CN109811356A - A kind of N-doped SiC single crystal nano-channel array and its photoelectric catalytic anode - Google Patents
A kind of N-doped SiC single crystal nano-channel array and its photoelectric catalytic anode Download PDFInfo
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Abstract
The present invention relates to a kind of N to adulterate SiC single crystal nanohole array, and in particular to a kind of N adulterates the preparation method of photoelectrocatalysis anode made from SiC single crystal nanohole array, belongs to technical field of material.The invention proposes a kind of N to adulterate SiC single crystal nanohole array, N doping SiC single crystal nanohole array is applied to N and adulterates SiC nanohole array photoelectrocatalysis anode, there is high density of photocurrent (up to~2.41mA/cm2), fast photoresponse and wide spectral response range under visible light.
Description
Invention field
The present invention relates to a kind of N to adulterate SiC single crystal nanohole array, and in particular to a kind of N doping SiC single crystal nano-pore
The preparation method of photoelectrocatalysis anode, belongs to technical field of material made from channel array.
Background technique
There is photoelectrocatalysis (Photoelectrochemical, PEC) from discovery monocrystalline TiO2 semi-conducting electrode in 1972
Since decomposing this phenomenon of water, technological development of the semiconductor nano material as catalyst in terms of photoelectrocatalysis decomposes aquatic products hydrogen
Have become current one of hot research direction.Wherein, one-dimensional nano structure, such as nanometer rods, nano wire, nanotube, due to
With fast electron-transport, many advantages, such as low electron-hole recombination rate, cause the very big concern of research worker.But
It is that one-dimensional nano structure is limited to that surface area is small, restriction of the interface mostly with the negative factors such as light capture ability difference simultaneously, it is difficult to real
The preparation of existing photoelectrocatalysielectrode electrode with high performance.Compared to the monodimension nanometer material of random graph, by a highly directional wiener
The three-dimensional manometer array structure of rice structure composition would generally show more excellent PEC characteristic.Three-dimensional matrix structure has height
Consistent electron-hole transmission direction is spent, the transmission range of shorter photo-generated carrier is more advantageous to the diffusion of photo-generated carrier
With transmission, the incident photon-to-electron conversion efficiency of electrode can be greatly improved.In addition to the configuration of nano material, the light absorpting ability of optoelectronic pole is also
Promote the key influence factor of PEC water decomposition, current main stream approach is sensitized by nonmetal doping and fuel, is reduced
The forbidden bandwidth of wide band gap semiconducter realizes the optoelectronic pole material development of high catalytic activity.
SiC is a kind of important third generation semiconductor material, has high chemical stability and carrier transport ability, excellent
Different thermal stability, it is nontoxic the advantages that.In addition, the forbidden bandwidth of SiC is 2.3~3.2eV, be especially suitable for photoelectrocatalysis electricity
Pole material.Currently, using the SiC of SiC block materials, one-dimentional structure, film, composite construction and various different crystal forms as PEC
The research of optoelectronic pole material has been reported that, shows good development prospect.But it is applied at present in SiC optoelectronic pole material
In terms of PEC water decomposition, still face following problem, it would be highly desirable to research and solve: (i) is based on large area, highly directional SiC nano-array
SiC optoelectronic pole research and development；(ii) the SiC optoelectronic pole constructed based on monocrystal SiC nanostructure；(iii) to have clean nothing
The SiC light anode obtained based on the doping SiC nanostructure of oxidized surface；(iv) research and development of SiC light anode, are reported at present
SiC photoelectricity extreme portions are all photocathode materials.
Although being achieved in terms of making every effort to obtain the research and development of SiC nanostructure optoelectronic pole of the aqueous energy of bloom electrocatalytic decomposition
Certain progress, but to meet in terms of the SiC light anode of preparation higher performance there is still a need for further prepare it is novel, have it is higher
The SiC nanostructure of photoelectrocatalysis ability.The present invention provides a kind of monocrystalline N of high PhotoelectrocatalytiPerformance Performance to adulterate SiC nano-pore
Channel array photoelectrocatalysis anode and preparation method thereof.Photoelectrocatalysis water decomposition detection shows: light anode has height under visible light
Density of photocurrent (up to~2.41mA/cm2), fast photoresponse and wide spectral response range, realize excellent light anode material
The research and development of material.
