CN107541724A - A kind of preparation method of the controllable metal-oxide film of pattern and composition - Google Patents
A kind of preparation method of the controllable metal-oxide film of pattern and composition Download PDFInfo
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- CN107541724A CN107541724A CN201610473674.2A CN201610473674A CN107541724A CN 107541724 A CN107541724 A CN 107541724A CN 201610473674 A CN201610473674 A CN 201610473674A CN 107541724 A CN107541724 A CN 107541724A
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Abstract
The present invention relates to photoelectrochemical cell field, the preparation method of the controllable metal-oxide film of specially a kind of pattern and composition.Using sheet metal or alloy sheet as matrix, amorphous metal oxide is generated in sheet metal or alloy substrates surface in situ using chemical attack oxidation；The amorphous metal oxide film of acquisition is subjected to crystallization and thermal treatment under different oxygen partial pressures, pattern and the controllable metal-oxide film of composition are obtained by regulating and controlling heat treatment temperature and time.The present invention passes through the oxygen partial pressure during regulating and controlling crystallization and thermal treatment, it is in situ on metallic matrix to obtain specific morphology and the method for component adjustable metal sull, the pattern and composition of metal-oxide film are two important parameters of photochemistry moisture electrolytic cell light electrode material, directly affect the final transformation efficiency of photoelectrochemical cell.The present invention is in situ on metallic matrix to obtain specific morphology and composition adjustable metal sull by regulating and controlling atmosphere and partial pressure in heat treatment process.
Description
Technical field
The present invention relates to photoelectrochemical cell field, the controllable metal oxide of specially a kind of pattern and composition is thin
The preparation method of film.
Background technology
Optical electro-chemistry moisture electrolytic cell is one of effective way of solar energy conversion and storage, and it is by solar energy with hydrogen
The form of key fixes conversion.Optoelectronic pole is the core component of photoelectrochemical cell, and it absorbs incident solar energy
And water decomposition reaction is induced to realize sun transformation of energy and storage.Metal oxide has high stability, height living
Property and it is inexpensive the advantages that, be a kind of preferably semiconductor photoelectrode material.
Surface atom/electronic structure of metal oxide directly determines the surface transfer process of photogenerated charge, final shadow
Ring the quantum conversion of optoelectronic pole.Metal-oxide semiconductor (MOS) difference crystal face has different surface atom/electronics
Structure, shows different photocatalytic activities, and usual high energy crystal face has higher photocatalytic activity.Meanwhile
Lattice surface defect can also modulate surface atom/electronic structure simultaneously, directly affect final quantum conversion.
By modulating surface atom/electronic structure, obtain particular crystal plane exposure and component can modulation metal-oxide film
The surface transfer efficiency of photogenerated charge can be effectively improved, it has high solar energy conversion quantum effect as optoelectronic pole
Rate.Therefore, prepare particular crystal plane exposure and component can the metal-oxide film optoelectronic pole of modulation be that structure is efficient
Optical electro-chemistry decomposes a kind of effective means of water battery.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the controllable metal-oxide film of pattern and composition,
It is in situ on metallic matrix to obtain specific morphology and composition by regulating and controlling atmosphere and partial pressure in heat treatment process
Adjustable metal sull.
The technical scheme is that：
The preparation method of the controllable metal-oxide film of a kind of pattern and composition, first, with sheet metal or alloy
Piece is matrix, and amorphous metal oxide is generated in sheet metal or alloy substrates surface in situ using chemical attack oxidation；
Then, the amorphous metal oxide film of acquisition is subjected to crystallization and thermal treatment under different oxygen partial pressures, passes through tune
Controlling heat treatment temperature and time obtains pattern and the controllable metal-oxide film of composition.
Described metal substrate is Fe, Ta, Ti, W, Zn, Cu or Co, described alloy substrates be Ti/Al,
Cu/Zn, Ti/Fe, Ti/W or Ti/Ta alloy.
Described chemical attack is oxidized to various metal erosion oxidizing process, rotten using chemical solution burn into air
Erosion or electrochemical oxidation corrosion.
Described crystallization and thermal treatment temperature is 300~1000 DEG C, and programming rate is 0.1~10 DEG C/min, during crystallization
Between be 0.5~48 hour.
The preparation method of the controllable metal-oxide film of described pattern and composition, it is preferred that described crystallization
Heat treatment temperature is 500~800 DEG C, and programming rate is 1~5 DEG C/min, and crystallization time is 1~24 hour.
Described Crystallizing treatment oxygen partial pressure is 0~105Pa。
The preparation method of the controllable metal-oxide film of described pattern and composition, it is preferred that described crystallization
Processing oxygen partial pressure is 0~1000Pa.
