CN106115771A - A kind of In2o3the preparation method that polyhedron micron is brilliant - Google Patents
A kind of In2o3the preparation method that polyhedron micron is brilliant Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 6
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012159 carrier gas Substances 0.000 claims abstract description 5
- 239000007792 gaseous phase Substances 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 239000000428 dust Substances 0.000 claims abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 27
- 230000012010 growth Effects 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000005518 electrochemistry Effects 0.000 claims description 8
- 230000003287 optical effect Effects 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 239000003708 ampul Substances 0.000 claims description 3
- 230000007480 spreading Effects 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 description 33
- 239000013081 microcrystal Substances 0.000 description 8
- 229910021607 Silver chloride Inorganic materials 0.000 description 6
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 6
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 5
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 208000036626 Mental retardation Diseases 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000009647 facial growth Effects 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses In2O3The preparation method that polyhedron micron is brilliant, prepares In with chemical vapour deposition technique2O3The method of polyhedron micron particle, first by high-purity for 300mg In2O3Powder and 150mg carbon dust are milled 10 ± 5min in mortar, make the two be sufficiently mixed；Then being put into by mixture in chemical gaseous phase deposited tube, after mixture, at 1.5cm, placement surface has the Si sheet of thick 10 50nm Au films, as the substrate collecting sample；Last deposited tube is passed through Ar gas and the O of 2% of 98%2Gas, as carrier gas, according to temperature (the 920 1000 DEG C) reaction 3 ± 1h set, is cooled to room temperature, takes out Si substrate, obtain In in its surface2O3Polyhedron micron particle.
Description
Technical field
The invention belongs to chemical gaseous phase deposition and prepare law areas, relate to a kind of accuracy controlling In2O3Micron crystal form looks method with
Application.
Background technology
The particular crystal plane that inorganic functional semi-conducting material is exposed because of show peculiar physics, chemical property and enjoy pass
Note, and in fields such as photocatalysis, dye-sensitized cell, detection of gas and lithium ion batteries, there is huge potential using value.
Synthesis has and exposes the micro-nano functional material of particular crystal plane at high proportion and be increasingly becoming the research of micro Nano material technology of preparing
One of focus.
In photoelectrocatalysis field, the crystal face with different surfaces Atomic Arrangement not only has different active sites,
And the barrier height of quasiconductor/electrolyte interface knot can be changed, thus cause different photoelectrochemical catalysis activity.In the recent period, greatly
Fluidization physics Institute Li Can et al. is with BiVO4Model catalyst, confirms to there is light between different crystal face from experiment aspect
Raw electron-hole pair be spatially separating effect, exposed the BiVO of different crystal faces by preparation system4Nanoparticle catalyst, significantly
Improve its photoelectric catalytically active, and using value (R.G.Li, et significant in photoelectrocatalysis field
al.Nat.Commun.2013,4,1432)。
Indium sesquioxide. (the In of cubic structure2O3) it is a kind of important n-type semiconductor, indirect band gap (2.8eV), chemistry
Stability is high, and suitable conduction band and valence band location are widely used in photoelectrocatalysis field.The most peculiar is In2O3{ 001}
Polarity crystal face can make hydrone (H2O) it is dissociated into H-And OH+.Document shows that the Dissociative of hydrone can be effectively improved photoelectricity
The efficiency that chemical water is decomposed.Additionally, recent result of calculation shows In2O3{ 001} and { 111} crystal face is respectively provided with converged light
Raw electronics and hole ability.Therefore, by regulation and control In2O3Pattern to improve its performance be the most all In2O3Nano material
The focus of research, and existing a large amount of report.Up to now, cube, truncation cube, cuboctahedron, truncated octahedron, eight
Difformities In such as face body2O3Micro-nano granules be the most designed to be synthesized.But these polyhedrons simultaneously appear in a lining
Bottom surface, and productivity is relatively low, it is impossible to it is carried out PhotoelectrocatalytiPerformance Performance test.This is due to relative to mental retardation crystal face, high energy
The surface of crystal face can be higher, and in crystal growing process, the growth rate along high miller index surface direction is brilliant far faster than mental retardation number
Face, causes high energy crystal face to tend to disappearing, finally can only obtain the crystal that mental retardation crystal face surrounds.One provided by the present invention prepares shape
Looks are single, size uniform and expose the In of different crystal face2O3The method that polyhedron micron is brilliant, has deepened cubic system growth machine
The understanding of system, the pattern for accuracy controlling cubic system provides new way.