Summary of the invention
The present invention in view of the above-mentioned problems existing in the prior art, proposes a kind of N doping SiC single crystal nanohole array,
N doping SiC single crystal nanohole array is applied to N and adulterates SiC nanohole array photoelectrocatalysis anode, under visible light
With high density of photocurrent (up to~2.41mA/cm2), fast photoresponse and wide spectral response range.
In a kind of above-mentioned N doping SiC single crystal nanohole array, the wall thickness of the N doping SiC single crystal nano pore is
The depth of 11-15nm, the N doping SiC single crystal nanohole array are 17-21 μm.SiC single crystal nanometer is adulterated in N of the present invention
In channel pore array, wall thickness is smaller, is more conducive to carrier mobility to SiC nano pore surface, realizes point of photo-generate electron-hole
From to improve photoelectrocatalysis efficiency；Thickness is bigger, and more surface areas can be generated, and is conducive to photoelectrocatalysis, but too thick
Words, are unfavorable for the axial transmission of carrier, unfavorable to PhotoelectrocatalytiPerformance Performance.
Preferably, the preparation method of the N doping SiC single crystal nanohole array includes the following steps: to adulterate with N
The small chip of SiC is anode, and graphite flake is cathode, is etched in the electrolytic solution with anodic oxidation, obtains N in the small wafer surface of SiC and mixes
Miscellaneous SiC single crystal nanohole array, the electrolyte are the mixed solution of hydrofluoric acid, ethyl alcohol and hydrogen peroxide, and hydrofluoric acid, ethyl alcohol
Volume ratio with hydrogen peroxide three is 6:6:(1-1.2).
In a kind of preparation method of above-mentioned N doping SiC single crystal nanohole array, the electrolyte is hydrofluoric acid, second
The mixed solution of pure and mild hydrogen peroxide, and the volume ratio of hydrofluoric acid, ethyl alcohol and hydrogen peroxide three is 6:6:(1-1.2).In electrolyte
The middle too big anode oxidation process of HF acid amount can bad control, N obtained adulterates SiC single crystal nanohole array photoelectrocatalysis anode
Photoresponse rate is relatively low, and if HF acid amount is very little, anode oxidation process speed is too slow, and no matter HF acid amount is excessive or mistake
It is few, the formation effect of final N doping SiC single crystal nanohole array photoelectrocatalysis anode can be all influenced, therefore in order to obtain more
High photoresponse rate, the volume ratio needs control of hydrofluoric acid, ethyl alcohol, hydrogen peroxide three is in 6:6:(1-1.2).
Preferably, the SiC single crystal piece that the N doping small chip of SiC is adulterated by N is cut into, the N adulterates the small chip of SiC
Size be (0.5-0.8) × (1.5-2) cm2。
Preferably, the SiC single crystal piece is 4H-SiC.
A kind of N doping SiC single crystal nanohole array photoelectrocatalysis anode, the N adulterate SiC single crystal nanohole array
Photoelectrocatalysis anode is made by N doping SiC single crystal nanohole array.The addition of N dopant can extend in the present invention
The optical absorption edge of SiC nanohole array increases light abstraction width, realizes the raising of PhotoelectrocatalytiPerformance Performance.
A kind of preparation method of N doping SiC single crystal nanohole array photoelectrocatalysis anode, the preparation method include:
One layer of conductive silver paste is coated in conductive glass surface, then the surrounding of conductive silver paste film is enclosed into closing with epoxy resin, then
N obtained above is adulterated into SiC single crystal nanohole array from the small wafer surface removing of SiC, surface is transferred to and is coated with conduction
The conductive glass surface of silver paste obtains N doping SiC single crystal nanohole array photoelectrocatalysis anode.
In a kind of preparation method of above-mentioned N doping SiC single crystal nanohole array photoelectrocatalysis anode, the conduction glass
Glass is ITO.
