CN108389727A - Semiconductors coupling heterojunction photovoltaic pole and preparation method thereof - Google Patents
Semiconductors coupling heterojunction photovoltaic pole and preparation method thereof Download PDFInfo
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- CN108389727A CN108389727A CN201810220254.2A CN201810220254A CN108389727A CN 108389727 A CN108389727 A CN 108389727A CN 201810220254 A CN201810220254 A CN 201810220254A CN 108389727 A CN108389727 A CN 108389727A
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
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Abstract
The present invention relates to a kind of preparation methods of semiconductors coupling heterojunction photovoltaic pole：Deposition thickness is the zinc-oxide film of 10 60nm in the conductive substrates of load pucherite nano thin-film, wherein zinc-oxide film, which is reacted by zinc source and oxygen source at 150 DEG C 200 DEG C, to be got；By treated, conductive substrates are put into copper salt solution, and displacement reaction occurs at 60 DEG C 100 DEG C, so that zinc oxide is transformed into copper oxide, then anneals at 350 DEG C 550 DEG C, forms the conductive substrates for loading and having pucherite and copper oxide hetero-junctions；Then there is the surface deposition of titanium oxide film of the conductive substrates of pucherite and copper oxide hetero-junctions in load, wherein titanium deoxid film, which is reacted by titanium source and oxygen source at 80 DEG C 150 DEG C, to be got.The hetero-junctions of the present invention has petal-shaped pattern, increases the specific surface area of electrode, the TiO of load2As co-catalyst, promotes hole and react with electrolyte, effectively raise photocatalytic water efficiency.
Description
Technical field
The present invention relates to photovoltaic electrodes technical field more particularly to a kind of semiconductors coupling heterojunction photovoltaic pole and its preparations
Method.
Background technology
Since 21 century, with the continuous development of society, energy shortage and environmental degradation two large problems gradually cause people
Attention, the two have become restrict human progress and social development biggest crisis.Wherein problem of energy crisis is more and more tighter
Weight, such as coal, oil, natural gas non-renewable energy resources are just in increasingly depleted.And it is big caused by various fossil fuels to burn
The let us mankind are also absorbed in the predicament that can not be extricated oneself by the global environmental degradation problem such as gas and water pollution, greenhouse effects.The world
Various countries in order to solve this problem all greatly develop it is novel using clean energy resource.In numerous regenerative resources, the sun
It can very be enriched with water, the energy of received solar radiation consumes the one of energy summation in 1 year by the current mankind on the earth
Wan Bei, but since solar energy metric density is low, restricted by destabilizing factors such as time, place and weathers, so solar energy
Utilization rate it is not high.Water is also a kind of compound most abundant on the earth, the whole world there are about 3/4ths area covering dampening,
The traditional approach such as power station are limited to more to the utilization of water energy at present.Therefore finding new ideal clean energy resource carrier becomes solution energy
One of source crisis most efficient method.
Hydrogen energy source is exactly the advantageous competitor of future source of energy carrier as up-and-coming youngster, and hydrogen can be generated by decomposition water,
And since the product after burning is water so that any pollution will not be generated.Therefore, photolysis water hydrogen system can be very good
This problem is solved, because the water decomposition of compound state can be generated free state by this system using solar energy as energy source
Hydrogen, so that unstable solar energy be stored in the form of Hydrogen Energy, both improved solar energy and water can utilization rate,
The reproducible hydrogen resource of cleaning can be generated again, be to kill two birds with one stone.Using the photocatalysis of semi-conducting material, will partly lead
System extremely provides new way using sunlight at the photoelectricity of photochemical cell to decompose water generation hydrogen.Preferably use light
Solution aqueous systems, which prepare hydrogen, becomes the ideal chose for solving energy energy shortage and two big crisis of environmental degradation.
The photoelectric material of the aquatic hydrogen producing of effective photodegradation should have following advantages：1, stronger light absorpting ability；
2, the presence that can stablize under any system；3, suitable band edge position is conducive to oxidation and the reduction reaction of water
It carries out；4, efficient carrier transport in body phase in the semiconductors；5, the global voltage transformation in redox reaction is relatively low；6、
Low cost；7, environmentally friendly.But there's almost no a kind of semi-conducting material at present can meet above-mentioned all advantages simultaneously,
Thus improve remaining aspect after meeting certain advantages is particularly important for improving the efficiency of photocatalytic water.
