CN111188082A - Preparation method and application of 4H-SiC integrated self-supporting photo-anode - Google Patents
Preparation method and application of 4H-SiC integrated self-supporting photo-anode Download PDFInfo
- Publication number
- CN111188082A CN111188082A CN202010071042.XA CN202010071042A CN111188082A CN 111188082 A CN111188082 A CN 111188082A CN 202010071042 A CN202010071042 A CN 202010071042A CN 111188082 A CN111188082 A CN 111188082A
- Authority
- CN
- China
- Prior art keywords
- sic
- supporting
- etching
- photoanode
- integrated self
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/12—Etching of semiconducting materials
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
- C25B1/55—Photoelectrolysis
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
-
- 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
- C25D11/32—Anodisation of semiconducting materials
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Weting (AREA)
Abstract
The invention relates to a preparation method and application of a 4H-SiC integrated self-supporting photo-anode, belonging to the technical field of photoelectrocatalysis. The preparation method of the 4H-SiC integrated self-supporting photo-anode comprises the following steps: s1, cleaning the 4H-SiC single crystal wafer; s2, taking the cleaned 4H-SiC single crystal wafer as an anode and the graphite wafer as a cathode, and carrying out anodic oxidation etching in etching liquid, wherein the anodic oxidation etching sequentially comprises cap layer removing etching and continuous periodic etching to obtain a photo-anode semi-finished product; and S3, cleaning and drying the photo-anode semi-finished product to obtain the 4H-SiC integrated self-supporting photo-anode. The self-supporting photoanode provided by the invention has an extremely low initial potential for photolytic water and a high photocurrent density for water decomposition.
Description
Technical Field
The invention belongs to the technical field of photoelectrocatalysis, and relates to a preparation method and application of a 4H-SiC integrated self-supporting photo-anode.
Background
The increasing exhaustion of energy and the greenhouse effect and extreme climate caused by the exhaustion become serious problems threatening the survival and sustainable development of human beings in the 21 st century or the future, and the search for clean energy which can replace the traditional high-pollution non-renewable energy is an especially important solution, and the research on the use of nano materials as catalysts and carriers of clean energy is not earnestly made. Since the discovery of carbon nanotubes by professor Iijima in 1991, the science of nano-material preparation and the application of devices thereof have been the focus and hot point of research in nanotechnology, and are an effective system for researching the correlation between the electrical, thermal and mechanical properties of materials and the dimension and quantum confinement effect, thus opening a new gate for the research and development of novel, efficient, energy-saving and environment-friendly photoelectric devices.
The photoelectrochemical decomposition of water to produce oxygen and hydrogen has attracted considerable attention since its introduction as a green clean energy source. The photochemical reaction of titanium dioxide as a photocatalyst material has been well known as early as 50 in the 20 th century, but the present poly-tenuadao effect, which has been reported by Nature as a catalyst for the photodecomposition of water, has not attracted much attention by many scientists until 1972. As a third generation semiconductor of great interest, nano-silicon carbide materials have many excellent characteristics, such as wide band gap, good chemical stability and thermal stability. Meanwhile, the SiC nano material also has the excellent characteristics of high hardness, toughness, wear resistance, low thermal expansion coefficient and the like. Based on the excellent physical and chemical properties of the SiC nanostructure, Nariki et al reported the catalytic properties of SiC ultrafine powder as a visible light response type photocatalyst in 1990, and the third generation of semiconductor material SiC was actively studied in the field of photocatalysis by performing photocatalytic electrolysis of water by irradiation of ultraviolet light.
