CN108642511A - A kind of preparation method of silicon nanowires/pucherite complex light anode - Google Patents
A kind of preparation method of silicon nanowires/pucherite complex light anode Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of silicon nanowires/pucherite complex light anode, it is included in monocrystalline silicon sheet surface and corrodes and vertical regular silicon nanowire array；Then the precursor solution of pucherite is prepared, solute is five nitric hydrate bismuths and vanadyl acetylacetonate in precursor solution, and solvent is glacial acetic acid and acetylacetone,2,4-pentanedione；Precursor solution is dropped in into surface of silicon nanowires again, after drying, drop coating is dried again repeatedly；Finally the sample after drop Tu is calcined, obtains the silicon nanowires/pucherite complex light anode.Silicon nanowires provided by the invention/pucherite complex light anode improves pucherite photo-generated carrier, and transmission efficiency is low, nano material is easily reunited, photocatalysis performance farther out from theoretical efficiency difference the problem of, unique silicon nanowires has been selected to form composite construction with pucherite, compared with other composite constructions, in addition to promoting separation of charge efficiency, the light absorption and catalytic capability of electrode are enhanced also while greatly, and obtains excellent photoelectrochemical behaviour.
Description
Technical field
The invention belongs to photochemical catalyzing technical field of material, more particularly, to a kind of silicon nanowires/vanadic acid
The preparation method of bismuth complex light anode.
Background technology
Currently, environmental pollution and energy shortage are two hang-ups of facing mankind, the sustainable development of the mankind is seriously threatened
Exhibition.As environmental problem and energy problem are increasingly serious, current fossil energy is substituted using green clean energy resource to be become not
Carry out one of the trend of energy development.Hydrogen Energy is because cleanliness without any pollution, calorific value are high and the advantages that derive from a wealth of sources, it is considered to be most ideal
Clean energy resource.Fossil fuel hydrogen manufacturing and water electrolysis hydrogen production are the main methods of current hydrogen manufacturing, however both technologies are required to
The additional energy is consumed to achieve the goal, and photocatalysis technology develops valence due to can be directly concerned using solar hydrogen making
Lattice are cheap, efficient photochemical catalyst and are applied to photodegradation water hydrogen manufacturing and become the center of gravity of research.
In the novel photocatalysis material reported, pucherite is a kind of photochemical catalyst of great potential, has visible light
Catalytic activity, narrow band gap prepare the advantages that simple, stability is high, nontoxic, thus cause the extensive concern of researcher.However
In light-catalyzed reaction, pucherite carrier transport efficiency is poor, easily cause electron-hole pair it is compound and influence photocatalysis effect
Rate, while the pucherite of nanostructure is easy to reunite, and to reduce the contact area of catalyst and electrolyte solution, influences to be catalyzed
Activity.Studies have shown that by adulterating, regulating and controlling crystalline phase, the photocatalysis of pucherite can be improved with modes such as other semiconductors couplings
Performance.Currently, in the photoelectrocatalysielectrode electrode having disclosed, prepared ferro-cobalt hydrogen-oxygen in Chinese patent CN106435635 A
Compound/pucherite complex light anode shows excellent photoelectrochemical behaviour, in 100 mW/cm2Simulated solar irradiation under,
Density of photocurrent under 1.23V reaches 2.48mA/cm2.However, in being studied with existing other, the photoelectricity of pucherite turns
Change efficiency and differs also far with theoretical efficiency（Theoretical maximum photoelectric current is 7.5 mW/cm2）.Therefore, how further to overcome vanadium
The problem of transmission efficiency is low for the photo-generated carrier of sour bismuth, nano material is easily reunited, and light absorption and utilization rate are further promoted, from
And it obtains the higher optoelectronic pole of photoelectrochemical behaviour and is of great significance.
Invention content
Transmission efficiency is low, nano material is easily reunited, photocatalysis performance is from reason for the photo-generated carrier of pucherite by the present invention
The problem of differing farther out by efficiency, for the first time using with unique sunken luminous effect, the silicon that specific surface area is very big, electronics radial transport is fast
Nano wire loads pucherite nanoshells and nano particle simultaneously as main body rack, in nanowire surface, obtained silicon nanometer
Line/pucherite complex light anode not only has efficient light absorption and separation of charge performance, is dispersed in the vanadium of surface of silicon nanowires
Sour bismuth nano particle additionally provides a large amount of active site for photochemical catalyzing, to which the photoelectric current for obtaining very high is close
Degree, shows excellent photoelectrochemical behaviour.