The present invention design philosophy be：
The present invention (closes using metal (or alloy) piece as matrix, by (electricity) chemical attack oxidation in metal
Gold) it is in situ on matrix obtain amorphous metal oxide film, regulate and control noncrystal membrane crystallization and thermal treatment atmosphere and point
Pressure, it is in situ on metal (alloy) matrix to obtain specific morphology and component adjustable metal sull：Profit
With the difference of metal oxide crystal Thermodynamically stable configuration under different partial, the amorphous metal of acquisition is aoxidized
Thing film carries out crystallization and thermal treatment under different oxygen partial pressures, and spy is can obtain by adjusting heat treatment temperature and time
Determine the metal-oxide film of crystal face exposure；Utilize the metallic matrix reduction to metal-oxide film at high temperature
Effect, by the amorphous metal oxide film of acquisition under anaerobic environment (such as：Under argon gas atmosphere) carry out crystallization
Processing, the metal-oxide film of heterogeneity can be obtained by adjusting heat treatment temperature and time.
Advantages of the present invention and beneficial effect are：
1st, the present invention utilizes (electricity) chemical attack method for oxidation in-situ oxidation on metal (alloy) matrix to carve
Erosion growth amorphous metal oxide film, easily realizes the preparation of various amorphous metal oxide films.
2nd, the present invention, can by the partial pressure of oxygen during simply regulating and controlling amorphous metal oxide film Crystallizing treatment
Pattern and composition adjustable metal (oxygen) nitride film are obtained, can Effective Regulation its photoelectrocatalysis decomposition water work
Property.
Brief description of the drawings
Fig. 1 amorphous TiO2The preparation process schematic diagram (a-b) and respective scanned electron microscope (SEM) of film
Photo (c-d).
Fig. 2 rutile TiO2Nano-pillar crystal array SEM photograph：(a) macrograph, (b) high power top
Photo and (c) high power side photo, the illustration schemed in (c) is rutile TiO2Thermodynamically stable configuration (Wulff
Configuration) schematic diagram.
Fig. 3 rutile TiO2Nano-pillar transmission electron microscope (TEM) photo：(A) single nano-pillar is low
Times photo, (B) high-resolution TEM photos and (C) choose electron diffraction spot.
Fig. 4 rutile TiO2Nano-pillar crystal array optoelectronic pole and traditional anatase TiO2Nanotube optoelectronic pole
Optical electro-chemistry decomposition water active testing：(a) rutile TiO2Test curve under nano-pillar crystal array dark-state, (b)
Traditional anatase TiO2Test curve under nanotube dark-state, (c) rutile TiO2Nano-pillar crystal array illumination
Lower test curve, (d) traditional anatase TiO2Test curve under nanotube illumination.X-axis is applied voltage (volt
/ V), Y-axis is density of photocurrent (mAcm-2)。
Fig. 5 stoichiometric proportions and non-stoichiometric rutile TiO2The x-ray photoelectron power spectrum of film
(XPS) element depth analysis (a) and element depth distribution (b-c) schematic diagram.X-axis is sputtering time (second/s),
Y-axis is O/Ti atomic ratios.
Fig. 6 stoichiometric proportion rutile TiO2Film photoelectric electrode and non-stoichiometric rutile TiO2Film light
The optical electro-chemistry decomposition water active testing of electrode：(a) stoichiometric proportion rutile TiO2Tested under film dark-state bent
Line, (b) non-stoichiometric rutile TiO2Film, (c) stoichiometric proportion rutile TiO2Film light shines
Lower test curve, (d) non-stoichiometric rutile TiO2Film shines lower test curve.X-axis is applied voltage
(volt/V), Y-axis are density of photocurrent (mAcm-2)。
Embodiment
In specific implementation process, the present invention utilizes (electricity) chemical attack oxidation on metal (alloy) matrix
Growth in situ amorphous metal oxide film, specific morphology is obtained by regulating and controlling the partial pressure of oxygen during Crystallizing treatment
The method of controllable metal-oxide film with composition.Using metal (alloy) piece as matrix, pass through (electricity) first
Chemical attack oxidation is in situ on metal (alloy) matrix to obtain amorphous metal oxide film；Utilize different oxygen
The difference of metal oxide crystal Thermodynamically stable configuration and metallic matrix aoxidize to metal at high temperature under partial pressure
The reduction of thing film, the amorphous metal oxide film of acquisition is carried out to crystallization heat under different oxygen partial pressures
Processing, by adjusting heat treatment temperature and the time can obtain specific morphology and the controllable metal-oxide film of composition,
It is specific as follows：
1st, described substrate is various metals and alloy substrates, including various simple metal pieces are (such as：Fe、Ta、
Ti, W, Zn, Cu, Co etc.) and various alloy sheets are (such as：Ti/Al、Cu/Zn、Ti/Fe、Ti/W、Ti/Ta
Alloy etc.).