However, although some work has been devoted to the research and progress of the SiC nanostructure photocatalysts, several fundamental problems still exist in the material preparation science in the current field, which need to be researched and solved: firstly, the preparation of the SiC nano array structure is exposed to harsh growth process conditions such as high temperature, special atmosphere and the like; secondly, most of the photo-anode materials for the research of photoelectrocatalysis are powder or block, and few self-supporting photo-anodes are researched; thirdly, the preparation of the photo-anode is mostly realized by attaching a catalyst on a current collector, the loss of a contact interface to the carrier transmission is difficult to ignore, and an integrated electrode is rarely reported; fourthly, the initial potential of the photoanode decomposed water is higher to block the further promotion of the photocatalytic efficiency of the photolysis of water.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a 4H-SiC integrated self-supporting photoanode with excellent photoelectrocatalysis performance.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a 4H-SiC integrated self-supporting photo-anode comprises the following steps:
s1, cleaning the 4H-SiC single crystal wafer;
s2, taking the cleaned 4H-SiC single crystal wafer as an anode and the graphite wafer as a cathode, and carrying out anodic oxidation etching in etching liquid, wherein the anodic oxidation etching sequentially comprises cap layer removing etching and continuous periodic etching to obtain a photo-anode semi-finished product;
and S3, cleaning and drying the photo-anode semi-finished product to obtain the 4H-SiC integrated self-supporting photo-anode.
Preferably, in the step S1, the 4H-SiC single crystal wafer is cleaned by ultrasonic cleaning with acetone, absolute ethyl alcohol and deionized water for 15-25 min.
Preferably, the anodic oxidation etching in step S2 uses a dc power analyzer as an electrochemical etching power source.
Preferably, the cap layer removing etching in the step S2 sequentially includes a pulse etching stage and a constant voltage stripping stage, the pulse etching stage applies a pulse voltage with a period of 0.7-0.9S, a retention time of 0.3-0.5S and a voltage of 19-21V for a duration of 0.8-0.9 min, and the constant voltage stripping stage applies a constant voltage of 28-32V for a duration of 0.1-0.2 min.
Preferably, in the step S2, the continuous periodic etching is performed with a pulse voltage with a period of 0.7-0.9S, a dwell time of 0.3-0.5S, and a voltage of 18-20V, and the duration time is 4-13 min.
Preferably, in the step S2, the etching solution is C with a volume ratio of (5-7): 12H5OH, HF and H2O2The mixed solution of (1).
Preferably, in step S3, the cleaning of the photo-anode semi-finished product is performed by respectively using anhydrous ethanol and deionized water.
Preferably, the drying in step S3 is constant temperature drying at 50-70 ℃ for 3-7 min.
The invention also aims to provide the 4H-SiC integrated self-supporting photoanode prepared by the preparation method, wherein the 4H-SiC integrated self-supporting photoanode is provided with a uniform 4H-SiC monocrystal highly-oriented nano hole array, the aperture is 20-70 nm, and the depth is 13-25 mu m.
The invention further aims to provide application of the 4H-SiC integrated self-supporting photo-anode in photoelectrocatalysis.
The invention adopts the 4H-SiC single crystal wafer as the matrix under normal temperature and pressure, prepares the SiC nano array integrated self-supporting photoanode by a chemical etching method, realizes the controllable preparation of the dimension, the appearance, the size, the crystal growth direction, the density and the like of the 4H-SiC etching layer by the controllable adjustment of the parameters of a power supply analyzer, has very mild preparation conditions, better reserves the single crystal structure of the 4H-SiC single crystal wafer, effectively reserves the original single crystal wafer form by the top-down preparation method of the direct current power supply analyzer, is beneficial to the directional transmission of electron-hole pairs by the 4H-SiC single crystal highly directional nano array, not only can exert the advantages of the single crystal structure, but also exert the high electron-hole transmission rate of the 4H-SiC, effectively reduces the loss and the recombination of electron holes in the transmission process, and further, the photoelectrocatalysis efficiency of the 4H-SiC integrated self-supporting photoanode is effectively improved, so that the prepared 4H-SiC integrated self-supporting photoanode can show higher photoelectrocatalysis activity at a lower initial potential, and possibility and support are provided for solving the severe energy and environmental problems faced by human beings.
The SiC nano array generates a non-nano hole structure layer at the initial stage of the anodic oxidation etching process, namely a cap covers the surface layer, so the SiC nano array is called a cap layer, and the cap layer needs to be stripped off to expose the following continuous periodically etched nano hole array structure so as to better play the role of the nano hole array structure. When the cap layer is stripped, higher constant voltage treatment is needed after pulse voltage etching so as to improve the etching speed and further facilitate the stripping of the cap layer, and the cap layer cannot be stripped when the voltage is too low during the constant voltage treatment.