A kind of detection method of N doping SiC single crystal nanohole array photoelectrocatalysis anode, in the detection method: with
Ag/AgCl is reference electrode, and Pt piece is to electrode, Na2SO4For electrolyte, Xe lamp is simulated visible light light source.
Using Ag/AgCl as reference electrode, Pt piece is to electrode, Na2SO4For electrolyte, Xe lamp is simulated visible light light source,
The photoelectric current and its stability for detecting N doping SiC single crystal nanohole array photoelectrocatalysis anode obtained, measure result are as follows:
N adulterates density of photocurrent of the SiC single crystal nanohole array photoelectrocatalysis anode at 1.4V and is up to 2.41mA/
cm2；N adulterates the screening in the appearance period and copped wave piece of SiC single crystal nanohole array photoelectrocatalysis anode photoelectric current and dark current
Photoperiod is completely corresponding, has high photoresponse rate；In the long-time of 5000s, the appearance period of photoelectric current and dark current
Always corresponding with the shading period of copped wave piece, and electric current photoelectric current is not decayed significantly.
N doping SiC single crystal nanohole array photoelectrocatalysis anode of the present invention has high photoelectric current close under visible light
Spend (up to~2.41mA/cm2), fast photoresponse and wide spectral response range, realize the research and development of excellent optical anode material.
Compared with prior art, the present invention has the following advantages:
1, the present invention not only realizes the SiC photoelectrocatalysis anode based on N doping SiC single crystal nanohole array structure
Preparation, and SiC photoelectrocatalysis anode obtained has high photoelectrocatalysis current density and catalytic stability；
2, N doping SiC single crystal nanohole array photoelectrocatalysis anode produced by the present invention has high under visible light
Density of photocurrent (up to~2.41mA/cm2), fast photoresponse and wide spectral response range, realize excellent optical anode material
Research and development.
Detailed description of the invention
Fig. 1 is the pictorial diagram that N prepared in the embodiment of the present invention one adulterates SiC single crystal nanohole array film；
Fig. 2 is the low power scanning electron microscope that N prepared in the embodiment of the present invention one adulterates SiC single crystal nanohole array
(SEM) figure；
Fig. 3 is the high power SEM figure that N prepared in the embodiment of the present invention one adulterates SiC single crystal nanohole array；
Fig. 4 is the high power SEM that N prepared in the embodiment of the present invention one adulterates SiC single crystal nanohole array cross section
Figure；
Fig. 5 is that N doping SiC single crystal nanohole array film prepared in the embodiment of the present invention one is transferred to conduction
Glass surface and the schematic diagram for constructing SiC photoelectrocatalysis anode；
Fig. 6 is that N prepared in the embodiment of the present invention one adulterates SiC single crystal nanohole array photoelectrocatalysis anode material object
Figure；
Fig. 7 is the linear voltammetric scan curve (LSV) of SiC photoelectrocatalysis anode prepared in the embodiment of the present invention one；
Fig. 8 is transient current of the SiC photoelectrocatalysis anode prepared in the embodiment of the present invention one under illumination and dark-state
Density-voltage curve；
Fig. 9 is that electric current of the SiC photoelectrocatalysis anode prepared in the embodiment of the present invention one under the conditions of cycling switch is close
Degree-time graph.
Specific embodiment
The following is specific embodiments of the present invention, and is described with reference to the drawings and further retouches to technical solution of the present invention work
It states, however, the present invention is not limited to these examples.
