CN105118694A - Preparation method for aluminum-doped zinc oxide (AZO) nano array - Google Patents
Preparation method for aluminum-doped zinc oxide (AZO) nano array Download PDFInfo
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Abstract
The invention provides a preparation method for an aluminum-doped zinc oxide (AZO) nano array. The method is performed as follows: precisely controlling the concentration of chemical reaction solution by continuously injecting growing sources and doping sources at a constant speed to controllably prepare an aluminum-doped zinc oxide (AZO) array with high carrier concentration; compounding the aluminum-doped zinc oxide (AZO) array and a nickel oxide material to obtain a capacitor electrode material with high electricity capacity. The capacitor electrode material with high electricity capacity is attained in such a way that an aluminum-doped zinc oxide (AZO) array with high conductivity prepared by a continuous flow injecting method and a nickelnanosheet material with poor conductivity but high electricity capacity are combined. In comparison to a conventional hydrothermal method, the carrier concentration obtained from the preparation method provided in the invention increases three orders of magnitude. In the method, an aluminum-doped zinc oxide (AZO) material with high carrier concentration and a nickel oxide with poor conductivity are combined such that the advantages of the two materials are brought into full play and the electricity capacity of a capacitor is substantially increased. Beyond that, the continuous flow injecting and doping method provides a new idea for controllable precise doping. The method is simple in operation, cost-effective and enjoys great application prospects.
Description
Technical field
The present invention relates to the technical field of electrode material performance, particularly relate to a kind of preparation method of Al-Doped ZnO nano-array.
Background technology
Society, under energy crisis and the serious pressure of environmental pollution, the storage of the energy seems particularly important.Ultracapacitor, as a kind of novel energy storage device, has the advantages such as energy density is high, the discharge and recharge time is short, have extended cycle life and is studied widely and be applied in various electronic product.Determine that the key factor of ultracapacitor performance is the quality of electrode material chemical property, the electrode material therefore synthesizing a kind of function admirable has become the focus of people's research.Traditional electrode material for super capacitor can be divided into three major types, material with carbon element, conducting polymer materials and transistion metal compound, wherein transistion metal compound has multiple accessible valence state center, more easily there is reversible electrochemical reaction, therefore there is larger capacitance, as: NiO theoretical capacity can reach 2573Fg
-1, but the actual capacitance of transistion metal compound is but not very good, and main cause is its poorly conductive, and in order to address this problem, researcher proposes the method for various its conductivity of raising, as doping vario-property, preliminary treatment and composite modified.
Wherein composite modifiedly be considered to the most effective modified method of one.Namely composite modified be a kind of method improving material conductivity together with Material cladding high to transistion metal compound and conductivity, mainly contains at present: Graphene, carbon fiber, zinc oxide and metal nanoparticle for composite modified material.Zinc oxide, due to cheap and environmental friendliness, receives and favors widely.In addition, One-Dimensional ZnO nanometer rods becomes the focus material of composite modified research due to its unidirectional electron transmission characteristic.In the recent period, some scholars are also had to attempt adopting the good Al doping zinc oxide nanometer rod of conductivity to improve the conductivity of transistion metal compound.High and the formation polycrystal film not easily electric transmission mostly of traditional ald doping and magnetron sputtering doping techniques complex process, cost.(the LiuJ such as J.Liu, XuL, WeiB, etal.One-stephydrothermalsynthesisandopticalpropertiesof aluminiumdopedZnOhexagonalnanoplatesonazincsubstrate.Cry stEngComm, 2011,13:1283-1286) hydrothermal reaction at low temperature direct and with low cost is fast adopted to successfully synthesize Al doping zinc oxide nanometer sheet, but due to the change of reactant concentration in reaction cavity, be difficult to effectively ensure the pattern of reactant and the uniformity of doping.
