CN107513723B - A method of it reducing Ni/n-Si light anode optical electro-chemistry and decomposes water unlatching current potential - Google Patents
A method of it reducing Ni/n-Si light anode optical electro-chemistry and decomposes water unlatching current potential Download PDFInfo
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- CN107513723B CN107513723B CN201710949886.8A CN201710949886A CN107513723B CN 107513723 B CN107513723 B CN 107513723B CN 201710949886 A CN201710949886 A CN 201710949886A CN 107513723 B CN107513723 B CN 107513723B
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Abstract
The invention discloses a kind of reduction Ni/n-Si light anode optical electro-chemistry to decompose the method that water opens current potential, by carrying out a simple rapid thermal treatment process to the Ni/n-Si light anode of preparation, reduce the interfacial state being present between the interface Ni/n-Si, relieve fermi level pinning effect caused by these interfacial states, it improves Ni/n-Si and is formed by schottky barrier height, to which Ni/n-Si light anode generates higher photovoltage in illumination, eventually reduces Ni/n-Si light anode optical electro-chemistry and decompose water unlatching current potential.The method that reduction Ni/n-Si light anode optical electro-chemistry decomposes water unlatching current potential is easy to operate, low in cost, is suitble to large-scale application into metal/n-Si light anode system, and the development and application for decomposing water technology for promotion optical electro-chemistry are with positive effect.
Description
Technical field
The present invention relates to PhotoelectrochemicalTechnique Technique fields, and in particular to a kind of reduction Ni/n-Si light anode optical electro-chemistry decomposition
The method of water unlatching current potential.
Background technique
Optical electro-chemistry, which decomposes water, can realize the green conversion of solar energy to Hydrogen Energy, it is considered to be solve increasingly serious at present
A kind of effective means of energy crisis and problem of environmental pollution.Optical electro-chemistry decompose the complete electrochemical reaction of water include produce hydrogen and
Two half-reactions of oxygen are produced, hydrogen reaction is produced and occurs in photocathode, oxygen reaction is produced and occurs in light anode.Wherein, oxygen reaction is produced due to same
When need 4 electronics to participate in reaction and be more difficult to realize.Therefore, developing high performance optical anode material is to realize solar energy highly effective light
The key of electrochemical decomposition water.
Si is the element abundant of reserves second on the earth, has suitable level of energy and high carrier mobility,
It is considered as thus a kind of ideal optical anode material.However, silicon is easy to occur as light anode when with electrolyte contacts
Anodic attack, and it is very slow in the dynamic process that the surface Si produces oxygen reaction.One layer is deposited on Si, and there is production oxygen to urge
Change active metal (such as Ni), Si can not only be protected not corroded very well, and can also greatly improve and produce oxygen reaction rate.But
It is that, when Ni is deposited on the surface Si in the interface Ni/Si there are a large amount of defect, these defects lead to the interface Ni/Si
Interface state density is higher.These highdensity interfacial states will cause very strong fermi level pinning, cause to be formed between Ni/n-Si
Low Schottky barrier.And the photovoltage that Ni/n-Si light anode is generated in illumination is strongly depend on schottky barrier height.
Low Schottky barrier causes Ni/n-Si light anode to generate low photovoltage, thus optical electro-chemistry decompose water open current potential compared with
Height needs the external world to provide higher energy again and realizes decomposition water.This is very to being able to achieve optical electro-chemistry to decompose water using the sun
Unfavorable.
Want that the photovoltage for improving Ni/n-Si light anode decomposes water unlatching current potential to reduce its optical electro-chemistry, reduces this
A little interfacial states are particularly important with eliminating fermi level pinning just.
Be based on this importance, the invention proposes by Ni/n-Si light anode in N2Under atmosphere at fast speed heat
Reason reduces the interfacial state at the interface Ni/Si, so that reducing optical electro-chemistry decomposes the new method that water opens current potential.
Summary of the invention
Based on the above technical problem, the present invention provides a kind of reduction Ni/n-Si light anode optical electro-chemistry decomposition water unlatching electricity
Position method, by Ni/n-Si light anode in N2Rapid thermal treatment reduces the interfacial state at the interface Ni/n-Si under atmosphere, thus
It reduces optical electro-chemistry and decomposes water unlatching current potential.
To achieve the above object, the invention adopts the following technical scheme:
A method of it reducing Ni/n-Si light anode optical electro-chemistry and decomposes water unlatching current potential, which is characterized in that by Ni/n-
Si light anode carries out rapid thermal treatment.
