CN104878426B - A kind of electrodeposition process original position prepares (Ga1‑xZnx)(N1‑xOx) soft-light anode method - Google Patents
A kind of electrodeposition process original position prepares (Ga1‑xZnx)(N1‑xOx) soft-light anode method Download PDFInfo
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Abstract
(Ga is prepared the present invention relates to a kind of electrodeposition process original position1‑ xZnx)(N1‑xOx) soft-light anode method, including：Zn (OH) is prepared on flexible metal basement2、Ga(OH)3Composite bed, obtains zinc gallium mixed hydroxides electrode, and then nitrogen treatment, obtains final product.(Ga prepared by the present invention1‑xZnx)(N1‑xOx) electrode is flexible, easy to install with dismounting, its microscopic appearance is the multilevel hierarchy for being conducive to light-receiving, and crystallite dimension is less than 20nm, and under visible light illumination with high photocurrent response, and Photoelectrochemical stabilization is good.
Description
Technical field
The invention belongs to the preparation field of soft-light anode, more particularly to a kind of electrodeposition process original position prepares (Ga1-xZnx)
(N1-xOx) soft-light anode method.
Background technology
Light-catalyzed reaction is the chemical reaction that material is carried out under light and photochemical catalyst collective effect.Due to its room temperature depth
React and can directly utilize the characteristics such as solar energy, in air and water pollution control, photocatalytic hydrogen production by water decomposition, photocatalysis also
Former CO2Etc. aspect have been a great concern.
(Ga1-xZnx)(N1-xOx) it is the stable solid solution being made up of ZnO and GaN, energy gap is about 2.4~2.8eV, tool
There is visible absorption activity, capable regulation and control can be transferred in its performance (such as absorption spectrum ranges) by adjusting Zn, Ga component ratio, and
And its stable chemical performance, there is significant visible light catalytic hydrogen production by water decomposition activity after load cocatalyst, it is in recent years emerging
A kind of visible light catalytic semi-conducting material.(Ga at present1-xZnx)(N1-xOx) it is usually the submicron order of high temperature solid-state method preparation
Powder body material.For example, Domen of Tokyo University etc. is in Nature, reported on 2006,440,295 with ZnO and Ga2O3Powder is
Raw material, through (Ga prepared by high temperature solid state reaction1-xZnx)(N1-xOx) particle.The method reaction temperature is high, the time is long, resulting
(Ga1-xZnx)(N1-xOx) particle is big, Size Distribution is wide, crystallite dimension is big, specific surface area is very low, light in reacting visible light catalytic
The separation of raw carrier, migration are combined no gain effect with suppression.Meanwhile, photocatalyst surface electron-hole pair it is quick
The compound application for also constraining photocatalysis technology.How the recombination rate of photo-generated carrier is effectively suppressed, so as to improve photocatalysis
Activity, the focus as research.
Photoelectrocatalysis is to suppress the compound effective technology means of photo-generated carrier by external biasing field.Domen etc.
With high temperature vapour deposition process prepare ZnO nanowire array as template, the Ga of high temperature vapour deposition thereon, finally nitrogenize be obtained with
ZnO is core, the conductive ZnO-ZnGaON nano-wire arrays with ZnGaON as shell.As applying 0.8VRHEDuring bias, its photoelectric current
Density is about 1.5mAcm-2, solar energy conversion efficiency be 0.75%, and photochemical stability preferably (M.Zhong,
Y.H.Ma,P.Oleynikov,K.Domen and J.-J.Delaunay,Energy Environ.Sci.,2014,7,1693-
1699).But the equipment of the method is complicated, and reaction temperature is high, and needs to carry out under vacuum.The radio frequency magnetron such as Shet splashes
Penetrate method one-step synthesis ZnO-GaN films (S.Shet, Y.F.Yan, J.Turner and M.Al-Jassim, J.Power
Sources, 2013,232,74-78), but the density of photocurrent of its product is smaller, only microampere order.The preparation process is equally needed
To be carried out in vacuum condition, equipment is complicated, and needs specific target.
