purity of 99.99% was placed in a muffle furnace, then the muffle furnace was heated to 450°C and kept at the temperature for 2 h, and the target was cooled with the furnace, thereby preventing the target from cracking.
S2. 100 mL of a nanocellulose suspension with a concentration of 0.1% was subjected to vacuum filtration and drying to obtain a nanocellulose film, and then the nanocellulose film was subjected to magnetron sputtering for 2 h at a sputtering power of 300 W in a magnetron sputtering device with the TiO, obtained after the annealing treatment in S1 as a target to obtain a raw material for preparing a nanoporous material, where pure argon was introduced into the vacuum chamber during the magnetron sputtering.
S3. After S2 was completed, the target in the magnetron sputtering device was replaced by a metallic titanium target with a purity of 99.99%, and then the material obtained in S2 was further subjected to magnetron sputtering for 450 s at a sputtering power of 100 W to obtain a semi-finished composite film, where pure argon was introduced into the vacuum chamber during the magnetron sputtering. A layer of metallic titanium is sputtered for the smooth progress of an anodic oxidation process in S4, because the metallic titanium is conductive and thus enables the formation of an electrical circuit between the two poles to start the anodic oxidation process. The metallic titanium is oxidized into titanium dioxide, and in the subsequent anodic oxidation process, the titanium dioxide in S2 serves as a raw material and grows in-situ on the nanocellulose film to form nanoporous titanium dioxide.
S4. The semi-finished composite film obtained in S3 was connected as an anode to a positive pole of a power supply, a platinum electrode was connected as a cathode to a negative 201287 pole, a distance between the two poles was 2.0 cm, and an EG solution with 0.5 wt% ammonium fluoride and 20 wt% deionized water was used as an electrolyte; at room temperature, the anode was oxidized for 60 min at 30 V; and after the oxidation was completed, a prepared sample was washed with deionized water and dried naturally to obtain a flexible porous TiO; nanocellulose network composite film with a thickness of 40 um.
As shown in the SEM top view of FIG. 1 and the SEM side view of FIG. 2, the flexible porous TiO; nanocellulose network composite film has densely-arranged honeycomb porous TiO; growing on the surface and has a layered structure, and the TiO; has an average pore size of 80 nm.
Example 2: A method for preparing a porous TiO, nanocellulose network composite film through in-situ growth was provided, including the following steps: S1. A TiO; target with a purity of 99.99% was placed in a muffle furnace, then the muffle furnace was heated to 450°C and kept at the temperature for 2 h, and the target was cooled with the furnace, thereby preventing the target from cracking.
S2. 100 mL of a nanocellulose suspension with a concentration of 0.1% was subjected to vacuum filtration and drying to obtain a nanocellulose film, and then the nanocellulose film was subjected to magnetron sputtering for 1 h at a sputtering power of 300 W in a magnetron sputtering device with the TiO, obtained after the annealing treatment in S1 as a target, where pure argon was introduced into the vacuum chamber during the magnetron sputtering.
S3. After S2 was completed, the target in the magnetron sputtering device was replaced by a metallic titanium target with a purity of 99.99%, and then the material obtained in S2 was further subjected to magnetron sputtering for 450 s at a sputtering power of 100 W to obtain a semi-finished composite film, where pure argon was introduced into the vacuum chamber during the magnetron sputtering.
S4. The semi-finished composite film obtained in S3 was connected as an anode to a positive pole of a power supply, a platinum electrode was connected as a cathode to a negative pole, a distance between the two poles was 2.5 cm, and an EG solution with 0.5 wt% ammonium fluoride and 20 wt% deionized water was used as an electrolyte; at room temperature, the anode was oxidized for 60 min at 20 V; and after the oxidation was completed, a prepared sample was washed with deionized water and dried naturally to obtain a flexible porous TiO; nanocellulose network composite film with a thickness of 40 um.