Compared with the prior art, the invention has the following beneficial effects: the 4H-SiC photoanode prepared by the invention is an integrated electrode, has self-supporting performance, has extremely low initial potential of water photolysis and higher photocurrent density of water photolysis, and is expected to become an excellent candidate material of the photoelectrode in catalytic reaction of water photolysis.
Drawings
FIG. 1 is a digital photograph of a 4H-SiC integrated self-supporting photoanode prepared in the first embodiment of the present invention;
FIG. 2 is a surface Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode prepared in the first embodiment of the invention;
FIG. 3 is a cross-sectional Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode prepared in the first example of the invention;
FIG. 4 is an X-ray powder diffraction (XRD) pattern of a 4H-SiC photoanode made in accordance with a first embodiment of the present invention;
FIG. 5 is a graph of a linear voltammetry scan (LSV) of a 4H-SiC photoanode made in a first example of the invention;
FIG. 6 is a surface Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode prepared in example two of the present invention;
FIG. 7 is a cross-sectional Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode prepared in example two of the present invention;
FIG. 8 is a graph of the linear voltammetry scan (LSV) of a 4H-SiC photoanode made in example two of the present invention;
FIG. 9 is a surface Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode prepared in example III of the present invention;
FIG. 10 is a cross-sectional Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode prepared in example III of the present invention;
FIG. 11 is a plot of the linear voltammetry scan (LSV) of a 4H-SiC photoanode made in example III of the present invention;
FIG. 12 is a surface Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode prepared in example four of the present invention;
FIG. 13 is a cross-sectional Scanning Electron Microscope (SEM) image of a 4H-SiC photoanode made in example four of the present invention;
fig. 14 is a graph of linear voltammetry scan (LSV) of a 4H-SiC photoanode made in example four of the present invention.
Fig. 15 is a graph comparing the linear voltammetry scan curves (LSVs) of 4H-SiC photoanodes prepared in examples one to four of the present invention.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Example 1
The preparation method of the 4H-SiC integrated self-supporting photo-anode in the embodiment comprises the following steps:
firstly, respectively ultrasonically cleaning a 4H-SiC single crystal wafer (a commercial 4H-SiC single crystal wafer purchased from Taiyuan Art Star Co., Ltd.) for 20min by sequentially using acetone, absolute ethyl alcohol and deionized water, then using a direct current power supply analyzer (model KEYSIGHT, N6705B) as an electrochemical etching power supply, using the cleaned 4H-SiC single crystal wafer as an anode and a graphite sheet as a cathode, and performing ultrasonic etching on the wafer C by using a C-shaped substrate2H5OH, HF and H2O2Carrying out anodic oxidation etching on the 4H-SiC single crystal wafer in the uniformly mixed etching solution (volume ratio 6:6: 1); the experimental reagents used were of analytical grade.
The anodic etching process is carried out in two steps:
the first step is to remove the cap layer and etch, firstly applying pulse voltage (T) with the period of 0.8s, the retention time of 0.4s and the voltage of 19V0.8s＝19V0.4s+0V0.4s) Performing cap layer etching for 0.9min, adjusting voltage to 30V, and stripping cap layer at constant voltage of 30V for 0.1min (T)0.8s＝19V0.4s+19V0.4s)；
Immediately thereafter, a second continuous periodic etching was carried out by applying a pulse voltage (T) of 19V with a dwell time of 0.4s and a period of 0.8s0.8s＝19V0.4s+0V0.4s) Etching for 10min to obtain the semi-finished product of the photo-anode.
And after the anode etching is finished, respectively carrying out ultrasonic cleaning on the photo-anode semi-finished product by using absolute ethyl alcohol and deionized water in sequence, and then putting the photo-anode semi-finished product into a constant-temperature drying oven at 60 ℃ for drying for 5min to obtain the 4H-SiC integrated self-supporting photo-anode, wherein a digital photo of the photo-anode is shown in figure 1.