Existing research work is directed generally to improve the light absorption of optoelectronic pole and efficient carrier transmission.It is utilizable
Means have：1, element doping can usually enhance wide bandgap semiconductor materials to the absorption of visible light or promote narrow band gap light sun
The transmission of pole carrier, so as to improve the PEC performances of optoelectronic pole；2, the shape characteristic of photo-anode film is to photoelectrochemical cell point
The efficiency of Xie Shui also functions to very important effect.Especially monodimension nano stick, nanotube, nano wire and mesoporous and multistage knot
Structure, these structures can shorten the length of carrier transport, increase the specific surface area and enhancing light absorption of optoelectronic pole.3, surface
Processing includes cladding passivation layer and supports total, co-catalyst, and can not only increase quantum efficiency can also improve photoelectrochemical behaviour.
4, hetero-junctions is built to enhance light absorption, is inhibited the compound of electron hole pair, is accelerated separation and the electron-transport of carrier.But
The preparation method of current optoelectronic pole is more complex, and cost is higher, and prepared optoelectronic pole is not high to the utilization ratio of light, makes significantly
The about development in photocatalytic water field.
Invention content
In order to solve the above technical problems, the object of the present invention is to provide a kind of semiconductors coupling heterojunction photovoltaic pole and its systems
Preparation Method, method and process of the invention is simple, at low cost, and environmental protection, prepared optoelectronic pole has petal-shaped hetero-junctions, electrode ratio
It is larger compared with area, and load cocatalyst, effectively increase the utilization ratio to light.
The present invention provides a kind of preparation methods of semiconductors coupling heterojunction photovoltaic pole, include the following steps：
(1) pucherite (BiVO that thickness is 70nm-200nm is prepared in conductive substrates4) nano thin-film, form load vanadium
The conductive substrates of sour bismuth；
(2) atomic layer deposition (ALD) method is used, is 10nm- in the surface deposition thickness of the conductive substrates of load pucherite
Zinc oxide (ZnO) film of 60nm, wherein zinc-oxide film, which is reacted by zinc source and oxygen source at 150 DEG C -200 DEG C, to be got；
(3) will through step (2), treated, and conductive substrates are put into copper salt solution, replaced at 60 DEG C -100 DEG C
Reaction (preferably 80 DEG C), reaction time 15min-60min makes zinc oxide be transformed into copper oxide (CuO), then 350 DEG C-
Annealing 0.5h-5h (preferably 1h) under 550 DEG C (preferably 450 DEG C), forming load has leading for pucherite and copper oxide hetero-junctions
Electric substrate；The crystallinity of sample can be improved in annealing；
(4) atomic layer deposition method is used, has the surface of the conductive substrates of pucherite and copper oxide hetero-junctions to deposit in load
Thickness is the titanium dioxide (TiO of 0.5nm-10nm2) film, obtain semiconductors coupling heterojunction photovoltaic pole, wherein titanium dioxide
Film, which is reacted by titanium source and oxygen source at 80 DEG C -150 DEG C, to be got.
Further, in step (1), conductive substrates are fluorine-doped tin oxide electro-conductive glass (FTO), monocrystal silicon substrate
(Si) or indium doping fin oxide condutire glass (ITO).
Further, in step (1), the preparation method for loading the conductive substrates of pucherite includes the following steps：
1g-2g bismuth nitrates and 1g-3.8g citric acids are dissolved in 5ml-20mL nitric acid, 0.1g-0.8g metavanadic acids are then added
Ammonium is reacted, and after 0.2g-2g polyvinyl alcohol is added, is stirred 1h-24h, is obtained blue solution, be then coated to blue solution
Conductive substrates surface forms the conductive substrates of load pucherite after 300 DEG C of -550 DEG C of calcining 2h-24h.
Further, it is coated using spin coating method, spin speed is 1000-5000 revs/min, spin coating number of repetition
It is 2-6 times, changes the thickness of rotary speed and the controllable pucherite nano thin-film of number.
Further, in step (2), zinc source be diethyl zinc (DEZ), zinc methide and one kind in a zinc ethyl or
It is several.Preferably, zinc source is diethyl zinc.