The purpose of the present invention is to provide a kind of preparation methods of silicon nanowires/pucherite complex light anode.
The above-mentioned technical purpose of the present invention is achieved through the following technical solutions：
The present invention provides a kind of preparation methods of silicon nanowires/pucherite complex light anode, include the following steps：
S1：Corrode in monocrystalline silicon sheet surface and vertical regular silicon nanowire array；
S2：The precursor solution for preparing pucherite, solute is five nitric hydrate bismuths and vanadyl acetylacetonate in precursor solution, molten
Agent is glacial acetic acid and acetylacetone,2,4-pentanedione；
S3：The obtained precursor solutions of step S2 are dropped in into the surface of silicon nanowires that step S1 is prepared, after drying, are dripped repeatedly
Painting is dried again；
S4：There is the sample of multilayer precursor solution to calcine the surface of silicon nanowires drop coating that step S3 is obtained, obtains the silicon and receive
Rice noodles/pucherite complex light anode；
A concentration of 10 ~ 80mM of five nitric hydrate bismuths in step S2, a concentration of 10 ~ 80mM of vanadyl acetylacetonate, acetic acid and second
The volume ratio of acyl acetone is（10~30）：（1~2）.
Preferably, corrode in monocrystalline silicon sheet surface using metal Assisted Chemical Etching Process method or ion etching method in step S1
Vertical regular silicon nanowire array, etchant solution are the mixed aqueous solution of silver nitrate and hydrofluoric acid, are cleaned after corrosion, removal is received
The oxide skin(coating) of nanowire surface obtains vertical regular silicon nanowire array.
Preferably, monocrystalline silicon piece is one kind in P-type silicon or N-type silicon in step S1.
Preferably, a concentration of 4 ~ 10M of a concentration of 0.01 ~ 0.05 M of silver nitrate, hydrofluoric acid solution.
Preferably, the time of corrosion is 30 ~ 60min, and is corroded at normal temperatures.
Preferably, use volume ratio for 3 in step S1:1 concentrated sulfuric acid and hydrogen peroxide is cleaned, and the temperature of cleaning is
180 ~ 220 DEG C, oxide skin(coating) is removed using the hydrofluoric acid of a concentration of 2.5 ~ 3.5M after cleaning.
Preferably, the number of plies of the precursor solution drop coating on silicon nanowires is 3 ~ 20 layers in step S3.
Preferably, the temperature calcined in step S4 is 450 ~ 650 DEG C, and the time of calcining is 60 ~ 360min, is used in calcining
Heating rate be 5 ~ 10 DEG C/min.
Currently, the complex light electrode that pucherite is combined with other semiconductors, typically forms only hetero-junctions to promote charge
Separation promotes carrier transmission performance, rarely while improving carrier separation, improves reactivity site and greatly increases
Strong light absorption integrates raising photocatalysis performance.The present inventor selects the silicon nanowires battle array provided in step S1 of the present invention
Row, with very strong sunken luminous effect, specific surface area greatly, the fast characteristic of electronics radial transport, and by regulating and controlling in step S2 before
The concentration for driving body loads pucherite nanoshells and nano particle simultaneously in nanowire surface, obtains and be provided simultaneously with strong light suction
It receives, separation of charge effect is good, catalytic activity is high complex light electrode, and significant increase photoelectrochemical behaviour, in particular, this hair
The material of bright offer density of photocurrent in 1.23V may be up to 5.2 mA/cm2。
The present invention protects the silicon nanometer that the preparation method of the silicon nanowires/pucherite complex light anode is prepared simultaneously
Line/pucherite complex light anode material.
It is also protected in the present invention using the silicon nanowires/application of the pucherite complex light anode in photochemical catalyzing
It protects in range.
Compared with the existing technology, the present invention has the advantage that and effect：
Silicon nanowires provided by the invention/pucherite complex light anode improves pucherite photo-generated carrier, and transmission efficiency is low, receives
The problem of rice material is easily reunited, photocatalysis performance is differed farther out from theoretical efficiency, unique silicon nanowires and pucherite are selected
Composite construction is formed, compared with other composite constructions, in addition to promoting separation of charge efficiency, also greatly enhances the light of electrode simultaneously
Absorption and catalytic capability, and obtain excellent photoelectrochemical behaviour.
Description of the drawings
Fig. 1 be embodiment 1 be prepared silicon nanowires, silicon nanowires/pucherite complex light anode scanning electron microscope and
The transmission electron microscope photo of silicon nanowires/pucherite.