Summary of the invention
It is an object of the present invention to provide a kind of In2O3The preparation method and applications that polyhedron micron is brilliant.
Technical scheme: In2O3The preparation method that polyhedron micron is brilliant, prepares with chemical vapour deposition technique
In2O3The method of polyhedron micron particle, first by high-purity for 300mg In2O3Powder and 150mg carbon dust mill 10 in mortar ±
5min, makes the two be sufficiently mixed；Then mixture is put in chemical gaseous phase deposited tube, after mixture, at 1.5cm, place table
There is the Si sheet of thick 10-50nm Au film in face, as the substrate collecting sample；Finally, deposited tube is passed through high-purity argon (98%)
With oxygen (2%), reaction temperature is respectively set as 920-1000 DEG C, and the response time is 3 ± 1h, is cooled to room temperature, takes out Si
Substrate, obtains In in its surface2O3Polyhedron micron particle.
In is prepared with chemical vapour deposition technique2O3The method of polyhedron micron particle, by high-purity In2O3Powder and carbon
Powder is sufficiently mixed, and grinds 10min so that it is diameter is about 10 μm, and then uniform spreading is in aluminium oxide boat in agate mortar；By this
Aluminium oxide boat is put in horizontal CVD boiler tube；In course of reaction, carrier gas is high-purity argon (98%) and the gaseous mixture of oxygen 2%
Body, flow is 150sccm (standard-state cubic centimeter per minute)；The Si being coated with Au film is served as a contrast
The end, is placed at distance aluminium oxide boat 1.5cm, and puts in the little quartz ampoule that internal diameter is 1.6cm simultaneously, then puts into CVD boiler tube together
In；At polyhedral In2O3Micron particle growth course, furnace temperature is heated to 920 with the programming rate of 50 DEG C/min respectively, 940,
960,980 and 1000 DEG C and keep 3h, air pressure remains at a normal atmosphere (atm).In above-mentioned corresponding growth temperature
Under the conditions of degree, In2O3The pattern of micron particle is octahedron, truncated octahedron, cuboctahedron, truncation cube respectively and stands
Cube.
It addition, the above-mentioned In that the present invention provides2O3Polyhedron micron crystalline substance is preparing efficient stable Optical Electro-Chemistry water decomposition electrode
In application, also belong to protection scope of the present invention.
The present invention is in chemical vapor deposition processes, by regulating and controlling the degree of supersaturation (temperature) of reactant, according to energy
Conservation principle carrys out accuracy controlling In2O3The crystal face (pattern) exposed that micron is brilliant, final acquisition exposes different { 111}/{ 001}
The In of area ratio2O3Polyhedron micron is brilliant.
Beneficial effect: the inventive method utilizes chemical vapour deposition technique, with high-purity In2O3Powder and toner mixture are
Source, when growth temperature is 920-1000 DEG C, obtains a series of pattern by carbothermic reduction reaction single, size uniform and sudden and violent
The In of the different crystal face of dew2O3Polyhedron micron is brilliant.In prepared by the present invention2O3Polyhedron micron is brilliant, by { 111} and { 001} crystal face
Encirclement forms, and the micron crystalline substance of different patterns has different { 001}/{ 111} surface areas ratios.The preparation method letter of the present invention
The features such as sample crystallinity single, easy to operate, with low cost and preparation is high and surface is clean.In in the present invention2O3Multiaspect
The crystal face that body micron particle is exposed affects its PhotoelectrocatalytiPerformance Performance, and cubic micron particle has efficient, stable photoelectrochemical
Learn catalytic performance, at other, there is the dependent application of crystal face--such as gas sensor, solaode and lithium-ion electric
The aspects such as pond have broad application prospects.The inventive method breaches existing In2O3Polyhedron micron crystalline substance is difficult to a large amount of accurately tune
The technical limitations of control, has the advantage that
1. need not additionally add surface agent to control In2O3Pattern, sample surfaces is clean, and subsequent treatment is simple and knot
Crystalline substance degree is high.