Further, in step (2) and step (4), oxygen source is water or air.Preferably, oxygen source is deionized water.
In step (2), the thickness of ZnO film can be controlled by controlling the cycle-index of ALD method.
Further, in step (3), the mantoquita in copper salt solution is one in copper nitrate, copper sulphate and copper chloride
Kind is several.Preferably, mantoquita is copper nitrate.
Further, in step (3), a concentration of the 2 × 10 of copper salt solution-3mol/L-1×10-2mol/L.It is preferred that
Ground, a concentration of the 3.2 × 10 of copper salt solution-3mol/L。
It in step (3), using ZnO as sacrifice agent template, is reacted by replacing, the copper ion in copper salt solution is by ZnO
In zinc atom cement out, CuO and zinc ion are formed, to form BVO in substrate4/ CuO hetero-junctions, between being due to CuO
It is connected on BVO4It is formed on film, so being formed by hetero-junctions has petal-shaped pattern, increases the specific surface of final electrode
Product, enhances the sunken photosensitiveness of the electrode material of electrode material, and the optoelectronic pole for increasing the present invention connects in application with electrolyte
Contacting surface is accumulated.Simultaneously compared with traditional single material electrodes, the formation of hetero-junctions effectively promotes photohole and light induced electron
Separating capacity.
Further, in step (4), titanium source is isopropyl titanate or tetramethylammonium titanium.
Preferably, in step (4), TiO2The thickness of film is 0.5nm-1nm.
Co-catalyst TiO is introduced by step (4)2, hole can be effectively promoted and reacted with electrolyte, be conducive to
It improves electron hole pair to detach in electrode surface, by a series of enhancing, effectively raises photocatalytic water efficiency.
The present invention also provides the semiconductors coupling heterojunction photovoltaic poles prepared by a kind of above-mentioned preparation method, including conduction
Substrate, in conductive substrates load have pucherite and copper oxide hetero-junctions and titanium dioxide co-catalyst, pucherite and copper oxide
Hetero-junctions is in petal-shaped.
Compared to traditional unitary electrode, the efficiency of photocatalytic water carries significantly for the semiconductors coupling heterojunction photovoltaic pole of the present invention
Height, 8-40 times before photoelectric current is increased under the voltage of 1.23V.Therefore the electrode prepared by the method for the present invention is to improve
The practicable means of photodegradation water efficiency.
According to the above aspect of the present invention, the present invention has at least the following advantages：
Semiconductor photoelectrode prepared by the method for the present invention, which has, promotes optoelectronic pole surface chemical reaction, is conducive to improve half
The advantages that conducting electrons hole is to detaching.Simultaneously because the raising of photosensitiveness is fallen into caused by pattern and narrow bandgap semiconductor material,
The utilization ratio of light is also greatly improved.Compared with the single semi-conducting electrode of tradition, the composite heterogenous junction prepared in the present invention is electric
Pole also overcomes the shortcomings of serious electron-hole recombinations existing for single semi-conducting electrode, carrier mobility energy force difference, effectively
Improve photocatalytic water efficiency, and this method preparation process has fairly simple, the advantages such as raw material are sufficient, price is low.Favorably
In large-scale production, there is huge potential using value.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, below with presently preferred embodiments of the present invention and after coordinating attached drawing to be described in detail such as.
Description of the drawings
Fig. 1 is the SEM (scanning electron microscope) of the semiconductors coupling heterojunction photovoltaic pole prepared by the embodiment of the present invention 1
Figure；
Fig. 2 is the performance diagram of photodegradation water of the Different electrodes under different voltages prepared by the present invention.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.
The present invention provides a kind of technology of preparing of semiconductors coupling heterojunction photovoltaic pole, by by two kinds of semi-conducting materials
The method for constituting hetero-junctions and composite catalyst is prepared.Specific method is to first pass through spin-coating method in FTO electro-conductive glass
On obtain vanadic acid bismuth thin film, by annealing process improve sample crystallinity.Then by the method for atomic layer deposition in vanadic acid
Zinc oxide is then converted to copper oxide by ion-exchange, obtains BiVO by developing zinc oxide on bismuth thin film4/ CuO compound electrics
Combination electrode is finally obtained BiVO by pole by the method for atomic layer deposition4/CuO/TiO2Optoelectronic pole.Implement below the present invention
In example, it is used as to electrode, with the sulfuric acid of 0.5M using the electrode material of preparation as the working electrode of photoelectrochemical cell, platinum electrode
Sodium (Na2SO4) aqueous solution as electrolyte, carries out photodegradation water experiment.