Fig. 2 be embodiment 1 be prepared planar silicon, silicon nanowires, planar silicon/pucherite, silicon nanowires/pucherite
Reflectance spectrum figure.
Fig. 3 is the resistance that planar silicon, silicon nanowires, planar silicon/pucherite, silicon nanowires/pucherite is prepared in embodiment 1
Anti- figure.
Fig. 4 be embodiment 1 be prepared planar silicon, silicon nanowires, planar silicon/pucherite, silicon nanowires/pucherite light
The linear sweep voltammetry curve of anode.
Specific implementation mode
Further illustrated the present invention below in conjunction with specific embodiments and the drawings, but embodiment the present invention is not done it is any
The restriction of form.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagent, methods
And equipment.
Unless stated otherwise, agents useful for same and material of the present invention are purchased in market.
Embodiment 1
A kind of preparation method of silicon nanowires/pucherite complex light anode is as follows：
（1）Corroded in monocrystal N type silicon chip surface using metal Assisted Chemical Etching Process method and vertical regular silicon nanowire array, it is rotten
Lose the mixed aqueous solution that solution is silver nitrate and hydrofluoric acid, a concentration of 0.02 M of silver nitrate, a concentration of the 5.5 of hydrofluoric acid solution
M, etching time are 45 min, are corroded under room temperature.It is cleaned in the concentrated sulfuric acid, hydrogen peroxide mixed solution after corrosion, the concentrated sulfuric acid
It is 3 with dioxygen water volume ratio:1, temperature is 200 DEG C when cleaning, after rinse repeatedly with deionized water, with the removal of diluted hydrofluoric acid
The oxide skin(coating) of nanowire surface obtains silicon nanowire array, a concentration of 3 M of dilute hydrofluoric acid；
（2）Prepare pucherite precursor solution, solute be five nitric hydrate bismuths and vanadyl acetylacetonate, five nitric hydrate bismuths
A concentration of 20 mM, a concentration of 20 mM of vanadyl acetylacetonate, solvent is that volume ratio is 20:1 glacial acetic acid and acetylacetone,2,4-pentanedione mixing
Liquid, ultrasonic disperse obtain uniformly mixed precursor solution；
（3）It will（2）In obtained precursor solution dropped in using the method for drippage coating（1）The silicon nanowires table being prepared
Drop coating and operation is dried to 12 layers of the number of plies in face repeatedly at room temperature after natural drying；
（4）It will（3）Obtained silicon line surface drop coating has the sample of multilayer precursor solution to calcine in vacuum tube furnace to obtain silicon
Nano wire/pucherite complex light anode, wherein calcination temperature are 550 DEG C, time 120min, and heating rate is 10 DEG C/min.
Embodiment 2
Silicon nanowires provided in this embodiment/the preparation method is the same as that of Example 1 for pucherite complex light anode, the difference is that,
A concentration of 30 mM of five nitric hydrate bismuths in the present embodiment, a concentration of 30 mM of vanadyl acetylacetonate.
Embodiment 3
Silicon nanowires provided in this embodiment/the preparation method is the same as that of Example 1 for pucherite complex light anode, the difference is that,
A concentration of 40 mM of five nitric hydrate bismuths in the present embodiment, a concentration of 40 mM of vanadyl acetylacetonate.
Embodiment 4
Silicon nanowires provided in this embodiment/the preparation method is the same as that of Example 1 for pucherite complex light anode, the difference is that,
A concentration of 50 mM of five nitric hydrate bismuths in the present embodiment, a concentration of 50 mM of vanadyl acetylacetonate.
Embodiment 5
Silicon nanowires provided in this embodiment/the preparation method is the same as that of Example 1 for pucherite complex light anode, the difference is that,
The drop coating number of plies is 6 layers in the present embodiment.
Embodiment 6
Silicon nanowires provided in this embodiment/the preparation method is the same as that of Example 1 for pucherite complex light anode, the difference is that,
The drop coating number of plies is 8 layers in the present embodiment.
Embodiment 7
Silicon nanowires provided in this embodiment/the preparation method is the same as that of Example 1 for pucherite complex light anode, the difference is that,
The drop coating number of plies is 10 layers in the present embodiment.
Embodiment 8
Silicon nanowires provided in this embodiment/the preparation method is the same as that of Example 1 for pucherite complex light anode, the difference is that,
The drop coating number of plies is 15 layers in the present embodiment.
A kind of 1 planar silicon light anode of comparative example
A kind of planar silicon light anode, the planar silicon light anode use merely the monocrystal N type silicon chip in embodiment 1.