In preferred embodiment provided by the invention, specifically includes the following steps:
Ni/n-Si light anode is put into rapid heat-treatment furnace, in the case where inertia protects gas atmosphere, heating is carried out at fast speed heat
Reason.
Preferably, the inertia protection gas is nitrogen.
Preferably, the temperature of the rapid thermal treatment is 450-550 DEG C.It is highly preferred that the temperature of the rapid thermal treatment
It is 450 DEG C.
Preferably, the heating rate of the heating is 20-60 DEG C/s.It is highly preferred that the heating rate of the heating is 30
℃/s。
Preferably, time 30-60 second of the rapid thermal treatment；Wherein rapid thermal annealing time does not include heating institute's used time
Between.
Beneficial effects of the present invention
The Ni/n-Si light anode optical electro-chemistry provided by the invention that reduces decomposes the method that water opens current potential, by preparation
Ni/n-Si light anode carry out a simple rapid thermal treatment process, reduce the interface being present between the interface Ni/n-Si
State relieves fermi level pinning effect caused by these interfacial states, improves Ni/n-Si and is formed by Schottky barrier height
It is photoelectrochemical to eventually reduce Ni/n-Si light anode so that Ni/n-Si light anode generates higher photovoltage in illumination for degree
Credit Xie Shui opens current potential.The method that reduction Ni/n-Si light anode optical electro-chemistry decomposes water unlatching current potential is easy to operate, cost
It is cheap, be suitble to large-scale application into metal/n-Si light anode system, for promote optical electro-chemistry decompose water technology development with
Using with positive effect.
Detailed description of the invention
It is not heat-treated Ni/n- in Ni/n-Si light anode and embodiment 1 in Fig. 1 embodiment of the present invention 2 through Overheating Treatment
The XRD of Si light anode compares spectrogram；
It is not heat-treated Ni/n- in Ni/n-Si light anode and embodiment 1 in Fig. 2 embodiment of the present invention 2 through Overheating Treatment
The cross section TEM comparison diagram of Si light anode；
It is not heat-treated Ni/n- in Ni/n-Si light anode and embodiment 1 in Fig. 3 embodiment of the present invention 2 through Overheating Treatment
The C-V curve comparison diagram of Si light anode；
It is not heat-treated Ni/n- in Ni/n-Si light anode and embodiment 1 in Fig. 4 embodiment of the present invention 3 through Overheating Treatment
The C-V curve comparison diagram of Si light anode；
It is not heat-treated Ni/n- in Ni/n-Si light anode and embodiment 1 in Fig. 5 embodiment of the present invention 4 through Overheating Treatment
The C-V curve comparison diagram of Si light anode；
It is not heat-treated Ni/n- in Ni/n-Si light anode and embodiment 1 in Fig. 6 comparative example 1 of the present invention through Overheating Treatment
The C-V curve comparison diagram of Si light anode.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that the present embodiment is served only for pair
The present invention is further described, and should not be understood as limiting the scope of the invention, and the person skilled in the art in the field can
To make some nonessential modifications and adaptations according to the content invented above.In the absence of conflict, the reality in the present invention
The feature applied in example and embodiment can be combined with each other.
Embodiment 1
N-shaped resistivity by P doping is that 0.8-1 Ω cm single crystalline Si piece is first soaked in H2SO4: H2O2Volume ratio is 3:1
Solution in cleaned within 10 minutes, then in H2O:HCl:H2O2Volume ratio is to impregnate 10 points in the solution of 5:1:1 at 75 DEG C
Clock is cleaned.Sample after cleaning is impregnated to 10 seconds removal surface oxide layers in 4% dilute HF solution.Surface oxidation will be removed
The silicon wafer of layer is immediately placed in e-beam evaporation chamber, and it is 2 × 10 that holding chamber temp, which is 50 DEG C of vacuum degrees,-4Pa.WithIt is heavy
Product rate electron beam hydatogenesis about 20nm Ni film on silicon wafer, obtains Ni/n-Si light anode.
Embodiment 2
Ni/n-Si light anode prepared by embodiment 1 is put into rapid heat-treatment furnace, in high-purity N2Under atmosphere, at 450 DEG C
Lower rapid thermal treatment 30 seconds, wherein heating rate is 30 DEG C/s.Being heat-treated 30 second time does not include the time used in temperature-rise period.?
Ni/n-Si light anode after to rapid thermal treatment.