Summary of the invention
In order to solve the problem, the invention provides a kind of preparation method of Al-Doped ZnO nano-array, described preparation method injects growth source and doped source by continuous constant rate of speed, the concentration of accurate control chemical reaction liquid, thus controlled synthesis goes out the Al-Doped ZnO array of high carrier concentration, and obtain the capacitor electrode material of high power capacity with nickel oxide material compound;
Further, described preparation method's concrete steps are as follows:
(1) glass is carried out cleaning also magnetron sputtering deposition and mix the zinc-oxide film of Al as crystal seed layer, this substrate crystal seed layer is upwards placed in the liquid-phase chemical reaction chamber of continuous growing device;
(2) prepare 50mM zinc nitrate and 5mM aluminum nitrate mixed aqueous solution and be injected into one of them syringe of continuous growing device used;
(3) preparing 50mM hexa is injected in another syringe of auto levelizer as alkali salt;
(4) by heating water bath, liquid-phase chemical reaction cavity temperature is remained on 95 DEG C, the setting constant charge velocity of reaction source (6ml/h) and constant injection length (16h) start the preparation of continuous flow injection and mix aluminium ZnO array;
(5), after hydro-thermal reaction terminates, stop heating reaction chamber, to be cooled to room temperature, take out sample, with deionized water rinsing and nitrogen dry up;
(6) capacitor electrode material is constructed by chemical bath deposition method mixing aluminium ZnO array outer cladding NiO nanometer sheet;
Further, the syringe of described continuous growing device has two, can push ahead growth-promoting media is injected reaction chamber with constant speed, and meanwhile, the waste liquid that reaction produces can be discharged with same speed;
Further, the cleaning method of described glass is respectively with acetone, isopropyl alcohol, deionized water ultrasonic cleaning 10min respectively, dries up subsequently with nitrogen;
Further, the zinc oxide films film thickness that described magnetron sputtering deposition mixes Al is 500nm;
Further, described chemical deposition for be 1M nickelous sulfate using 40ml concentration, 30ml concentration is that 0.25M potassium peroxydisulfate and 10ml ammoniacal liquor join in 100ml beaker successively as deposit solution, by the aluminium doping zinc oxide nanometer rod array sample prepared, stand upright on the deposition reaction carrying out nickel source in above-mentioned deposit solution, react under 25 degrees Celsius after 30 minutes, take out sample, anneal 1.5 hours in 350 degree of air;
Further, a kind of capacitor electrode material, the aluminium-doped zinc oxide nano-array of the high conductivity of described electrode material prepared by continuous flow injection with poorly conductive but the high nickel oxide nano sheet material of capacitance in conjunction with gained;
Further, the thickness of described nickel oxide nano sheet material is 100-200nm.
Beneficial effect of the present invention is as follows:
1) use two syringes, push ahead growth-promoting media is injected reaction chamber with constant speed, waste liquid is discharged with same speed, controls the constant concentration of growth-promoting media in reaction chamber with this;
2) magnetron sputtering deposition mixes the zinc oxide films film thickness of Al is 500nm, and it is as the crystal seed layer mixing aluminium ZnO nano array hydrothermal growth thus ensures its better crystallinity and chemical orientation;
3) constant charge velocity accurately can control the ratio of growth source, doped source and alkali salt, keeps constant pH value, is conducive to Al atom and substitutes Zn atom, thus synthesizes even aluminium doping zinc oxide nanometer rod array;
4) by the aluminium-doped zinc oxide nano-array of the high conductivity prepared by continuous flow injection with poorly conductive but the high nickel oxide nano sheet material of capacitance be combined, both advantages can be given full play to, increase substantially the capacitance of electrode material for super capacitor;
5) Al-Doped ZnO material carrier concentration compared with common hydro thermal method that prepared by the present invention improves 3 orders of magnitude.The aluminium-doped zinc oxide material of this high carrier concentration and the nickel oxide of poorly conductive are combined, gives full play to both advantages, the capacitance of capacitor can be increased substantially;
6) this continuous flow injection doping method is that controlled accurate doping provides new approaches and technique is simple, with low cost, has good application prospect.