Embodiment 1
The N SiC single crystal piece adulterated is cut into having a size of 0.5 × 1.5cm2Small chip；SiC single crystal piece is 4H-SiC；With N
The doping small chip of SiC is anode, and graphite flake is cathode, is for the mixed liquor of 6:6:1 with hydrofluoric acid, ethyl alcohol and hydrogen peroxide portion rate
Electrolyte is etched using anodic oxidation, obtains N doping SiC single crystal nanohole array in the small wafer surface of SiC；In conductive glass
Glass surface coats one layer of conductive silver paste, then the surrounding of conductive silver paste film is enclosed closing with epoxy resin；N doping SiC is mono-
Brilliant nanohole array film is transferred to the conductive glass surface that surface is coated with conductive silver paste from the small wafer surface removing of SiC,
Electro-conductive glass is ITO.The embodiment SiC nanostructure etching film obtained stripped down from the small wafer surface of SiC is in kind
Figure is as shown in Figure 1, Fig. 1, which shows it after etching, may be implemented large area, undamaged removing；The doping of N made from the embodiment
SiC single crystal nanohole array photoelectrocatalysis anode low power scanning electron microscope (SEM) figure is as shown in Fig. 2, Fig. 2 and Fig. 3 show system
The N doping SiC single crystal nanohole array photoelectrocatalysis anode obtained has highly directional, large area, the nano pore battle array of homogenization
Array structure, the wall thickness of nano pore are only 15nm.The SEM of nanohole array cross section made from the embodiment schemes such as Fig. 4 institute
Show, the depth that Fig. 4 shows nano surface channel pore array is about 17 μm；The SiC nano pore that will be stripped down in the embodiment
Array film is transferred on electro-conductive glass, and the schematic diagram for preparing SiC photoelectrocatalysis anode is as shown in Figure 5；The embodiment is made
N doping SiC single crystal nanohole array photoelectrocatalysis anode pictorial diagram it is as shown in Figure 6.
Embodiment 2
Difference with embodiment 1 is only that electrolyte is with hydrofluoric acid, ethyl alcohol and hydrogen peroxide according to number in the embodiment
Than for mixed liquor made from 6:6:1.05, other are same as Example 1, and details are not described herein again.N made from embodiment 2 adulterates SiC
Nanometer monocrystalline channel pore array photoelectrocatalysis anode has highly directional, large area, the nanohole array structure of homogenization, nano-pore
The wall thickness in road is only 14nm.The depth of nanohole array cross section made from the embodiment is about 18 μm.
Embodiment 3
Difference with embodiment 1 is only that electrolyte is with hydrofluoric acid, ethyl alcohol and hydrogen peroxide according to number in the embodiment
Than for mixed liquor made from 6:6:1.1, other are same as Example 1, and details are not described herein again.N made from embodiment 3 adulterates SiC
Nanometer monocrystalline channel pore array photoelectrocatalysis anode has highly directional, large area, the nanohole array structure of homogenization, nano-pore
The wall thickness in road is only 13nm.The depth of nanohole array cross section made from the embodiment is about 19 μm.
Embodiment 4
Difference with embodiment 1 is only that electrolyte is with hydrofluoric acid, ethyl alcohol and hydrogen peroxide according to number in the embodiment
Than for mixed liquor made from 6:6:1.15, other are same as Example 1, and details are not described herein again.N made from embodiment 4 adulterates SiC
Nanometer monocrystalline channel pore array photoelectrocatalysis anode has highly directional, large area, the nanohole array structure of homogenization, nano-pore
The wall thickness in road is only 12nm.The depth of nanohole array cross section made from the embodiment is about 20 μm.
Embodiment 5
Difference with embodiment 1 is only that electrolyte is with hydrofluoric acid, ethyl alcohol and hydrogen peroxide according to number in the embodiment
Than for mixed liquor made from 6:6:1.2, other are same as Example 1, and details are not described herein again.N made from embodiment 5 adulterates SiC
Nanometer monocrystalline channel pore array photoelectrocatalysis anode has highly directional, large area, the nanohole array structure of homogenization, nano-pore
The wall thickness in road is only 11nm.The depth of nanohole array cross section made from the embodiment is about 21 μm.
Can be seen that the mechanism of etching and hydrofluoric acid from the result of embodiment 1-5 has much relations, and the ratio of hydrofluoric acid is got over
Height, etching it is more severe.In short, hydrofluoric acid ratio is higher, the wall thickness of nano pore is thinner, and depth is bigger.