The structure of the 4H-SiC integrated self-supporting photoanode prepared in example 1 is characterized by using a scanning electron microscope (FESEM, S-4800, Hitachi, Japan), and a surface SEM image of the photoanode is shown in FIG. 2, so that the photoanode has a uniform nano-pore structure and the pore diameter is about 50-70 nm; the cross-sectional SEM image is shown in FIG. 3, and it can be seen that the nanohole array etch layer has a depth of about 18.4 μm.
The phase and composition of the 4H-SiC integral self-supporting photoanode prepared in example 1 was characterized using an X-ray powder diffractometer (XRD, D8Advance, Bruker, Germany), whose XRD pattern is shown in fig. 4, indicating that it still retains the composition of the original single-crystal phase structure.
The 4H-SiC integrated self-supporting photoanode prepared in example 1 was subjected to photoelectrocatalysis performance characterization under simulated sunlight irradiation of a xenon lamp by using Chenghua CHI-660D electrochemical workstation, and a linear voltammetry scan curve prepared at a scan speed of 25mV/s is shown in FIG. 5, from which it can be seen from FIG. 5 that the photocurrent density was 2.5mA/cm2The initial potential is 0.019V, which indicates that the 4H-SiC integrated self-supporting photoanode prepared by the embodiment has excellent photoelectrocatalysisAnd (4) performance.
Example 2
The only difference between embodiment 2 and embodiment 1 is that the etching time lasts for 4min when the second step of continuous periodic etching is performed, and the rest is the same as embodiment 1, and will not be described again here.
The structure of the 4H-SiC integrated self-supporting photoanode prepared in example 2 was characterized by using a scanning electron microscope (FESEM, S-4800, Hitachi, Japan), and a surface SEM image thereof is shown in FIG. 6, which shows that the photoanode has a uniform nanopore structure and a pore diameter of about 50-70 nm; the cross-sectional SEM image is shown in FIG. 7, and it can be seen that the nanohole array etch layer has a depth of about 13.3 μm.
The photoelectrocatalysis performance of the xenon lamp is characterized by using Chenghua CHI-660D electrochemical workstation under the simulated sunlight irradiation of the xenon lamp, a linear volt-ampere scanning curve prepared at the scanning speed of 25mV/s is shown in figure 8, and the photo current density of the linear volt-ampere scanning curve is 1.81mA/cm as can be known from figure 82The initial potential is 0.069V, which indicates that the 4H-SiC integrated self-supporting photoanode prepared by the embodiment has excellent photoelectrocatalysis performance.
Example 3
The only difference between embodiment 3 and embodiment 1 is that the etching time lasts for 7min when the second step of continuous periodic etching is performed, and the rest is the same as embodiment 1, and will not be described again here.
The structure of the 4H-SiC integrated self-supporting photoanode prepared in example 3 was characterized by using a scanning electron microscope (FESEM, S-4800, Hitachi, Japan), and a surface SEM image thereof is shown in fig. 9, which shows that the photoanode has a uniform nanopore structure, and the pore diameter is about 50 to 70 nm; the cross-sectional SEM image is shown in FIG. 10, and it can be seen that the nanohole array etch layer has a depth of about 15.5 μm.
Under the irradiation of simulated sunlight of a xenon lamp, a Chenghua CHI-660D electrochemical workstation is used for carrying out photoelectric catalytic performance characterization on the xenon lamp. The linear voltammetric sweep curve obtained at a sweep rate of 25mV/s is shown in FIG. 11. it can be seen from FIG. 11 that the photocurrent density was 1.92mA/cm2And the initial potential is 0.047V, which shows that the 4H-SiC integrated self-supporting photoanode prepared by the embodiment has excellent photoelectrocatalysis performance.
Example 4
The only difference between embodiment 4 and embodiment 1 is that the etching time lasts for 13min when the second step of continuous periodic etching is performed, and the rest is the same as embodiment 1, and will not be described again here.
The structure of the 4H-SiC integrated self-supporting photoanode prepared in example 4 was characterized by using a scanning electron microscope (FESEM, S-4800, Hitachi, Japan), and a surface SEM image thereof is shown in FIG. 12, which shows that the photoanode has a uniform nanopore structure and a pore diameter of about 50-70 nm; the cross-sectional SEM image is shown in FIG. 13, and it can be seen that the nanohole array etch layer has a depth of about 24.5 μm.