Accompanying drawing explanation
Fig. 1 is continuous flow injection device figure;
Fig. 2 is continuously growth Al-Doped ZnO array scanning Electronic Speculum figure;
Fig. 3 is continuously growth Al-Doped ZnO array scanning energy spectrogram;
Fig. 4 is conventional hydrothermal method Al-Doped ZnO array carrier concentration figure;
Fig. 5 is continuously growth Al-Doped ZnO array carrier concentration figure;
Fig. 6 is conventional hydrothermal method Al-Doped ZnO array and grows Al-Doped ZnO Array Cycle volt-ampere curve and constant current charge-discharge curve comparison figure continuously;
Fig. 7 is embodiment 1 growth Al-Doped ZnO array scanning Electronic Speculum figure continuously;
Fig. 8 is embodiment 2 growth Al-Doped ZnO array scanning Electronic Speculum figure continuously;
Fig. 9 is embodiment 3 growth Al-Doped ZnO array scanning Electronic Speculum figure continuously.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is explained in further detail.Should be appreciated that specific embodiment described herein only for explaining the present invention, being not intended to limit the present invention.On the contrary, the present invention is contained any by the substituting of making on marrow of the present invention and scope of defining of claim, amendment, equivalent method and scheme.Further, in order to make the public have a better understanding to the present invention, in hereafter details of the present invention being described, detailedly describe some specific detail sections.Do not have the description of these detail sections can understand the present invention completely for a person skilled in the art yet.
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but not as a limitation of the invention.Most preferred embodiment is enumerated below for of the present invention:
A kind of preparation method of Al-Doped ZnO nano-array, described preparation method injects growth source and doped source by continuous constant rate of speed, the concentration of accurate control chemical reaction liquid, thus controlled synthesis goes out the Al-Doped ZnO array of high carrier concentration, and obtain the capacitor electrode material of high power capacity with nickel oxide material compound, described preparation method's concrete steps are as follows:
(1) glass is carried out cleaning also magnetron sputtering deposition and mix the zinc-oxide film of Al as crystal seed layer, this substrate crystal seed layer is upwards placed in the liquid-phase chemical reaction chamber of continuous growing device;
(2) prepare 50mM zinc nitrate 5mM aluminum nitrate mixed aqueous solution and be injected into one of them syringe of continuous growing device used;
(3) preparing 50mM hexa is injected in another syringe of auto levelizer as alkali salt;
(4) by heating water bath, liquid-phase chemical reaction cavity temperature is remained on 95 DEG C, the setting constant charge velocity of reaction source (6ml/h) and constant injection length (16h) start the preparation of continuous flow injection and mix aluminium ZnO array;
(5), after hydro-thermal reaction terminates, stop heating reaction chamber, to be cooled to room temperature, take out sample, with deionized water rinsing and nitrogen dry up;
(6) capacitor electrode material is constructed by chemical bath deposition method mixing aluminium ZnO array outer cladding NiO nanometer sheet.
The syringe of described continuous growing device has two, can push ahead with constant speed and growth-promoting media is injected reaction chamber, meanwhile, the waste liquid that reaction produces can be discharged with same speed, the cleaning method of described glass is for use acetone respectively, isopropyl alcohol, deionized water is ultrasonic cleaning 10min respectively, dry up with nitrogen subsequently, described chemical deposition is for being 1M nickelous sulfate by 40ml concentration, 30ml concentration is that 0.25M potassium peroxydisulfate and 10ml ammoniacal liquor join in 100ml beaker successively as deposit solution, by the aluminium doping zinc oxide nanometer rod array sample prepared, stand upright on the deposition reaction carrying out nickel source in above-mentioned deposit solution, react under 25 degrees Celsius after 30 minutes, take out sample, anneal 1.5 hours in 350 degree of air, the zinc oxide films film thickness that described magnetron sputtering deposition mixes Al is 500nm.