A kind of 2 silicon nanowires light anode of comparative example
A kind of silicon nanowires light anode, the silicon nanowires light anode are step in embodiment 1（1）It is middle to utilize metal assistant chemical
Etching method is corroded in monocrystal N type silicon chip surface vertical regular silicon nanowire array.
A kind of 3 planar silicon of comparative example/pucherite complex light anode
A kind of planar silicon/pucherite complex light anode, the preparation method of the planar silicon/pucherite complex light anode are as follows：
（1）Planar silicon is monocrystal N type silicon chip；
（2）Prepare pucherite precursor solution, solute be five nitric hydrate bismuths and vanadyl acetylacetonate, five nitric hydrate bismuths
A concentration of 20 mM, a concentration of 20 mM of vanadyl acetylacetonate, solvent is that volume ratio is 20:1 glacial acetic acid and acetylacetone,2,4-pentanedione mixing
Liquid, ultrasonic disperse obtain uniformly mixed precursor solution；
（3）It will（2）Obtained precursor solution is dropped in using the method for drippage coating in planar silicon, at room temperature naturally dry
Afterwards, drop coating and operation is dried to 12 layers of the number of plies repeatedly；
（4）It will（3）Obtained flat silicon surface drop coating has the sample of multilayer precursor solution to calcine in vacuum tube furnace to obtain
Planar silicon/pucherite complex light anode, wherein calcination temperature be 550 DEG C, the time be 120 min, heating rate be 10 DEG C/
min。
Application Example：
Above-described embodiment 1 and comparative example 1,2,3 obtained samples are tested for the property.
The optical electro-chemistry test of all samples all uses 300W xenon lamps to carry AM1.5 optical filters in 100mW/cm2Simulation
It is carried out under sunlight, electrolyte solution is the Na of 0.5M2SO4Solution is tested using three-electrode system, i.e. Ag/AgCl conducts
Reference electrode, Pt are used as to electrode, and prepared sample is as working electrode.
Fig. 1 is the silicon nanowires light anode being prepared in embodiment 1（It is denoted as Si NWs）And silicon nanowires/pucherite is multiple
Closing light anode（It is denoted as Si NWs/BiVO4）Scanning electron microscope and transmission electron microscope photo, as the scanning electron microscope in Fig. 1 (a) can be seen
Go out, silicon nanowires is the regular array of vertical-growth, and in Fig. 1 (b) after loading pucherite, surface of silicon nanowires has nanometer
Grain attachment, it can be seen that there is the pucherite shell of flood densification in surface of silicon nanowires from the transmission electron microscope picture of figure (c),
Also uniform load has a large amount of pucherite nano particle outside shell, schemes to see in the high magnification transmission electron microscope picture of (d) apparent
Hetero-junctions, the lattice of silicon and the lattice of pucherite.
Fig. 2 is silicon nanowires/pucherite complex light anode that embodiment 1 is prepared（It is denoted as Si NWs/BiVO4）And it is right
The planar silicon being prepared in ratio 1,2,3（It is denoted as Planar Si）, silicon nanowires（It is denoted as Si NWs）, planar silicon/pucherite
（It is denoted as Planar Si/BiVO4）Reflectance spectrum figure；Figure it is seen that planar silicon average reflectance is 31%, planar silicon/
Pucherite is 25%, and the reflectivity of silicon nanowires is only 1.2%, and the average rate of silicon nanowires/pucherite is 1.5%.As it can be seen that by vanadium
Sour bismuth is supported on silicon nanowires the significant increase light absorption of combination electrode.
Fig. 3 is silicon nanowires/pucherite complex light anode that 1 embodiment 1 of embodiment is prepared（It is denoted as Si NWs/
BiVO4）And the planar silicon being prepared in comparative example 1,2,3（It is denoted as Planar Si）, silicon nanowires（It is denoted as Si NWs）, it is flat
Face silicon/pucherite（It is denoted as Planar Si/BiVO4）Impedance diagram.As seen from Figure 3, silicon nanowires/pucherite complex light
Half circular diameter of anode is minimum, illustrates relative to planar silicon（It is denoted as Planar Si）, silicon nanowires（It is denoted as Si NWs）, plane
Its resistance of silicon/pucherite is minimum, charge transfer efficiency highest.