2nd, described (electricity) chemical attack is oxidized to various metal erosion oxidizing process, including chemical solution burn into
Atmospheric corrosion and electrochemical oxidation corrosion etc..
3rd, described crystallization and thermal treatment temperature is 300~1000 DEG C, and programming rate is 0.1~10 DEG C/min, brilliant
It is 0.5~48 hour to change the time.
4th, described Crystallizing treatment oxygen partial pressure scope is 0~105Pa。
The present invention is further elaborated on reference to embodiment and accompanying drawing.
Embodiment 1
By Titanium (Ti) piece (long 1cm × wide 2.5cm) respectively in deionized water, ethanol, acetone, different
It is cleaned by ultrasonic 15 minutes in propyl alcohol, positive source is connected to after drying, Pt pieces are connected to negative pole, and insert
Enter to containing NH4F (2~5wt%) ethylene glycol and water (volume ratio 9：1) in mixed solution.Apply constant
Voltage 60V is kept for 6 hours, and TiO is generated in the anodic oxidation of metal titanium sheet surface in situ2Nano-tube array, so
Titanium sheet is taken out afterwards and is put into ultrasound in hydrogen peroxide, gets rid of the TiO on surface2Nano-tube array obtains bottom densification
Amorphous TiO2Film (Fig. 1).By obtained amorphous dense film, Crystallizing treatment, oxygen divide under oxygen atmosphere
Voltage-controlled system is incubated crystallization 2h at 1000Pa, 550 DEG C, and programming rate is 5 DEG C/min, obtains rutile TiO2
Nanometer monocrystalline post array, top expose high energy (111) and (101) crystal face (Fig. 2).Because high energy is brilliant
Face has higher water oxidation activity, the rutile TiO being prepared2Nanometer monocrystalline post array is as optical electro-chemistry
Water decomposition battery light anode has excellent activity.
As shown in figure 1, TiO is obtained by electrochemical anodic oxidation Ti pieces2Nano-tube array (a), further
The TiO on top layer is got rid of by ultrasound stripping2Nanometer is in control amorphous TiO2Dense film (b).
As shown in Fig. 2 after being handled 2 hours under the conditions of 550 DEG C, 1000Pa oxygen partial pressures, swept from low power
Retouch in electromicroscopic photograph, farmland area TiO can be observed2Crystal array (a)；On high power top (b) and side (c)
In surface sweeping electromicroscopic photograph, it is observed that it is the rutile TiO of particular crystal plane exposure2Nano-pillar array structure,
By being contrasted with Thermodynamically stable configuration (Wulff configurations), top exposure crystal face is (101) and (111)
Crystal face, side are (110) crystal face.
As shown in figure 3, the complete single nano-pillar low power transmission electron microscope photo (A) of crystal face development, with reference to receiving
Meter Zhu high-resolution-ration transmission electric-lens photo (B) and SEAD photo (C) proves single nano-pillar for list
Crystal structure.
As shown in figure 4, in the dark state, rutile TiO2Nanometer monocrystalline post array (a) and anatase TiO2Receive
The anhydrous decomposition current-responsive of mitron array (b)；Under light illumination, with traditional anatase TiO2Nano-tube array
Photoelectric current (d) compare, rutile TiO2Nanometer monocrystalline post array (c) shows more excellent optical electro-chemistry
Water dispersible energy.
Embodiment 2
By Titanium (Ti) piece (long 1cm × wide 2.5cm) respectively in deionized water, ethanol, acetone, different
It is cleaned by ultrasonic 15 minutes in propyl alcohol, positive source is connected to after drying, Pt pieces are connected to negative pole, and insert
Enter to containing NH4F (2~5wt%) ethylene glycol and water (volume ratio 9：1) in mixed solution.Apply constant
Voltage 60V is kept for 6 hours, and TiO is generated in the anodic oxidation of metal titanium sheet surface in situ2Nano-tube array, so
Titanium sheet is taken out afterwards and is put into ultrasound in hydrogen peroxide, gets rid of the TiO on surface2Nano-tube array obtains bottom densification
Amorphous TiO2Film (Fig. 1).By obtained amorphous dense film in anaerobic gas atmosphere (Ar or N gas atmosphere)
Lower Crystallizing treatment, oxygen partial pressure 0Pa, 2h is incubated at 550 DEG C, using Titanium under high temperature to TiO2Also
Original work are used, and obtain non-stoichiometric rutile TiO2Film.Compared to (oxygen partial pressure amount in air atmosphere
Level is 104Pa) the stoichiometric proportion rutile TiO that Crystallizing treatment obtains2Film, non-stoichiometric rutile
TiO2Film has higher optical electro-chemistry decomposition water activity.