Front and back Ni/n-Si light anode XRD diagram and cross section TEM figure are heat-treated we can observe that at heat by comparison
The variation of reason front and back Ni/n-Si light anode object phase and structure.Fig. 1 is that Ni/n-Si is heat-treated front and back XRD diagram, by comparing me
It can be found that the diffraction maximum of Ni becomes sharply after heat treatment, half-peak breadth narrows, and illustrates the crystallinity raising of Ni after heat treatment.
Fig. 2 (a) and (b) are respectively to scheme before being heat-treated with Ni/n-Si light anode cross section TEM after heat treatment.Pass through comparison
We can be found that being heat-treated preceding Ni film is that there are many little crystal grains of each crystal orientation to form, these small crystal grain after heat treatment
Become the big crystal grain of single crystal orientation.
Ni/n-Si light anode heat treatment front and back C-V curve is as shown in figure 3, we can be found that Ni/n-Si light after heat treatment
Anode, which opens current potential, an apparent negative shifting, and negative shifting degree is about 150mV.This just illustrates us by implementing to Ni/n-Si
One rapid thermal treatment process can significantly reduce its optical electro-chemistry and decompose water unlatching current potential.
Embodiment 3
Ni/n-Si light anode prepared by embodiment 1 is put into rapid heat-treatment furnace, in high-purity N2Under atmosphere, at 550 DEG C
Rapid thermal treatment 30 seconds, wherein heating rate was 30 DEG C/s.Being heat-treated 30 second time does not include the time used in temperature-rise period.It obtains
Ni/n-Si light anode after rapid thermal treatment.
Ni/n-Si light anode heat treatment front and back C-V curve is as shown in figure 4, we can be found that Ni/n-Si light after heat treatment
Anode unlatching current potential is negative to have moved 100mV.
Embodiment 4
Ni/n-Si light anode prepared by embodiment 1 is put into rapid heat-treatment furnace, in high-purity N2Under atmosphere, at 550 DEG C
Rapid thermal treatment 60 seconds, wherein heating rate was 30 DEG C/s.Being heat-treated 60 second time does not include the time used in temperature-rise period.It obtains
Ni/n-Si light anode after rapid thermal treatment.
Ni/n-Si light anode heat treatment front and back C-V curve is as shown in figure 5, we can be found that Ni/n-Si light after heat treatment
Anode unlatching current potential is negative to have moved 80mV.
Embodiment 5
Ni/n-Si light anode prepared by embodiment 1 is put into rapid heat-treatment furnace, in high-purity N2Under atmosphere, at 550 DEG C
Rapid thermal treatment 60 seconds, wherein heating rate was 20 DEG C/s.Being heat-treated 60 second time does not include the time used in temperature-rise period.It obtains
Ni/n-Si light anode after rapid thermal treatment.
Embodiment 6
Ni/n-Si light anode prepared by embodiment 1 is put into rapid heat-treatment furnace, in high-purity N2Under atmosphere, at 550 DEG C
Rapid thermal treatment 30 seconds, wherein heating rate was 60 DEG C/s.Being heat-treated 30 second time does not include the time used in temperature-rise period.It obtains
Ni/n-Si light anode after rapid thermal treatment.
Comparative example 1
Ni/n-Si light anode prepared by embodiment 1 is put into rapid heat-treatment furnace, quick heat treatment method step is the same as implementation
Example 2, difference is: rapid heat-treatment temperature is 800 DEG C.
Ni/n-Si light anode heat treatment front and back C-V curve is as shown in fig. 6, we can be found that when heat treatment temperature is 800
DEG C when, open current potential become than calibration, photoelectric current becomes smaller, Ni/n-Si light anode degradation.This explanation works as rapid thermal treatment temperature
When spending high, it cannot not only reduce Ni/n-Si light anode and open current potential, but also entire performance is also deteriorated.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (4)
1. a kind of Ni/n-Si light anode optical electro-chemistry that reduces decomposes the method that water opens current potential, which is characterized in that by Ni/n-Si
Light anode carries out rapid thermal treatment；Ni/n-Si light anode is subjected to rapid thermal treatment the following steps are included: by Ni/n-Si light sun
Pole is put into rapid heat-treatment furnace, and in the case where inertia protects gas atmosphere, heating carries out rapid thermal treatment；
The heating rate of the heating is 20-60 DEG C/s；Time 30-60 second of the rapid thermal treatment；The rapid thermal treatment
Temperature be 450-550 DEG C；Wherein rapid thermal annealing time does not include the time used of heating up.
2. the method according to claim 1, wherein inertia protection gas is nitrogen.
3. the method according to claim 1, wherein the temperature of the rapid thermal treatment is 450 DEG C.
4. the method according to claim 1, wherein the heating rate of the heating is 30 DEG C/s.
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