According to test results, the flexible porous TiO, nanocellulose network composite film has honeycomb porous TiO; on the surface, and the TiO has an average pore size of 70 nm.
Example 3: A method for preparing a porous TiO, nanocellulose network composite film through in-situ growth was provided, including the following steps: 501267 S1. A TiO; target with a purity of 99.99% was placed in a muffle furnace, then the muffle furnace was heated to 500°C and kept at the temperature for 3 h, and the target was cooled with the furnace, thereby preventing the target from cracking.
S2. 200 mL of a nanocellulose suspension with a concentration of 0.1% was subjected to vacuum filtration and drying to obtain a nanocellulose film, and then the nanocellulose film was subjected to magnetron sputtering for 1 h at a sputtering power of 200W in a magnetron sputtering device with the TiO, obtained after the annealing treatment in S1 as a target, where pure argon was introduced into the vacuum chamber during the magnetron sputtering.
S3. After S2 was completed, the target in the magnetron sputtering device was replaced by a metallic titanium target with a purity of 99.99%, and then the material obtained in S2 was further subjected to magnetron sputtering for 350 s at a sputtering power of 100 W to obtain a semi-finished composite film, where pure argon was introduced into the vacuum chamber during the magnetron sputtering.
S4. The semi-finished composite film obtained in S3 was connected as an anode to a positive pole of a power supply, a platinum electrode was connected as a cathode to a negative pole, a distance between the two poles was 2.5 cm, and an EG solution with 0.6 wt% ammonium fluoride and 25 wt% deionized water was used as an electrolyte; at room temperature, the anode was oxidized for 30 min at 15 V; and after the oxidation was completed, a prepared sample was washed with deionized water and dried naturally to obtain a flexible porous TiO; nanocellulose network composite film with a thickness of 50 um.
According to test results, the flexible porous TiO, nanocellulose network composite film has honeycomb porous TiO, and the TiO; has an average pore size of 65 nm.
Example 4: A method for preparing a porous TiO, nanocellulose network composite film through in-situ growth was provided, including the following steps: S1. A TiO; target with a purity of 99.99% was placed in a muffle furnace, then the muffle furnace was heated to 550°C and kept at the temperature for 4 h, and the target was cooled with the furnace, thereby preventing the target from cracking.
S2. 100 mL of a nanocellulose suspension with a concentration of 0.2% was subjected to vacuum filtration and drying to obtain a nanocellulose film, and then the nanocellulose film was subjected to magnetron sputtering for 1 h at a sputtering power of 300 W in a magnetron sputtering device with the TiO, obtained after the annealing treatment in S1 as a target, where pure argon was introduced into the vacuum chamber during the magnetron sputtering.
S3. After S2 was completed, the target in the magnetron sputtering device was replaced by a metallic titanium target with a purity of 99.99%, and then the material obtained in S2 was further subjected to magnetron sputtering for 450 s at a sputtering power of 100 W to obtain à 201287 semi-finished composite film, where pure argon was introduced into the vacuum chamber during the magnetron sputtering.
S4. The composite film obtained in S3 was connected to a positive pole of a power supply, a platinum electrode was connected to a negative pole, a distance between the two poles was 2.5 cm, and an EG solution with 0.5 wt% ammonium fluoride and 30 wt% deionized water was used as an electrolyte; at room temperature, the anode was oxidized for 60 min at 15 V; and after the oxidation was completed, a prepared sample was washed with deionized water and dried naturally to obtain a flexible porous TiO, nanocellulose network composite film with a thickness of 50 um.
According to test results, the flexible porous TiO, nanocellulose network composite film has honeycomb porous TiO, and the TiO; has an average pore size of 70 nm.