As shown in figure 5, being analyzed by XPS element depth distributions, what is be thermally treated resulting under air counts for chemistry
Amount is than golden red potato TiO2Film, O//Ti atomic ratios connect in thin-film body is bordering on 2；And it is heat-treated under anaerobism atmosphere
Obtain for non-stoichiometric rutile TiO2Film.O//Ti atomic ratios in film body phase are less than 2.
As shown in fig. 6, in the dark state, non-stoichiometric rutile TiO2Film (a) and stoichiometric proportion
Rutile TiO2The anhydrous decomposition current-responsive of film (b)；Under light illumination, with stoichiometric proportion rutile TiO2
Film (c) is compared, non-stoichiometric rutile TiO2Film (d) shows more excellent optical electro-chemistry water
Decomposability.
Embodiment result shows that the present invention (is closed by the oxygen partial pressure during regulating and controlling crystallization and thermal treatment in metal
Gold) in situ on matrix obtain specific morphology and the method for component adjustable metal sull, metal oxide
The pattern and composition of film are two important parameters of photochemistry moisture electrolytic cell light electrode material, are directly affected
The final transformation efficiency of photoelectrochemical cell.
Claims (7)
- A kind of 1. preparation method of pattern and the controllable metal-oxide film of composition, it is characterised in that：First, Using sheet metal or alloy sheet as matrix, generated using chemical attack oxidation in sheet metal or alloy substrates surface in situ Amorphous metal oxide；Then, the amorphous metal oxide film of acquisition is carried out to crystalline substance under different oxygen partial pressures Change heat treatment, pattern and the controllable metal-oxide film of composition are obtained by regulating and controlling heat treatment temperature and time.
- 2. according to the preparation method of the controllable metal-oxide film of the pattern described in claim 1 and composition, its It is characterised by：Described metal substrate is Fe, Ta, Ti, W, Zn, Cu or Co, described alloy substrates For Ti/Al, Cu/Zn, Ti/Fe, Ti/W or Ti/Ta alloy.
- 3. according to the preparation method of the controllable metal-oxide film of the pattern described in claim 1 and composition, its It is characterised by：Described chemical attack is oxidized to various metal erosion oxidizing process, using chemical solution burn into Atmospheric corrosion or electrochemical oxidation corrosion.
- 4. according to the preparation method of the controllable metal-oxide film of the pattern described in claim 1 and composition, its It is characterised by：Described crystallization and thermal treatment temperature is 300~1000 DEG C, and programming rate is 0.1~10 DEG C/min, Crystallization time is 0.5~48 hour.
- 5. according to the preparation method of the controllable metal-oxide film of the pattern described in claim 4 and composition, its It is characterised by：Preferably, described crystallization and thermal treatment temperature be 500~800 DEG C, programming rate be 1~5 DEG C/ Minute, crystallization time is 1~24 hour.
- 6. according to the preparation method of the controllable metal-oxide film of the pattern described in claim 1 and composition, its It is characterised by：Described Crystallizing treatment oxygen partial pressure is 0~105Pa。
- 7. according to the preparation method of the controllable metal-oxide film of the pattern described in claim 6 and composition, its It is characterised by：Preferably, described Crystallizing treatment oxygen partial pressure is 0~1000Pa.
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| CN108754403A (en) * | 2018-06-01 | 2018-11-06 | 天津大学 | Method for preparing Zr-Al-O ternary amorphous oxide layer |
| CN110158020A (en) * | 2019-04-09 | 2019-08-23 | 山东大学 | A kind of method of ultrasonic wave added induction heating preparation nanostructure oxidation film |
| CN111204799A (en) * | 2018-11-22 | 2020-05-29 | 中国科学院金属研究所 | Preparation method of double-sided metal oxide or nitride hollow shell structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108754403A (en) * | 2018-06-01 | 2018-11-06 | 天津大学 | Method for preparing Zr-Al-O ternary amorphous oxide layer |
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| CN111204799A (en) * | 2018-11-22 | 2020-05-29 | 中国科学院金属研究所 | Preparation method of double-sided metal oxide or nitride hollow shell structure |
| CN111204799B (en) * | 2018-11-22 | 2021-11-05 | 中国科学院金属研究所 | Preparation method of double-sided metal oxide or nitride hollow shell structure |
| CN110158020A (en) * | 2019-04-09 | 2019-08-23 | 山东大学 | A kind of method of ultrasonic wave added induction heating preparation nanostructure oxidation film |
| CN110158020B (en) * | 2019-04-09 | 2020-04-21 | 山东大学 | Method for preparing nano-structure oxide film by ultrasonic-assisted induction heating |
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