Fig. 4 is silicon nanowires/pucherite complex light anode that embodiment 1 is prepared（It is denoted as Si NWs/BiVO4）And it is right
The planar silicon being prepared in ratio 1,2,3（It is denoted as Planar Si）, silicon nanowires（It is denoted as Si NWs）, planar silicon/pucherite
（It is denoted as Planar Si/BiVO4）Linear sweep voltammetry curve.As seen from Figure 4, in 1.23VvsUnder the voltage of RHE, silicon
The density of photocurrent of nano wire/pucherite complex light anode is up to 5.2 mA/cm2, it is 173 times of planar silicon, the 6.3 of silicon nanowires
Times, 6.8 times of planar silicon/pucherite.It can be seen that pucherite is supported on, sunken luminous effect is strong, large specific surface area, electron-transport are imitated
On the good silicon nanowires of rate, significantly improve pucherite in photochemical catalyzing light absorption and utilization rate is low, easy reunion, electricity
The problem of sub- transmission performance difference, is greatly improved its photoelectrochemical behaviour.
Claims (10)
1. a kind of preparation method of silicon nanowires/pucherite complex light anode, which is characterized in that include the following steps：
S1. corrode in monocrystalline silicon sheet surface and vertical regular silicon nanowire array；
S2. the precursor solution for preparing pucherite, solute is five nitric hydrate bismuths and vanadyl acetylacetonate in precursor solution, molten
Agent is glacial acetic acid and acetylacetone,2,4-pentanedione；
S3. the obtained precursor solutions of step S2 are dropped in into the surface of silicon nanowires that step S1 is prepared, after drying, dripped repeatedly
Painting is dried again；
S4. there is the sample of multilayer precursor solution to calcine the surface of silicon nanowires drop coating that step S3 is obtained, obtain the silicon and receive
Rice noodles/pucherite complex light anode；
A concentration of 10 ~ 80mM of five nitric hydrate bismuths in step S2, a concentration of 10 ~ 80mM of vanadyl acetylacetonate, acetic acid and second
The volume ratio of acyl acetone is（10~30）：（1~2）.
2. the preparation method of silicon nanowires/pucherite complex light anode according to claim 1, which is characterized in that step S1
Middle corroded in monocrystalline silicon sheet surface using metal Assisted Chemical Etching Process method or ion etching method vertical regular silicon nanowires battle array
Row, etchant solution are the mixed aqueous solution of silver nitrate and hydrofluoric acid, are cleaned after corrosion, the oxide skin(coating) for removing nanowire surface obtains
To vertical regular silicon nanowire array.
3. the preparation method of silicon nanowires/pucherite complex light anode according to claim 1, which is characterized in that step S1
Middle monocrystalline silicon piece is one kind in P-type silicon or N-type silicon.
4. the preparation method of silicon nanowires/pucherite complex light anode according to claim 2, which is characterized in that silver nitrate
A concentration of 0.01 ~ 0.05 M, hydrofluoric acid solution a concentration of 4 ~ 10M.
5. the preparation method of silicon nanowires/pucherite complex light anode according to claim 2, which is characterized in that corrosion
Time is 30 ~ 60min, and is corroded at normal temperatures.
6. the preparation method of silicon nanowires/pucherite complex light anode according to claim 1, which is characterized in that step S1
It is middle to use volume ratio for 3:1 concentrated sulfuric acid and hydrogen peroxide is cleaned, and the temperature of cleaning is 180 ~ 220 DEG C, using dense after cleaning
The hydrofluoric acid that degree is 2.5 ~ 3.5M removes oxide skin(coating).
7. the preparation method of silicon nanowires/pucherite complex light anode according to claim 1, which is characterized in that step S3
The number of plies of the middle precursor solution drop coating on silicon nanowires is 3 ~ 20 layers.
8. the preparation method of silicon nanowires/pucherite complex light anode according to claim 1, which is characterized in that step S4
The temperature of middle calcining is 450 ~ 650 DEG C, and time of calcining is 60 ~ 360min, the heating rate used in calcining for 5 ~ 10 DEG C/
min。
9. the silicon nanometer that the preparation method of any silicon nanowires/pucherite complex light anode of claim 1~8 is prepared
Line/pucherite complex light anode material.
10. silicon nanowires/application of the pucherite complex light anode in photochemical catalyzing described in claim 9.
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| CN109748320A (en) * | 2019-03-20 | 2019-05-14 | 广州大学 | A kind of monoclinic phase vanadium dioxide nano wire film and its preparation method and application |
| CN111809197A (en) * | 2020-07-21 | 2020-10-23 | 陕西师范大学 | Preparation method of porous bismuth vanadate film photo-anode |
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