Under the irradiation of simulated sunlight of a xenon lamp, a Chenghua CHI-660D electrochemical workstation is used for carrying out photoelectric catalytic performance characterization on the xenon lamp. The linear voltammetric sweep curve obtained at a sweep rate of 25mV/s is shown in FIG. 14, which shows that the photocurrent density is 1.58mA/cm2And the initial potential is 0.025V, which indicates that the 4H-SiC integrated self-supporting photoanode prepared by the embodiment has excellent photoelectrocatalysis performance.
In conclusion, the preparation conditions are mild, and the prepared 4H-SiC integrated self-supporting photoanode shows higher photoelectrocatalysis activity under lower initial potential.
The technical scope of the invention claimed by the embodiments of the present application is not exhaustive, and new technical solutions formed by equivalent replacement of single or multiple technical features in the technical solutions of the embodiments are also within the scope of the invention claimed by the present application; in all the embodiments of the present invention, which are listed or not listed, each parameter in the same embodiment only represents an example (i.e., a feasible embodiment) of the technical solution, and there is no strict matching and limiting relationship between the parameters, wherein the parameters may be replaced with each other without departing from the axiom and the requirements of the present invention, unless otherwise specified.
The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and the technical scheme also comprises the technical scheme formed by any combination of the technical characteristics. While the foregoing is directed to embodiments of the present invention, it will be appreciated by those skilled in the art that various changes may be made in the embodiments without departing from the principles of the invention, and that such changes and modifications are intended to be included within the scope of the invention.
Claims (10)
1. A preparation method of a 4H-SiC integrated self-supporting photo-anode is characterized by comprising the following steps:
s1, cleaning the 4H-SiC single crystal wafer;
s2, taking the cleaned 4H-SiC single crystal wafer as an anode and the graphite wafer as a cathode, and carrying out anodic oxidation etching in etching liquid, wherein the anodic oxidation etching sequentially comprises cap layer removing etching and continuous periodic etching to obtain a photo-anode semi-finished product;
and S3, cleaning and drying the photo-anode semi-finished product to obtain the 4H-SiC integrated self-supporting photo-anode.
2. The method for preparing a 4H-SiC integrated self-supporting photoanode according to claim 1, wherein the step S1 of cleaning the 4H-SiC single crystal wafer is to respectively ultrasonically clean the 4H-SiC single crystal wafer for 15-25 min by sequentially using acetone, absolute ethyl alcohol and deionized water.
3. The method for preparing a 4H-SiC integrated self-supporting photoanode according to claim 1, wherein the anodic oxidation etching in step S2 uses a DC power analyzer as an electrochemical etching power source.
4. The method for preparing a 4H-SiC integrated self-supporting photoanode according to claim 1, wherein the step S2 of removing the cap layer comprises a pulse etching stage and a constant voltage stripping stage in sequence, the pulse etching stage applies a pulse voltage with a period of 0.7-0.9S, a retention time of 0.3-0.5S and a voltage of 19-21V for a duration of 0.8-0.9 min, and the constant voltage stripping stage applies a constant voltage of 28-32V for a duration of 0.1-0.2 min.
5. The method for preparing a 4H-SiC integrated self-supporting photoanode according to claim 1, wherein the continuous periodic etching in step S2 applies a pulse voltage with a period of 0.7-0.9S, a dwell time of 0.3-0.5S, and a voltage of 18-20V for a duration of 4-13 min.
6. The method for preparing a 4H-SiC integrated self-supporting photoanode as claimed in claim 1, wherein the etching solution in step S2 is C with a volume ratio of (5-7): 12H5OH, HF and H2O2The mixed solution of (1).
7. The method for preparing a 4H-SiC integrated self-supporting photoanode according to claim 1, wherein the step S3 is to clean the photoanode semi-finished product by using absolute ethyl alcohol and deionized water respectively.
8. The method for preparing a 4H-SiC integrated self-supporting photoanode according to claim 1, wherein the drying in step S3 is constant temperature drying at 50-70 ℃ for 3-7 min.