Further, the applicants conducted XDR on the flexible porous TiO, nanocellulose network composite film prepared in Example 1 to obtain the XRD pattern of the flexible porous TiO» nanocellulose network composite film, as shown in FIG. 3. It can be seen from FIG. 3 that, in the curve, in addition to the diffraction peaks of nanocellulose (16° and 22°), diffraction peaks of the anatase phase TiO, appear around 25°, 38°, 48°, 55° and 63°, which is consistent with the standard card of the anatase phase TiO». It indicates that the flexible porous TiO, nanocellulose network composite film prepared by the method of the present disclosure includes both a nanocellulose crystal and an anatase phase TiO, crystal. It can be known that, in the present disclosure, a nanoporous structure is constructed through the crosslinking characteristics of nanocellulose and the in-situ growth of TiO; to simply and quickly prepare an integrated flexible composite film material, which not only improves the performance of the flexible composite film material as a semiconductor material, but also promotes the use of the composite film material in flexible wearable devices. The present disclosure can also be widely used in the field of environmental protection research.
Claims (5)
1. A method for preparing a porous TiO, nanocellulose network composite film through in-situ growth, comprising the following steps: S1: incubating TiO; at 450°C to 550°C for 2 h to 4 h, and cooling naturally; S2: subjecting a nanocellulose suspension to vacuum filtration and drying to obtain a nanocellulose film, and subjecting the nanocellulose film to magnetron sputtering in a magnetron sputtering device with the TiO, obtained in S1 as a target; S3: after S2 is completed, replacing the target in the magnetron sputtering device with metallic titanium, and conducting magnetron sputtering once again to obtain a semi-finished composite film; and S4: connecting the semi-finished composite film as an anode to a positive pole of a power supply for an oxidation treatment, washing an obtained sample with deionized water, and naturally drying the sample to obtain a finished product.
2. The method for preparing a porous TiO, nanocellulose network composite film through in-situ growth according to claim 1, wherein in S2, the nanocellulose suspension has a concentration of 0.05% to 0.3%.
3. The method for preparing a porous TiO; nanocellulose network composite film through in-situ growth according to claim 1, wherein when the TiO; is used as a target for magnetron sputtering, argon is introduced as a working gas, and the magnetron sputtering is conducted for min to 2 h at a sputtering power of 150 W to 350 W.
4. The method for preparing a porous TiO, nanocellulose network composite film through in-situ growth according to claim 1, wherein in S3, argon is introduced as a working gas, and the magnetron sputtering is conducted for 90 s to 450 s at a sputtering power of 50 W to 100 W.
5. The method for preparing a porous TiO, nanocellulose network composite film through in-situ growth according to claim 1, wherein in S4, the semi-finished composite film is connected as an anode to the positive pole of the power supply, a platinum electrode is connected as a cathode to a negative pole, a distance between the two poles is 2.0 cm to 3.0 cm, and an ethylene glycol (EG) solution with 0.5 wt% to 0.6 wt% ammonium fluoride and 20 wt% to 30 wt% deionized water is used as an electrolyte; and at room temperature, the anode is oxidized for 10 min to 60 min at 15 V to 30 V.
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| JP2007224370A (en) * | 2006-02-24 | 2007-09-06 | National Institute For Materials Science | MANUFACTURING METHOD OF TiO2 SPUTTER COATING FILM |
| CN100554521C (en) * | 2008-05-29 | 2009-10-28 | 南京航空航天大学 | The room temperature preparation method of titania nanotube combined electrode |
| CN101892460A (en) * | 2010-06-22 | 2010-11-24 | 浙江大学 | Method for preparing titanium dioxide porous membrane |
| CN102623186B (en) * | 2012-04-01 | 2015-05-13 | 东华大学 | Titanium-foil-based flexible dye-sensitized solar cell and preparation method thereof |
| CN106498478B (en) * | 2016-11-22 | 2019-05-14 | 华南理工大学 | A kind of preparation method of transparent independent titanium dioxide nano-pipe array thin film |
| CN112630181B (en) * | 2020-12-15 | 2024-03-22 | 浙江科技学院 | Preparation method of ultraviolet light excited nanocellulose flexible gas sensor |
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