Embodiment 1
(1) using FTO as conductive substrates, by conductive substrates according to acetone, the sequence of absolute ethyl alcohol and deionized water is super
Respectively it is cleaned by ultrasonic in sound machine 30 minutes.
By five nitric hydrate bismuths of 1.6169g, 1.2808g anhydrous citric acids are dissolved in 10mL nitric acid (concentration 23.3%),
Continue stirring until uniform mixing.0.39g ammonium metavanadates are dissolved in above-mentioned solution and are stirred, wait for that solution is completely dissolved, are added
It is stirred 5 hours after 0.4g polyvinyl alcohol (PVA), obtains transparent blue solution.
Cleaned conductive substrates are placed on spin coating instrument, take appropriate transparent blue solution to drop in conductive substrates with liquid-transfering gun
On, vanadic acid bismuth thin film is obtained by way of spin coating, spin speed is 4000 revs/min, which recycles 5 times.Spin coating is good
Conductive substrates in the lehr 400 DEG C calcine 5 hours, heating rate be two degrees it is per minute.It is born after Temperature fall cooling
The conductive substrates of vanadic acid bismuth thin film are carried, the thickness of vanadic acid bismuth thin film is 120nm or so.
(2) the step of obtaining (1) processed conductive substrates are put into the cavity of atomic layer deposition, using DEZ as
Zinc source, deionized water is as oxygen source, and control reaction cavity temperature is 200 DEG C, in BiVO4Film surface prepares zinc-oxide film,
Form BiVO4/ ZnO samples.The zinc oxide thickness of preparation is 40nm.
0.302g Gerhardites are dissolved in 500ml deionized waters and obtain copper nitrate solution.By BiVO4/ ZnO samples
Product are put into the copper nitrate solution just prepared, then react 45min in 80 DEG C of water-bath, and ZnO is converted into CuO.For
The crystallinity for improving sample, finally needs the sample of drying being put into annealing furnace and be calcined 1 hour at 450 DEG C, heating rate is
Five degree per minute.BiVO is obtained after Temperature fall4/ CuO samples.
(3) by BiVO4/ CuO samples are put into the cavity of atomic layer deposition, using isopropyl titanate or tetramethylammonium titanium as
Titanium source, for deionized water as oxygen source, control reaction cavity temperature is 150 DEG C, prepares the TiO of 0.5nm thickness2Film finally obtains
BiVO4/CuO/TiO2Combination electrode, as semiconductors coupling heterojunction photovoltaic pole.
BiVO4/CuO/TiO2The pattern of combination electrode is as shown in Figure 1.As can be seen from Figure 1 it is grown on vanadic acid bismuth thin film
A large amount of petal-like copper oxide.The pattern makes the specific surface area of electrode become larger, and is conducive to the promotion of photocatalytic water efficiency.
The optoelectronic pole of above-mentioned preparation is assembled into photoelectrochemical cell, then the photodegradation water under different voltages.In order to
As a contrast, while to load BiVO4The FTO of the film and BiVO prepared according to the method described above4/ CuO samples are respectively as work
Make electrode, platinum guaze as to electrode, photodegradation water, is as a result shown in Fig. 2 under identical condition.As can be seen from Figure 2,1.23V's
Under voltage, dark current (dotted line in figure) can be ignored substantially, and the photoelectric current of the optoelectronic pole prepared by the method for the present embodiment can be with
Reach 0.479mA/cm2；And BiVO4Film and BiVO4The photoelectric current of/CuO only has 0.013mA/cm2And 0.299mA/cm2。
Embodiment 2
BiVO is prepared according to the method for 1 step of embodiment (1)-(3)4/CuO/TiO2Combination electrode, difference lies in step
(3) in, the TiO of different recurring numbers is deposited by controlling ALD technique2Program, to obtain the TiO of different-thickness2So that step
(3) TiO in2Thickness is 1nm.
The optoelectronic pole of above-mentioned preparation is assembled into photoelectrochemical cell, then the photodegradation water under different voltages.