A kind of capacitor electrode material, the aluminium-doped zinc oxide nano-array of the high conductivity of described electrode material prepared by continuous flow injection with poorly conductive but the high nickel oxide nano sheet material of capacitance in conjunction with gained, the thickness of described nickel oxide nano sheet material is 100-200nm.
Embodiment 1:
(1) glass is carried out cleaning also magnetron sputtering deposition and mix the zinc-oxide film of Al as crystal seed layer, this substrate crystal seed layer is upwards placed in the liquid-phase chemical reaction chamber of continuous growing device;
(2) prepare 50mM zinc nitrate and 5mM aluminum nitrate mixed aqueous solution and be injected into one of them syringe of continuous growing device used;
(3) preparing 50mM hexa is injected in another syringe of auto levelizer as alkali salt;
(4) by heating water bath, liquid-phase chemical reaction cavity temperature is remained on 95 DEG C, the setting constant charge velocity of reaction source (6ml/h) and constant injection length (16h) start the preparation of continuous flow injection and mix aluminium ZnO array;
(5), after hydro-thermal reaction terminates, stop heating reaction chamber, to be cooled to room temperature, take out sample, with deionized water rinsing and nitrogen dry up;
(6) be 1M nickelous sulfate using 40ml concentration, 30ml concentration is that 0.25M potassium peroxydisulfate and 10ml ammoniacal liquor join in 100ml beaker successively as deposit solution.By the aluminium doping zinc oxide nanometer rod array sample of having synthesized, stand upright on the deposition reaction carrying out nickel source in above-mentioned deposit solution.React under 25 degrees Celsius after 30 minutes, take out sample, in 350 degree of air, annealing obtains electrode material for super capacitor in 1.5 hours.
Embodiment 2:
Other steps are as constant in embodiment 1, do not repeat them here, just step (3) changes into: preparation 50mM hexa and 5M sodium hydroxide solution are as alkali lye respectively, keep the addition of hexa constant, by the addition that changes NaOH alkali lye PH is adjusted to after 5.00 and is injected in another syringe of device.
Embodiment 3:
Other steps are as constant in embodiment 1, do not repeat them here, just step (3) changes into: preparation 50mM hexa and 5M sodium hydroxide solution are as alkali lye respectively, keep the addition of hexa constant, by the addition that changes NaOH alkali lye PH is adjusted to after 6.00 and is injected in another syringe of device.
Above-described embodiment, the just one of the present invention's more preferably embodiment, the usual change that those skilled in the art carries out within the scope of technical solution of the present invention and replacing all should be included in protection scope of the present invention.
Claims (8)
1. the preparation method of an Al-Doped ZnO nano-array, it is characterized in that, described preparation method injects growth source and doped source by continuous constant rate of speed, the concentration of accurate control chemical reaction liquid, thus controlled synthesis goes out the Al-Doped ZnO array of high carrier concentration, and obtain the capacitor electrode material of high power capacity with nickel oxide material compound.
2. preparation method according to claim 1, is characterized in that, described preparation method's concrete steps are as follows:
(1) glass is carried out cleaning also magnetron sputtering deposition and mix the zinc-oxide film of Al as crystal seed layer, this substrate crystal seed layer is upwards placed in the liquid-phase chemical reaction chamber of continuous growing device;
(2) prepare 50mM zinc nitrate and 5mM aluminum nitrate mixed aqueous solution and be injected into one of them syringe of continuous growing device used;
(3) preparing 50mM hexa is injected in another syringe of auto levelizer as alkali salt;
(4) by heating water bath, liquid-phase chemical reaction cavity temperature is remained on 95 DEG C, the setting constant charge velocity of reaction source (6ml/h) and constant injection length (16h) start the preparation of continuous flow injection and mix aluminium ZnO array;
(5), after hydro-thermal reaction terminates, stop heating reaction chamber, to be cooled to room temperature, take out sample, with deionized water rinsing and nitrogen dry up;
(6) capacitor electrode material is constructed by chemical bath deposition method mixing aluminium ZnO array outer cladding NiO nanometer sheet.