2. the In prepared by the method2O3The average-size of polyhedron micron crystalline substance is 1 μm, and corner angle are bright and sharp, pattern rule,
Size uniformity；In2O3Polyhedron micron is brilliant by { 111} is with { 001} crystal face surrounds and forms, and the ratio of two surface areas is with pattern not
Different together.
3.In2O3Polyhedron micron crystalline substance exposed 001} crystal face not only have converge photohole ability, Er Qieke
So that hydrone (H2O) it is dissociated into H-And OH+, the efficiency of its Optical Electro-Chemistry decomposition water can be improved greatly.
4. the In prepared by the present invention2O3Polyhedron micron crystalline substance may be used for Optical Electro-Chemistry water decomposition, and function admirable, as
Shown in accompanying drawing 6.
Accompanying drawing explanation
Fig. 1 is the In prepared by the present invention2O3The FE-SEM image that polyhedron micron is brilliant, figure is the most successively
In2O3Cube (f), truncation cube (g), cuboctahedron (h), truncated octahedron (i) and octahedra (j) (in figure outer ring with
Inner ring is the regular shape graph that photo and the simulation of brilliant material draws respectively)；(figure a-e is also In2O3Micron brilliant with temperature and
Time-varying process).Can be seen that this In2O3Polyhedron micron crystalline substance exposed { 001}/{ 111} crystal face growth rate ratio is i.e.
R value=γ(001)/γ(111)With growth temperature increase and increase (in figure inner ring give this ratio increase process, outmost turns is P
=S(001)/(S(001)+S(111)) value increase), this is owing to growth temperature is the highest, and the degree of supersaturation of reactant is the highest, ties accordingly
Brilliant driving force is the biggest.In order to meet preservation of energy, growth temperature is the highest, and { probability of 001} crystal face is the biggest in exposure.
In obtained by Fig. 2 present invention2O3The pattern different with growth temperature (evolution mechanism) figure of micro-crystal, 920 DEG C
(figure i, j corresponding 5 μm of difference and 2 μm scales), 940 DEG C (figure g, h corresponding 5 μm respectively and 2 μm scales), 960 DEG C of (figure e, f difference
Corresponding 5 μm and 2 μm scales), 980 DEG C (figure c, d corresponding 5 μm respectively and 2 μm scales) and 1000 DEG C (scheme a, b corresponding 5 μm of difference and
2 μm scales).
Fig. 3 is In prepared by gained of the present invention2O3The XRD figure that polyhedron micron is brilliant, figure is followed successively by cube from top to bottom
The XRD figure spectrum of (a), truncation cube (b), cuboctahedron (c), truncated octahedron (d) and octahedral (e).In crystal growth mistake
Cheng Zhong, the probability that the relative growth rate of crystal face is exposed to plane of crystal the most slowly is the biggest, and then has relatively in XRD figure is composed
Stronger diffracted intensity.When pattern is developed into vertical octahedral cube by cube, { 001} and the { intensity of 111} crystallographic plane diffraction peak
It is reduced to 0.3 by 6.5, illustrates that { 001} surface areas is gradually reduced and { 111} surface areas gradually increases.
Fig. 4 is that the FE-TEM of the exposed crystal face of the cube prepared by the present invention analyzes, and (a is b) cubical respectively
FE-SEM image (scale: 500nm) and analog image are along cubical [001] direction.C () cubical low power FE-TEM is schemed
As [001] direction, edge (scale: 500nm).D () SAED style is along [001] direction.(e) HR-TEM image (scale: 5nm).
F () atomic structure projection, along [001] direction, illustrates that cube is by { 001} crystal face surrounds and forms.