Under the voltage of 1.23V, the photoelectric current of the optoelectronic pole prepared by the method for the present embodiment can reach 0.412mA/cm2；And with
BiVO4/ CuO samples only have 0.299mA/cm as the photoelectric current of working electrode2。
Embodiment 3
BiVO is prepared according to the method for 1 step of embodiment (1)-(3)4/CuO/TiO2Combination electrode, difference lies in steps
(2) water-bath time in is 15min, so that ZnO is converted into the reaction time difference of this step of CuO, is obtained and real
Applying example 1 has the CuO petal-shaped patterns of different densities.
The optoelectronic pole of above-mentioned preparation is assembled into photoelectrochemical cell, then the photodegradation water under different voltages.
Under the voltage of 1.23V, the photoelectric current of the optoelectronic pole prepared by the method for the present embodiment can reach 0.38mA/cm2；And with
BiVO4/ CuO samples only have 0.2mA/cm as the photoelectric current of working electrode2。
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of semiconductors coupling heterojunction photovoltaic pole, which is characterized in that include the following steps：
(1) the pucherite nano thin-film that thickness is 70-200nm is prepared in conductive substrates, forms the conductive base of load pucherite
Bottom；
(2) atomic layer deposition method is used, is 10nm-60nm's in the surface deposition thickness of the conductive substrates of the load pucherite
Zinc-oxide film, wherein the zinc-oxide film, which is reacted by zinc source and oxygen source at 150 DEG C -200 DEG C, to be got；
(3) will through step (2), treated, and conductive substrates are put into copper salt solution, it is anti-that displacement occurs at 60 DEG C -100 DEG C
It answers, zinc oxide is made to be transformed into copper oxide, then anneal at 350 DEG C -550 DEG C, forming load has pucherite and copper oxide heterogeneous
The conductive substrates of knot；
(4) atomic layer deposition method is used, has the surface of the conductive substrates of pucherite and copper oxide hetero-junctions to deposit in the load
Thickness is the titanium deoxid film of 0.5-10nm, obtains semiconductors coupling heterojunction photovoltaic pole, wherein the titanium dioxide
Film, which is reacted by titanium source and oxygen source at 80 DEG C -150 DEG C, to be got.
2. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 1 pole, it is characterised in that：In step
(1) in, the conductive substrates are fluorine-doped tin oxide electro-conductive glass, monocrystal silicon substrate or indium doping fin oxide condutire glass.
3. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 1 pole, which is characterized in that in step
(1) in, the preparation method of the conductive substrates of the load pucherite includes the following steps：
Bismuth nitrate and citric acid are dissolved in nitric acid, ammonium metavanadate is then added and is reacted, after polyvinyl alcohol is added, obtains blue
Then the blue solution is coated to conductive substrates surface by solution, the load vanadic acid is formed after 300 DEG C of -550 DEG C of calcinings
The conductive substrates of bismuth.
4. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 3 pole, it is characterised in that：Respectively with body
The ratio of product and quality meter, the nitric acid and polyvinyl alcohol is 5ml-20mL：0.2g-2g.
5. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 1 pole, it is characterised in that：In step
(2) in, the zinc source is one or more of diethyl zinc, zinc methide and a zinc ethyl.
6. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 1 pole, it is characterised in that：In step
(2) and in step (4), the oxygen source is water or air.
7. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 1 pole, it is characterised in that：In step
(3) in, the mantoquita in the copper salt solution is one or more of copper nitrate, copper sulphate and copper chloride.
8. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 1 pole, it is characterised in that：In step
(3) in, a concentration of the 2 × 10 of the copper salt solution-3mol/L-1×10-2mol/L。
9. the preparation method of semiconductors coupling heterojunction photovoltaic according to claim 1 pole, it is characterised in that：In step
(4) in, the titanium source is isopropyl titanate or tetramethylammonium titanium.
10. the semiconductors coupling heterojunction photovoltaic pole prepared by the preparation method described in a kind of any one of claim 1-9,
It is characterized in that：Being loaded including conductive substrates, in the conductive substrates has pucherite and copper oxide hetero-junctions and titanium dioxide to help
Catalyst, the pucherite and copper oxide hetero-junctions are in petal-shaped.
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