9. The 4H-SiC integrated self-supporting photoanode is characterized in that the 4H-SiC integrated self-supporting photoanode is prepared by the preparation method of any one of claims 1 to 8, and the 4H-SiC integrated self-supporting photoanode is provided with a uniform 4H-SiC monocrystal highly-oriented nanohole array, wherein the aperture is 20-70 nm, and the depth is 13-25 μm.
10. Use of a 4H-SiC integral self-supporting photoanode according to claim 9 in photoelectrocatalysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010071042.XA CN111188082B (en) | 2020-01-21 | 2020-01-21 | Preparation method and application of 4H-SiC integrated self-supporting photo-anode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010071042.XA CN111188082B (en) | 2020-01-21 | 2020-01-21 | Preparation method and application of 4H-SiC integrated self-supporting photo-anode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111188082A true CN111188082A (en) | 2020-05-22 |
| CN111188082B CN111188082B (en) | 2021-01-26 |
Family
ID=70706554
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010071042.XA Active CN111188082B (en) | 2020-01-21 | 2020-01-21 | Preparation method and application of 4H-SiC integrated self-supporting photo-anode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111188082B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5376241A (en) * | 1992-10-06 | 1994-12-27 | Kulite Semiconductor Products, Inc. | Fabricating porous silicon carbide |
| DE19948184A1 (en) * | 1999-10-06 | 2001-05-03 | Fraunhofer Ges Forschung | Electrochemical production of peroxodisulfuric acid using diamond coated electrodes |
| CN102534648A (en) * | 2012-01-11 | 2012-07-04 | 南京大学 | Method for hydrogen production by electrochemically decomposing water by using surface autocatalytic effect of superfine 3C-SiC nanocrystals |
| WO2018112297A1 (en) * | 2016-12-16 | 2018-06-21 | Elwha Llc | Methods for fabricating and etching porous silicon carbide structures |
| CN108251888A (en) * | 2017-11-29 | 2018-07-06 | 宁波工程学院 | A kind of preparation method of transparent 4H-SiC nanohole arrays |
| CN108930057A (en) * | 2018-07-03 | 2018-12-04 | 宁波工程学院 | A method of cap layers in removal anodic oxidation preparation SiC nanostructure |
| CN109811356A (en) * | 2019-01-11 | 2019-05-28 | 宁波工程学院 | A kind of N doping SiC single crystal nanohole array and its photoelectrocatalysis anode obtained |
-
2020
- 2020-01-21 CN CN202010071042.XA patent/CN111188082B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5376241A (en) * | 1992-10-06 | 1994-12-27 | Kulite Semiconductor Products, Inc. | Fabricating porous silicon carbide |
| DE19948184A1 (en) * | 1999-10-06 | 2001-05-03 | Fraunhofer Ges Forschung | Electrochemical production of peroxodisulfuric acid using diamond coated electrodes |
| CN102534648A (en) * | 2012-01-11 | 2012-07-04 | 南京大学 | Method for hydrogen production by electrochemically decomposing water by using surface autocatalytic effect of superfine 3C-SiC nanocrystals |
| WO2018112297A1 (en) * | 2016-12-16 | 2018-06-21 | Elwha Llc | Methods for fabricating and etching porous silicon carbide structures |
| CN108251888A (en) * | 2017-11-29 | 2018-07-06 | 宁波工程学院 | A kind of preparation method of transparent 4H-SiC nanohole arrays |
| CN108930057A (en) * | 2018-07-03 | 2018-12-04 | 宁波工程学院 | A method of cap layers in removal anodic oxidation preparation SiC nanostructure |
| CN109811356A (en) * | 2019-01-11 | 2019-05-28 | 宁波工程学院 | A kind of N doping SiC single crystal nanohole array and its photoelectrocatalysis anode obtained |
Non-Patent Citations (6)
| Title |
|---|
| C. LI ET AL.: "Electro-Chemical Mechanical Polishing of Silicon Carbide", 《MATERIALS SCIENCE FORUM》 * |
| HUIQIANG LI ET AL.: "Mild fabrication of large-scale and well-aligned 4H–SiC nanoarrays with controlled configurations", 《CERAMICS INTERNATIONAL》 * |
| JAGANATHAN SENTHILNATHAN ET AL.: "Synthesis of carbon films by electrochemical etching of SiC with hydrofluoric acid in nonaqueous solvents", 《CARBON》 * |