Comparative example 1
Difference with embodiment 1 is only that electrolyte is with hydrofluoric acid, ethyl alcohol and hydrogen peroxide according to number in the comparative example
Than for mixed liquor made from 6:6:0.8, other are same as Example 1, and details are not described herein again.
Comparative example 2
Difference with embodiment 1 is only that electrolyte is with hydrofluoric acid, ethyl alcohol and hydrogen peroxide according to number in the comparative example
Than for mixed liquor made from 6:6:1.4, other are same as Example 1, and details are not described herein again.
It has been observed that nano pore structure can not be obtained using comparative example 1 and 2.Therefore, only in electrolyte of the present invention
Under conditions of number, it is just able to achieve the preparation of the SiC photoelectrocatalysis anode based on N doping SiC single crystal nanohole array structure,
And SiC photoelectrocatalysis anode obtained has high photoelectrocatalysis current density and catalytic stability.
Using Ag/AgCl as reference electrode, Pt piece is to electrode, Na2SO4For electrolyte, Xe lamp is simulated visible light light source,
Detect the photoelectric current and its stability in embodiment 1, testing result is as shown in Fig. 7, Fig. 8, Fig. 9: wherein Fig. 7 is in illumination and secretly
The appearance period of instantaneous current density-voltage curve under state, photoelectric current and dark current and the shading period of copped wave piece are complete
It is corresponding, show the SiC photoelectrocatalysis anode photoresponse rate with higher of preparation；Fig. 8 is instantaneous under illumination and dark-state
The appearance period of current density voltage curve, photoelectric current and dark current and the shading period of copped wave piece are completely corresponding, show to make
Standby SiC photoelectrocatalysis anode photoresponse rate with higher；Current density-time of Fig. 9 under the conditions of cycling switch is bent
Line, in the long-time of 5000s, the appearance period of photoelectric current and dark current is corresponding with the shading period of copped wave piece always, and
Electric current photoelectric current is not decayed significantly, shows the SiC photoelectrocatalysis anode photoelectrocatalysis stability with higher of preparation.
This place embodiment is not exhaustive claimed midpoint of technical range and in embodiment technology
In scheme to single or multiple technical characteristics it is same replacement be formed by new technical solution, equally all the present invention claims
In the range of protection, and between the parameter that is related to of the present invention program if not otherwise specified, then there is no can not between each other
The unique combinations of replacement.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can do various modifications or supplement or is substituted in a similar manner to described specific embodiment, but simultaneously
Spirit or beyond the scope defined by the appended claims of the invention is not deviated by.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (7)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111188082A (en) * | 2020-01-21 | 2020-05-22 | 宁波工程学院 | A kind of preparation method and application of 4H-SiC integrated self-supporting photoanode |
| CN113308743A (en) * | 2021-04-29 | 2021-08-27 | 北京科技大学 | Method for regulating and controlling 4H-SiC nano structure based on single N doping and simultaneously collecting mechanical energy and optical energy for water splitting |
| CN114038934A (en) * | 2021-09-24 | 2022-02-11 | 北京科技大学 | Preparation method of high-temperature ultraviolet photoelectric detector based on co-doped one-dimensional SiC nanostructure |
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| 陈春梅: "阳极氧化法制备4H-SiC 纳米阵列与结构调控及其光电特性", 《中国优秀硕士学位论文全文数据库》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111188082A (en) * | 2020-01-21 | 2020-05-22 | 宁波工程学院 | A kind of preparation method and application of 4H-SiC integrated self-supporting photoanode |
| CN113308743A (en) * | 2021-04-29 | 2021-08-27 | 北京科技大学 | Method for regulating and controlling 4H-SiC nano structure based on single N doping and simultaneously collecting mechanical energy and optical energy for water splitting |
| CN114038934A (en) * | 2021-09-24 | 2022-02-11 | 北京科技大学 | Preparation method of high-temperature ultraviolet photoelectric detector based on co-doped one-dimensional SiC nanostructure |
| CN114038934B (en) * | 2021-09-24 | 2024-02-09 | 北京科技大学 | Preparation method of high-temperature ultraviolet photoelectric detector based on co-doped one-dimensional SiC nano structure |
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