Fig. 5 is the In prepared by the present invention2O3Truncation cube, cuboctahedron, truncated octahedron and octahedral FE-
FEM analyzes, and (figure a, b, c) be the cubical analog image of truncation respectively, low power FE-SEM image, and low power FE-TEM is with corresponding
SAED style is along [001] directional diagram；(figure d, e, f) be the analog image of cuboctahedron respectively, low power FE-SEM image, low power
FE-TEM and corresponding SAED style are along [111] directional diagram；(figure g, h, i) be the analog image of truncated octahedron, low power respectively
FE-SEM image, low power FE-TEM and corresponding SAED style are along [001] direction；(figure j, k, l) be octahedral simulation respectively
Image, low power FE-SEM image, low power FE-TEM and corresponding SAED style are along [111] directional diagram.
Fig. 6 is In2O3The J-V curve of polyhedral micro-crystal photo cathode (270mW/cm under illumination condition2) (figure
A) at 0.22VAg/AgClTime J-t curve and (figure b) oxygen evolution amount change over curve.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated.
Example: by high-purity for 350mg In2O3Powder is sufficiently mixed with the graphite powder of 150mg, grinds in agate mortar
10min, then uniform spreading is in aluminium oxide boat.This aluminium oxide boat is put into (internal diameter: 1.6cm, length in the quartz ampoule of pipe with small pipe diameter
Degree: 20cm), then puts into little quartz guard system entirety in horizontal CVD boiler tube.With the Si sheet of plated surface 10nm thickness Au film for receiving
The substrate of collection sample.In course of reaction, carrier gas is the mixed gas of high-purity argon and oxygen, and wherein argon volume ratio accounts for
98%, oxygen volume ratio accounts for 2%, and flow is 150sccm (standard-state cubic centimeter per
minute).The Si substrate being coated with Au film is placed on distance aluminium oxide boat 1.5cm, and puts into the little quartz that internal diameter is 1.6cm simultaneously
Guan Zhong, then put into together in boiler tube.At polyhedral In2O3Micron particle growth course, furnace is respectively with 50 DEG C/min's
Programming rate is heated to 920, and 920,940,960,980, and 1000 DEG C and keep 3h, air pressure remains at a standard atmosphere
Pressure (atm).After reaction terminates, wait temperature fall in reacting furnace.Continue logical Ar gas and close O2Gas makes sample in Ar atmosphere
It is down to room temperature.Finally close Ar gas, take out sample.At Si substrate surface lodgment In2O3Polyhedron micro-crystal.
In said method step, collect the acquisition methods of Si substrate of sample: by N-shaped Si sheet (<100>crystal orientation, thickness:
0.5mm, resistivity: 1-10 Ω cm) it is cut into 1 × 1cm2Square pieces, then according to following step is carried out.First will cutting
Good Si sheet is sequentially placed in acetone soln, dehydrated alcohol and deionized water sonic oscillation 20min respectively.Deionized water rinsing is done
After Jing, then silicon chip substrate is put into the SiO on 1wt% Fluohydric acid. (HF) removal surface2Layer.The most again use deionized water rinsing silicon
Sheet, dries stand-by under vacuum.Finally utilize the Au of vacuum coater Si substrate surface plating 10nm thickness after cleaning thin
Film, as the substrate collecting sample in deposition process.
Described In2O3Polyhedron micron crystalline substance has five kinds of patterns: cube, truncation cube, cuboctahedron, truncation eight
Face body and octahedron.The size uniform of sample, about 1 micron.Product morphology is as shown in Figure 2.
In of the present invention2O3Polyhedron micron crystalline substance can be used for Optical Electro-Chemistry water decomposition, and polyhedron micron particle is exposed
Crystal face affect its PhotoelectrocatalytiPerformance Performance and cubic micron particle has efficient, stable Optical Electro-Chemistry catalytic performance.