3. preparation method according to claim 2, it is characterized in that, the syringe of described continuous growing device has two, can push ahead growth-promoting media is injected reaction chamber with constant speed, meanwhile, the waste liquid that reaction produces can be discharged with same speed.
4. preparation method according to claim 2, is characterized in that, the cleaning method of described glass is respectively with acetone, isopropyl alcohol, deionized water ultrasonic cleaning 10min respectively, dries up subsequently with nitrogen.
5. preparation method according to claim 2, is characterized in that, the zinc oxide films film thickness that described magnetron sputtering deposition mixes Al is 500nm.
6. preparation method according to claim 2, it is characterized in that, described chemical deposition for be 1M nickelous sulfate using 40ml concentration, 30ml concentration is that 0.25M potassium peroxydisulfate and 10ml ammoniacal liquor join in 100ml beaker successively as deposit solution, by the aluminium doping zinc oxide nanometer rod array sample prepared, stand upright on the deposition reaction carrying out nickel source in above-mentioned deposit solution, react under 25 degrees Celsius after 30 minutes, take out sample, anneal 1.5 hours in 350 degree of air.
7. a capacitor electrode material, based on the preparation method one of the claims 1-6 Suo Shu, its feature with, the aluminium-doped zinc oxide nano-array of the high conductivity of described electrode material prepared by continuous flow injection with poorly conductive but the high nickel oxide nano sheet material of capacitance in conjunction with gained.
8. electrode material according to claim 7, is characterized in that, the thickness of described nickel oxide nano sheet material is 100-200nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107393654A (en) * | 2017-07-11 | 2017-11-24 | 扬州乾照光电有限公司 | A kind of method for the ZnO transparent conductive thin film that nanostructured is formed on substrate |
| CN107715890A (en) * | 2017-11-02 | 2018-02-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of heterogeneous ozone catalyst and products thereof and application |
| CN108597879A (en) * | 2018-03-19 | 2018-09-28 | 西北师范大学 | A kind of TiO2The preparation method of nano wire/NiO nanometer sheets/porphyrin composite material |
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| CN102368502A (en) * | 2011-10-13 | 2012-03-07 | 上海电力学院 | Zinc oxide film doped with Al and preparation method thereof |
| CN104020260A (en) * | 2014-06-18 | 2014-09-03 | 清华大学 | NiO and Al-doped ZnO heterogeneous nano structure as well as preparation method and application |
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| CN102368502A (en) * | 2011-10-13 | 2012-03-07 | 上海电力学院 | Zinc oxide film doped with Al and preparation method thereof |
| CN104020260A (en) * | 2014-06-18 | 2014-09-03 | 清华大学 | NiO and Al-doped ZnO heterogeneous nano structure as well as preparation method and application |
Non-Patent Citations (3)
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| JANG BO SHIM,ET AL.: ""Electrical properties of rapid hydrothermal synthesised Al-doped zinc oxide nanowires in flexible electronics"", 《MICRO & NANO LETTERS》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107393654A (en) * | 2017-07-11 | 2017-11-24 | 扬州乾照光电有限公司 | A kind of method for the ZnO transparent conductive thin film that nanostructured is formed on substrate |
| CN107715890A (en) * | 2017-11-02 | 2018-02-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of heterogeneous ozone catalyst and products thereof and application |
| CN108597879A (en) * | 2018-03-19 | 2018-09-28 | 西北师范大学 | A kind of TiO2The preparation method of nano wire/NiO nanometer sheets/porphyrin composite material |
| CN108597879B (en) * | 2018-03-19 | 2020-09-22 | 西北师范大学 | TiO 22Preparation method of nanowire/NiO nanosheet/porphyrin composite material |
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