Electrochemical deposition is under electric field action, loop to be constituted by negative electrode and anode in certain electrolyte solution, is led to
Oxidization-reduction reacts, and makes ion deposition in solution that the process of required coating is obtained to negative electrode or anode surface.It
Can in various baroque substrates uniform deposition, by control process conditions (such as solution composition, concentration, pH value, temperature,
Electric current, sedimentation time etc.), chemical composition, structure, thickness and deposition velocity of sedimentary etc. are accurately controlled, and be usually normal
Temperature or slightly above room temperature, the liquid phase reactor of normal pressure, process equipment is simple, operation is easy, Environmental security, mode are flexible, is suitable to work
Industryization is mass produced.But so far, prepare (Ga on electrodeposition process original position1-xZnx)(N1-xOx) soft-light anode document
There is not been reported with patent.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of electrodeposition process original position and prepare (Ga1-xZnx)(N1-xOx) flexible
The method of light anode, the method synthesize a series of morphology controllables, Different Zinc gallium than (Ga1-xZnx)(N1-xOx) light anode, this hair
Bright cost of material is low, be easy to get, and process equipment is simple, and operation is easy, Environmental security, and mode flexibly, is adapted to industrialization extensive raw
Produce.
A kind of electrodeposition process original position of the invention prepares (Ga1-xZnx)(N1-xOx) soft-light anode method, including：
(1) Zn (OH) is prepared2Layer：Flexible metal basement is placed in containing in zinc salt, the aqueous solution of pattern controlling agent, Ran Houjin
Row electro-deposition, obtains that surface is long Zn (OH)2Flexible metal basement；Wherein zinc salt, the mol ratio of pattern controlling agent are 1:5~
5:1；
(2) Zn (OH) is prepared2、Ga(OH)3Composite bed：There is Zn (OH) by above-mentioned surface is long2Flexible metal basement be placed in and contain
In zinc salt, gallium salt, the aqueous solution of pattern controlling agent, electro-deposition is then carried out, obtain zinc gallium mixed hydroxides electrode；Wherein zinc
Salt is 1 with the mol ratio of gallium salt:5~5:1, zinc salt is 1 with the mol ratio of pattern controlling agent:5~5:1；
(3) nitridation prepares (Ga1-xZnx)(N1-xOx)：Above-mentioned zinc gallium mixed hydroxides electrode is placed in tube-type atmosphere furnace
In, nitrogenized in ammonia, in nitridation process, hydroxide is decomposed into oxide at a lower temperature, and then oxide exists
Role transformation at of a relatively high temperature through ammonia is oxynitride, through natural cooling, obtains final product (Ga1-xZnx)(N1-xOx) flexible
Light anode, wherein x are that scope is 0.05~0.90.
Flexible metal basement is titanium silk, titanium net or titanium foil in the step (1).
Pattern controlling agent is NaCl, KCl, NaF or KF in the step (1), (2).
The concentration of zinc salt is 0.02~2mol/L in the aqueous solution in the step (1).
Electro-deposition is carried out by three-electrode system in the step (1), (2), and three-electrode system is biased (negative
Pressure) it is -0.7~-1.4V；Electrodeposition time is 60~1800s.
Aqueous temperature is 45~75 DEG C in the step (1), (2).
Zinc salt concentration in aqueous is 0.02~2mol/L in the step (2).
Ammonia flow is 100~400mL/min in the step (3).
Nitridation conditions are that heating rate is 2~8 DEG C/min in the step (3), and nitriding temperature is 400~900 DEG C, insulation
Time is 3~8h.
Beneficial effect
(1) the inventive method synthesize a series of morphology controllables, Different Zinc gallium than (Ga1-xZnx)(N1-xOx) light anode；
(2) (Ga prepared by the present invention1-xZnx)(N1-xOx) electrode be flexible, it is easy to install with dismounting, its microcosmic shape
Looks are the multilevel hierarchy for being conducive to light-receiving, and crystallite dimension is less than 20nm, is rung with high photoelectric current under visible light illumination
Should, and Photoelectrochemical stabilization is good；
(3) present invention can substantially reduce synthesis (Ga1-xZnx)(N1-xOx) needed for nitridation reaction temperature, significantly shorten reaction
Time, reducing energy consumption；
(4) the inventive method cost of material is relatively low, be easy to get, process equipment is simple, operation easily, the spirit of Environmental security, mode
It is living, it is suitable to industrialization large-scale production.
Brief description of the drawings
Fig. 1 is that embodiment 1 prepares (Ga1-xZnx)(N1-xOx) electrode electromicroscopic photograph；Wherein a is (Ga1-xZnx)(N1- xOx) electrode surface stereoscan photograph；Illustration is the (Ga of low power in a1-xZnx)(N1-xOx) electrode surface stereoscan photograph；b
It is (Ga1-xZnx)(N1-xOx) electrode surface (Ga1-xZnx)(N1-xOx) transmission electron microscope photo after ultrasonic disperse；
(a) is that embodiment 1 prepares (Ga in Fig. 21-xZnx)(N1-xOx) electrode top layer (Ga1-xZnx)(N1-xOx) X penetrate
Ray diffraction diagram；B () is (Ga prepared by embodiment 11-xZnx)(N1-xOx) electrode UV-Vis DRS absorption spectrum；
(a) is that embodiment 1 prepares (Ga in Fig. 31-xZnx)(N1-xOx) current-voltage of the electrode under the conditions of continuous illumination
Curve；Fig. 3 (b) is that embodiment 1 prepares (Ga1-xZnx)(N1-xOx) current -voltage curve of the electrode under the conditions of intermittent illumination；
Fig. 4 is that embodiment 3 prepares (Ga1-xZnx)(N1-xOx) current -voltage curve of the electrode under the conditions of intermittent illumination.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) by line footpath be 150 μm, mesh number be 15 mesh, size for 2 × 3cm titanium net as working electrode, platinum plate electrode is
To electrode, Ag/AgCl electrodes are immersed in the (NO of Zn containing 0.05mol/L for reference electrode3)2·6H2O and 0.1mol/L NaCl's
In the aqueous solution.It is 55 DEG C to keep solution temperature, applies the bias 20min of -1.1V to titanium net by electrochemical workstation, in its table
One layer of Zn (OH) of face growth in situ2.(2) there is Zn (OH) by surface is long2Titanium net as working electrode, platinum plate electrode be to electrode,
Ag/AgCl electrodes are reference electrode, are immersed in (the NO of Zn containing 0.05mol/L3)2·6H2O、0.025mol/L Ga(NO3)3·
xH2In the aqueous solution of O and 0.1mol/L NaCl.Keep solution temperature be 55 DEG C, by electrochemical workstation to titanium net apply-
The bias 20min of 1.1V, in one layer of zinc gallium mixed hydroxides of its surface in situ electro-deposition.(3) by obtained zinc gallium mixing hydrogen
Oxide electrode is put into tube-type atmosphere furnace, is passed through the ammonia of flowing, and ammonia flow is maintained at 200mL/min, is raised to from room temperature
700 DEG C, heating rate is 3 DEG C/min, is incubated 5h, then naturally cools to room temperature, obtains (Ga1-xZnx)(N1-xOx) electrode (its
Middle x=0.76).Fig. 1 (a) is (Ga manufactured in the present embodiment1-xZnx)(N1-xOx) electrode stereoscan photograph, show prepare
Electrode top layer is by hexagonal plate (Ga1-xZnx)(N1-xOx) cross layered formation tree constitute, the tree perpendicular to
Electrode surface and it is uniformly distributed in electrode surface.Fig. 1 (b) is (Ga manufactured in the present embodiment1-xZnx)(N1-xOx) electrode top layer
(Ga1-xZnx)(N1-xOx) transmission electron microscope photo in ethanol after ultrasonic disperse, it can be seen that (Ga manufactured in the present embodiment1- xZnx)(N1-xOx) crystallite dimension it is more uniform, average diameter is about 20nm.Fig. 2 (a) is (Ga manufactured in the present embodiment1- xZnx)(N1-xOx) electrode top layer (Ga1-xZnx)(N1-xOx) X-ray diffractogram, due to crystal along (002) high preferred orientation give birth to
Long, the diffraction maximum of (002) crystal face is extremely strong so that other diffraction maximums are not obvious, and the present embodiment is can be seen that from the position of diffraction maximum
(the Ga for preparing1-xZnx)(N1-xOx) it is hexagonal wurtzite structure, mutually exist without other impurities, and high preferred orientation is mainly (002)
Crystal face.Fig. 2 (b) is (Ga manufactured in the present embodiment1-xZnx)(N1-xOx) electrode UV-Vis DRS absorption spectrum, absorb
Side position is about 580nm, illustrates (Ga manufactured in the present embodiment1-xZnx)(N1-xOx) electrode pair visible ray has absorption.
Embodiment 2
(the Ga that will be prepared in embodiment 11-xZnx)(N1-xOx) electrode (wherein x=0.76) is used as working electrode, platinized platinum is electric
Extremely to electrode, Ag/AgCl electrodes are reference electrode, are immersed in the Na of 0.5mol/L2SO4In solution.It is a standard with light intensity
Lamp source irradiation (the Ga of sunshine1-xZnx)(N1-xOx) electrode surface, with electrochemical workstation to (Ga1-xZnx)(N1-xOx) electrode
Apply the bias of -0.4~1.0V, the current -voltage curve tested under the conditions of its continuous illumination and intermittent illumination.Fig. 3 (a) is this
(the Ga of embodiment test1-xZnx)(N1-xOx) current -voltage curve of the electrode under the conditions of continuous illumination, when voltage is 1V,
Its current density is about 1.05mA/cm-2.Fig. 3 (b) is (Ga of the present embodiment test1-xZnx)(N1-xOx) electrode is in intermittent illumination
Under the conditions of current -voltage curve, it can be seen that (the Ga when not having illumination1-xZnx)(N1-xOx) current density in electrode is basic
It is zero, (the Ga in illumination1-xZnx)(N1-xOx) current density in electrode substantially increases, and illustrates (the Ga in the present embodiment1- xZnx)(N1-xOx) electrode pair illumination response is substantially.
Embodiment 3
(1) by line footpath be 150 μm, mesh number be 15 mesh, size for 2 × 3cm titanium net as working electrode, platinum plate electrode is
To electrode, Ag/AgCl electrodes are immersed in the (NO of Zn containing 0.05mol/L for reference electrode3)2·6H2O and 0.1mol/L NaCl's
In the aqueous solution.It is 60 DEG C to keep solution temperature, applies the bias 30min of -1.1V to titanium net by electrochemical workstation, in its table
One layer of Zn (OH) of face growth in situ2.(2) there is Zn (OH) by surface is long2Titanium net as working electrode, platinum plate electrode be to electrode,
Ag/AgCl electrodes are reference electrode, are immersed in (the NO of Zn containing 0.05mol/L3)2·6H2O、0.025mol/L Ga(NO3)3·
xH2In the aqueous solution of O and 0.1mol/L NaCl.Keep solution temperature be 60 DEG C, by electrochemical workstation to titanium net apply-
The bias 5min of 1.2V, in one layer of zinc gallium mixed hydroxides of its surface in situ electro-deposition.(3) by obtained zinc gallium mixing hydrogen-oxygen
Compound electrode is put into tube-type atmosphere furnace, is passed through the ammonia of flowing, and ammonia flow is maintained at 200mL/min, and 700 are raised to from room temperature
DEG C, heating rate is 3 DEG C/min, is incubated 5h, then naturally cools to room temperature, obtains (Ga1-xZnx)(N1-xOx) electrode (wherein x
=0.86).(the Ga that will be prepared1-xZnx)(N1-xOx) used as working electrode, platinum plate electrode is to electrode, Ag/AgCl electrodes to electrode
For reference electrode is immersed in the 0.5mol/L Na adjusted with NaOH to pH=132SO4In solution.It is a standard sun with light intensity
Lamp source irradiation (the Ga of light1-xZnx)(N1-xOx) electrode surface, with electrochemical workstation to (Ga1-xZnx)(N1-xOx) electrode applying-
The bias of 0.4~1.0V, the current -voltage curve tested under the conditions of its intermittent illumination.Fig. 4 is (Ga manufactured in the present embodiment1- xZnx)(N1-xOx) current -voltage curve of the electrode under the conditions of intermittent illumination, it can be seen that (the Ga when not having illumination1-xZnx)
(N1-xOx) current density in electrode is substantially zeroed, (the Ga in illumination1-xZnx)(N1-xOx) current density in electrode substantially increases
Plus, when voltage is 1V, its current density is about 4.3mA/cm-2, illustrate (the Ga in the present embodiment1-xZnx)(N1-xOx) electrode
It is obvious to illumination response.
Embodiment 4
(1) it is the titanium foil of 2 × 3cm using size as working electrode, platinum plate electrode is that to electrode, Ag/AgCl electrodes are ginseng
(the NO of Zn containing 0.05mol/L are immersed in than electrode3)2·6H2In the aqueous solution of O and 0.1mol/L NaCl.Keep solution temperature be
60 DEG C, apply the bias 30min of -1.1V to titanium foil by electrochemical workstation, one layer of Zn (OH) is grown in its surface in situ2。
(2) there is Zn (OH) by surface is long2Titanium foil as working electrode, platinum plate electrode is that to electrode, Ag/AgCl electrodes are reference electrode
It is immersed in (the NO of Zn containing 0.05mol/L3)2·6H2O、0.025mol/L Ga(NO3)3·xH2O and 0.1mol/L NaCl's is water-soluble
In liquid.It is 55 DEG C to keep solution temperature, applies the bias 30min of -1.1V to titanium foil by electrochemical workstation, former on its surface
Position one layer of zinc gallium mixed hydroxides of electro-deposition.(3) obtained zinc gallium mixed hydroxides electrode is put into tube-type atmosphere furnace,
The ammonia of flowing is passed through, ammonia flow is maintained at 200mL/min, 700 DEG C are raised to from room temperature, heating rate is 3 DEG C/min, insulation
5h, then naturally cools to room temperature, obtains (Ga1-xZnx)(N1-xOx) electrode (wherein x=0.59).(the Ga that will be prepared1-xZnx)
(N1-xOx) used as working electrode, platinum plate electrode is that, to electrode, Ag/AgCl electrodes are immersed in 0.1mol/L for reference electrode to electrode
Na2SO4In solution.It is that a lamp source for standard sunshine irradiates (Ga with light intensity1-xZnx)(N1-xOx) electrode surface, use electrochemistry
Work station is to (Ga1-xZnx)(N1-xOx) electrode applies the bias of -0.4~1.0V, the current-voltage tested under its illumination condition is bent
Line.(the Ga in no light1-xZnx)(N1-xOx) current density in electrode is substantially zeroed, (the Ga in illumination1-xZnx)(N1-xOx)
Current density in electrode increases with voltage and substantially increases, and when voltage is 1V, its current density is about 0.6mA/cm-2。
Claims (7)
1. a kind of electrodeposition process original position prepares (Ga1-xZnx)(N1-xOx) soft-light anode method, including：
(1) during flexible metal basement is placed in containing zinc salt, the aqueous solution of pattern controlling agent, electro-deposition is then carried out, obtains surface
Length has Zn (OH)2Flexible metal basement；Wherein zinc salt, the mol ratio of pattern controlling agent are 1:5~5:1；Wherein flexible metal
Substrate is titanium silk, titanium net or titanium foil；
(2) there is Zn (OH) by above-mentioned surface is long2Flexible metal basement be placed in containing zinc salt, gallium salt, pattern controlling agent the aqueous solution
In, electro-deposition is then carried out, obtain zinc gallium mixed hydroxides electrode；Wherein zinc salt and the mol ratio of gallium salt is 1:5~5:1,
Zinc salt is 1 with the mol ratio of pattern controlling agent:5~5:1；
(3) above-mentioned zinc gallium mixed hydroxides electrode is placed in tube-type atmosphere furnace, is nitrogenized in ammonia, natural cooling is obtained final product
(Ga1-xZnx)(N1-xOx) soft-light anode；Wherein x scopes are 0.05~0.90；Wherein nitridation conditions are that heating rate is 2~8
DEG C/min, nitriding temperature is 400~900 DEG C, and soaking time is 3~8h.
2. a kind of electrodeposition process original position according to claim 1 prepares (Ga1-xZnx)(N1-xOx) soft-light anode method,
It is characterized in that：Pattern controlling agent is NaCl, KCl, NaF or KF in the step (1), (2).
3. a kind of electrodeposition process original position according to claim 1 prepares (Ga1-xZnx)(N1-xOx) soft-light anode method,
It is characterized in that：The concentration of zinc salt is 0.02~2mol/L in the aqueous solution in the step (1).
4. a kind of electrodeposition process original position according to claim 1 prepares (Ga1-xZnx)(N1-xOx) soft-light anode method,
It is characterized in that：Electro-deposition is carried out by three-electrode system in the step (1), (2), and three-electrode system is biased
It is -0.7~-1.4V；Electrodeposition time is 60~1800s.
5. a kind of electrodeposition process original position according to claim 1 prepares (Ga1-xZnx)(N1-xOx) soft-light anode method,
It is characterized in that：Aqueous temperature is 45~75 DEG C in the step (1), (2).
6. a kind of electrodeposition process original position according to claim 1 prepares (Ga1-xZnx)(N1-xOx) soft-light anode method,
It is characterized in that：Zinc salt concentration in aqueous is 0.02~2mol/L in the step (2).
7. a kind of electrodeposition process original position according to claim 1 prepares (Ga1-xZnx)(N1-xOx) soft-light anode method,
It is characterized in that：Ammonia flow is 100~400mL/min in the step (3).
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| CN1461791A (en) * | 2002-04-09 | 2003-12-17 | 日亚化学工业株式会社 | Phosphorus gallium fluorophor, its making method and display device using the fluorophor |
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|---|---|---|---|---|
| JPH09208396A (en) * | 1996-02-05 | 1997-08-12 | Furukawa Electric Co Ltd:The | Production of gallium nitride substrate |
| JP3595829B2 (en) * | 2003-03-19 | 2004-12-02 | 株式会社東北テクノアーチ | GaN substrate manufacturing method |
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|---|---|---|---|---|
| CN1461791A (en) * | 2002-04-09 | 2003-12-17 | 日亚化学工业株式会社 | Phosphorus gallium fluorophor, its making method and display device using the fluorophor |
| CN101113533A (en) * | 2007-08-17 | 2008-01-30 | 中国科学院上海硅酸盐研究所 | Modified method for preparing single c-axle oriented zinc oxide film by electrochemical deposition process |
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