Optical Electro-Chemistry test all uses the three-electrode system of standard to carry out, wherein on electrochemical workstation (CHI 660D)
Polyhedral In2O3Micron crystalline substance, Pt (mesh) electrode, Ag/AgCl (3mol L-1KCl-filled) respectively as photo cathode,
To electrode and reference electrode.Electrolyte is 1mol/L NaOH solution (pH=13.6).Before test, first high pure nitrogen is passed through
Electrolyte is discharged the dissolved oxygen in electrolyzer, persistent period 1h.Light source uses 500W Xe lamp, power adjustable.Voltage scanning model
Enclose: it is the stone of 1cm that-0.6-0.9V (Ag/AgCl), scanning speed: 10mV/s. put into a thickness in the middle of light source and electrolyzer
English tank, it is therefore an objective to filter long wavelength's part of xenon lamp, it is to avoid the impact on photoelectrochemical property of heat effect.At xenon lamp irradiation
Under (270mW/cm2), cubic, truncation cubic, cuboctahedron shape, truncation cubic In2O3The light of micro-crystal
Electric current increases rapidly with scanning voltage, and octahedra shape In2O3The photocurrent variations of micro-crystal and Si is less obvious, explanation
The increase of photoelectric current is mainly due to { increase of the area ratio of 001} crystal face causes, as shown in Figure 6.In order to become apparent from
This phenomenon of explanation, compare magnitude of voltage at 0.22VAg/AgClTime polyhedral In2O3Micro-crystal density of photocurrent value.
0.22VAg/AgClIt it is the value of thermodynamics unlatching gesture (Onset potential) of testing herein condition.When voltage is
0.22VAg/AgClTime, cubic In2O3The photocurrent values of micro-crystal is about 2.1mA/cm2, it is octahedra shape In2O3Micro-
42 times of meter Jing Ti density of photocurrent, much larger than the photocurrent values 1.4mA/cm of truncated octahedron2, as shown in Figure 6.To sum up institute
State, polyhedral In in Optical Electro-Chemistry water splitting processes2O3The density of photocurrent value of micro-crystal with { shared by 001} crystal face
Ratio increases and increases.
Claims (3)
1.In2O3The preparation method that polyhedron micron is brilliant, is characterized in that preparing In with chemical vapour deposition technique2O3Polyhedron micron
The method of granule, first by high-purity for 300mg In2O3Powder and 150mg carbon dust are milled 10 ± 5min in mortar, make the two abundant
Mixing；Then being put into by mixture in chemical gaseous phase deposited tube, after mixture, at 1.5cm, placement surface has thick 10-50nm Au
The Si sheet of film, as the substrate collecting sample；Finally, deposited tube is passed through Ar gas and the O of 2% of 98%2Gas as carrier gas,
According to the 920-1000 DEG C of thermotonus 3 ± 1h set, it is cooled to room temperature, takes out Si substrate, obtain In in its surface2O3
Polyhedron micron particle.
In the most according to claim 12O3The preparation method that polyhedron micron is brilliant, is characterized in that grinding in agate mortar
10min so that it is diameter is about 10 μm, and then uniform spreading is in aluminium oxide boat；This aluminium oxide boat is put into horizontal CVD boiler tube
In；In course of reaction, carrier gas is high-purity argon by volume 98% and mixed gas of oxygen 2%, and flow is 150sccm；
The Si substrate being coated with Au film is placed at distance aluminium oxide boat 1.5cm, and puts in the little quartz ampoule that internal diameter is 1.6cm simultaneously,
Put into the most together in CVD boiler tube；At polyhedral In2O3Micron particle growth course, furnace temperature is respectively with the intensification speed of 50 DEG C/min
Degree is separately heated to 920,940,960,980 and 1000 DEG C and keeps 3h, air pressure to remain at a normal atmosphere；Upper
Under the conditions of stating corresponding growth temperature, In2O3The pattern of micron particle be respectively octahedron, truncated octahedron, cuboctahedron,
Truncation cube and cube.
3. the In described in claim 1 or 22O3Polyhedron micron is brilliant in preparing efficient stable Optical Electro-Chemistry water decomposition electrode
Application.
Priority Applications (1)
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