| MATTHIAS SACHSENHAUSER ET AL.: "Suppression of Photoanodic Surface Oxidation of N-type 6H-SiC Electrodes in Aqueous Electrolytes", 《LANGMUIR》 * |
| SHANG XU ET AL.: "Single-Crystal Integrated Photoanodes Based on 4H‑SiC Nanohole Arrays for Boosting Photoelectrochemical Water Splitting Activity", 《ACS APPL. MATER. INTERFACES》 * |
| TOMONARI YASUDA ET AL.: "SiC photoelectrodes for a self-driven water-splitting cell", 《APPLIED PHYSICS LETTERS》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111188082B (en) | 2021-01-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gong et al. | Electrochemically multi-anodized TiO2 nanotube arrays for enhancing hydrogen generation by photoelectrocatalytic water splitting | |
| Li et al. | Effect of water and annealing temperature of anodized TiO2 nanotubes on hydrogen production in photoelectrochemical cell | |
| Zhu et al. | CdS and PbS nanoparticles co-sensitized TiO2 nanotube arrays and their enhanced photoelectrochemical property | |
| CN103132120B (en) | Method for preparing photoelectrocatalysis electrode material capable of efficiently degrading organic pollutants | |
| CN109261177B (en) | Nano-scale nickel phosphide/carbon cloth composite material, preparation method thereof and application thereof in electrocatalyst | |
| CN109621981B (en) | Metal oxide-sulfide composite oxygen evolution electrocatalyst and preparation method and application thereof | |
| CN105986292B (en) | Preparation method of cobalt-nickel double-layer hydroxide modified titanium dioxide nanotube array and application of photoelectrochemical hydrolysis hydrogen production | |
| CN110965076A (en) | Preparation method of electrolytic water electrode with double-function three-dimensional layered core-shell structure | |
| Ampelli et al. | The use of a solar photoelectrochemical reactor for sustainable production of energy | |
| CN111437841B (en) | Tungsten telluride-tungsten boride heterojunction electrocatalyst and preparation method and application thereof | |
| CN112090436B (en) | Nickel-based catalyst, preparation method and application | |
| Liu et al. | Ultrafast fabrication of nanostructure WO3 photoanodes by hybrid microwave annealing with enhanced photoelectrochemical and photoelectrocatalytic activities | |
| CN103872174A (en) | Method for preparing photo-anode of Au-modified TiO2 nano-rod array | |
| CN108043378B (en) | Nonmetal-doped porous-wall titanium nanotube array visible-light-driven photocatalyst and preparation method and application thereof | |
| CN111097451A (en) | Preparation method of porous cobalt disulfide catalyst with titanium mesh as substrate, porous cobalt disulfide crystal nanosheet and application | |
| CN108707924B (en) | TiO modified by ruthenium selenide nano-particles2Hydrogen evolution electrocatalyst of nanotube array, preparation method and application | |
| Zhang et al. | Electrochemically prepared cuprous oxide film for photo-catalytic oxygen evolution from water oxidation under visible light | |
| CN113600175A (en) | General synthesis method of three-dimensional ordered macroporous structure sodium tantalate photocatalytic hydrogen production material | |
| CN110408947B (en) | Nickel-cobalt oxide electrode material of composite silver oxide and preparation method and application thereof | |
| CN111188082B (en) | Preparation method and application of 4H-SiC integrated self-supporting photo-anode | |
| CN113293404A (en) | Heterojunction photo-anode material and preparation method and application thereof | |
| CN111804317A (en) | Method for directly growing high-density cobalt phosphide nano-wire electrocatalyst on conductive substrate and application thereof | |
| CN109402654B (en) | MoS with substrate protection function2/Ni3Se2Composite hydrogen evolution electrocatalyst and preparation method thereof | |
| CN107164780A (en) | A kind of WO3The preparation method of/graphene quantum dot composite film photo-anode | |
| CN114086202B (en) | Non-noble metal catalyst for glycerol oxidation-assisted hydrogen production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |