CN102891008A - Nickel hydroxide nanosheet thin-film material as well as preparation method and application thereof - Google Patents
Nickel hydroxide nanosheet thin-film material as well as preparation method and application thereof Download PDFInfo
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- CN102891008A CN102891008A CN2011102055861A CN201110205586A CN102891008A CN 102891008 A CN102891008 A CN 102891008A CN 2011102055861 A CN2011102055861 A CN 2011102055861A CN 201110205586 A CN201110205586 A CN 201110205586A CN 102891008 A CN102891008 A CN 102891008A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a nickel hydroxide nanosheet thin-film material as well as a preparation method and application thereof, and belongs to the technical field of nanometer thin-film materials and the technical field of chemical energy storage. Nickel hydroxide nanosheets vertically and sequentially grow on a foam nickel base, wherein the particle size of the nickel hydroxide nanosheets is 0.7-1.5 microns and the thickness is 5-9 nanometers. The preparation method comprises the following steps of: respectively placing foam nickel base sheets in hydrochloric acid, ionized water and ethanol for ultrasonic washing, dissolving soluble nickel salt and hexamine in deionized water to obtain clear solution, obliquely placing the foam nickel sheets in a reaction still, transferring the nickel salt and hexamine solution to the reaction still to carry out hydrothermal reaction, cooling to room temperature by using cooling water after the reaction, taking the foam nickel sheets out from the reaction still for cleaning via water and ethanol, and placing the products in a dryer until the products are dried. The integrated product has large capacitance value (range: 1500-3000F/g or 5-12F/cm<2>), can be well kept under high-current density and has good cycle performance, so that the integrated product is a super capacitor material with huge application prospect.
Description
Technical field
The present invention relates to a kind of nickel hydroxide nano sheet film materials and its preparation method and application, belong to inorganic advanced nano-sized membrane technical field.
Background technology
Ultracapacitor has cycle life, the environmentally safe of very high power density, higher energy density, overlength and the advantage [Chinese science and technology information, 2010,17:36] such as can under low pressure operate, and is expected to become novel green energy resource of 21 century.As everyone knows, unformed ruthenium oxide hydration is the most promising electrode material of high power high-energy-density ultracapacitor, but its expensive, scarcity of resources [Nano Lett.2006,6,2690-2695], used electrolyte pollution environment has limited business development greatly.And nickel hydroxide possesses advantages such as chemical property is good, relative low price have caused broad research and concern in the electrochemical capacitance field in the recent period.Because pattern, the size of nano material play conclusive effect for its performance, therefore, the nickel hydroxide nano material of large-area homogeneous structural and size becomes the emphasis of domestic and international research in addition.
Present stage, multiple nickel hydroxide synthetic with and electrochemical capacitance character reported, such as nickel hydroxide and graphene composite material [J.Am.Chem.Sci.2010,132,7472-7477], nickel hydroxide three-dimensional structure film [Chem.Commun., 2008,6537-6539] etc.Its preparation method generally adopts precipitation from homogeneous solution [J.Power.Sources., 2009,188,338-342], negative electrode or anodic electrodeposition method [Electro.Commum., 2007,9,869-874; Int.J.Electrochem.Sci., 2009,4,1052-1062] etc.These nickel hydroxides are the preparation method be widely adopted, but they all have certain apparent limitation, if any the relatively high synthesis temperature of needs, the product degree of crystallinity that has is relatively poor, the surface is residual impurity easily; What have has obvious pollution to environment; Being not easy of having realized the size of granularity and the control that distributes.And the product of filming has the structure homogeneous, and without reuniting, the large characteristics of relative surface area are by many worker's extensive concerns.Therefore develop a kind of simple to operately, efficient is high, cost is low, eco-friendly preparation method, and the nickel hydroxide film of the characteristics such as obtain the structure homogeneous, arrangement is regular, controllability is good, tool is of great significance.
Summary of the invention
The purpose of this invention is to provide a kind of nickel hydroxide nano sheet film and preparation method thereof, be growth nickel hydroxide nano sheet thin film technology method on a kind of nickel foam sheet, nickel hydroxide film of the present invention can be used as the super capacitor material.This inventive method need not to use template and surfactant, utilizes the hydrolysis of nickel salt under the hydrothermal condition, prepares very simply fine and close uniformly nickel hydroxide nano sheet order thin film in the nickel foam substrate.The advantage of the method is simple to operate, and efficient is high, cost is low, the characteristics such as environmental friendliness, good reproducibility, and the characteristics such as product has integral type, structure homogeneous, arrangement is regular, pattern is controlled.Simultaneously, the nickel hydroxide nano sheet film morphology homogeneous of preparation, vertically growth, particle diameter is the 0.7-1.5 micron, thickness is the 5-9 nanometer.In addition, the product of this integral type has very large capacitance, also can well keep under high current density, and cycle performance is fine, is a kind of super capacitor material with very big application prospect.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of nickel hydroxide nano sheet film materials is characterized in that, the nickel hydroxide nano sheet vertically is grown in the nickel foam substrate in an orderly manner, and nickel hydroxide nano sheet particle diameter is the 0.7-1.5 micron, and thickness is the 5-9 nanometer.
Utilization is characterized in that in nickel foam sheet growth nickel hydroxide nano sheet thin film technology method the method comprises the steps:
A. get the nickel foam substrate, put into the hydrochloric acid supersound washing, then be transferred in deionized water and the ethanol, respectively supersound washing;
B. soluble nickel salt and hexa are dissolved in the deionized water and obtain, be stirred well to settled solution, obtaining nickel salt concentration is the 0.05-0.25 mol/L, and hexa concentration is the solution of 0.05-0.5 mol/L;
C. the tilting reactor of putting into of the nickel foam sheet of step a being processed, again the solution that obtains among the step b is transferred to and carries out hydro-thermal reaction in the reactor, hydrothermal temperature is 70-140 ℃, and the reaction time is 6-48 hour, after reaction finishes with water quench to room temperature;
D. the nickel foam sheet in the reactor is taken out water, alcohol flushing, and water and respectively ultrasonic cleaning of ethanol;
E. the product that steps d is obtained is put into baking oven until dry the nickel hydroxide nano sheet film film that can obtain growing on the nickel foam.
Soluble nickel salt among the step b comprises Nickelous nitrate hexahydrate, single nickel salts, Nickel dichloride hexahydrate.
Nickel hydroxide nano sheet film materials of the present invention is as super capacitor material.
The present invention is the nickel hydroxide nano sheet that direct growth goes out orderly densification in substrate on the nickel foam sheet, and the method is synthetic under simple hydrothermal condition, and method is easy, and is with low cost, good reproducibility; Do not adopt any organic solvent and surfactant, very friendly to environment; The product structure homogeneous, the ordered arrangement that obtain, even more important is that this is an integral type material, has the character such as good separation, conduction; By kind and the concentration of nickel salt in the control solution, can synthesize the nanometer sheet with different size size and density degree in addition, realize that the pattern of material is controlled.Because this sintetics has structural advantage as above, so that (capacitance is large corresponding good electrochemical capacitance speciality to have occurred, cyclicity is good, can fine must the maintenance under high low current density), it will have broad application prospects in fields such as ultracapacitor, catalysis, electro-catalysis, electricity absorption.
Description of drawings
Fig. 1 is the stereoscan photograph of nickel hydroxide nano sheet film in the embodiment of the invention 1.
Fig. 2 is the XRD spectra of nickel hydroxide nano sheet film in the embodiment of the invention 1.
Fig. 3 is the electric capacity cyclic voltammogram of nickel hydroxide nano sheet film in the embodiment of the invention 1.
Fig. 4 is the capacitance characteristic figure of nickel hydroxide nano sheet film in the embodiment of the invention 1.
Fig. 5 is the electric capacity cycle graph of nickel hydroxide nano sheet film in the embodiment of the invention 1.
Fig. 6 is the stereoscan photograph of nickel hydroxide nano sheet film in the embodiment of the invention 2.
Fig. 7 is the XRD spectra of nickel hydroxide nano sheet film in the embodiment of the invention 2.
Fig. 8 is the stereoscan photograph of nickel hydroxide nano sheet film in the embodiment of the invention 3.
Fig. 9 is the stereoscan photograph of nickel hydroxide nano sheet film in the embodiment of the invention 4.
Embodiment
The present invention is described in further detail below in conjunction with several embodiment:
Embodiment 1:
A. get the nickel foam sheet, put into the hydrochloric acid supersound washing, then be transferred in deionized water and the ethanol, respectively supersound washing;
B. preparing Nickelous nitrate hexahydrate concentration is that 0.125 mol/L and hexa concentration are the solution of 0.25 mol/L, fully stirs and obtains stable homogeneous solution;
C. the nickel foam sheet that step a is obtained is tilting to be put into 40 milliliters and has the teflon-lined autoclave, again solution among the step b is transferred in the reactor at 100 ℃ of lower hydro-thermal 10h, after reaction finishes with water quench to room temperature, cooling time was less than 15 minutes;
D. the nickel sheet in the reactor is taken out water and alcohol flushing, at last respectively ultrasonic cleaning in water and ethanol;
E. the product that steps d is obtained is put into 100 ℃ of baking ovens dries 6h, can obtain the nickel hydroxide nano sheet film of vertical ordering growth on the nickel foam sheet, and nickel hydroxide nano sheet particle diameter is the 0.7-1.5 micron, and the thickness degree is the 5-9 nanometer.
Its stereoscan photograph is referring to Fig. 1, and XRD is referring to Fig. 2, and the electric capacity cyclic voltammogram is referring to Fig. 3, and capacitance characteristic figure sees Fig. 4, and the electric capacity cycle graph is seen Fig. 5.
A. get the nickel foam sheet, put into the hydrochloric acid supersound washing, then be transferred in deionized water and the ethanol, respectively supersound washing;
B. preparing Nickelous nitrate hexahydrate concentration is that 0.05 mol/L and hexa concentration are the solution of 0.05 mol/L, fully stirs and obtains stable homogeneous solution;
C. the nickel foam sheet that step a is obtained is tilting to be put into 40 milliliters and has the teflon-lined autoclave, again solution among the step b is transferred in the reactor at 140 ℃ of lower hydro-thermal 48h, after reaction finishes with water quench to room temperature, cooling time was less than 15 minutes;
D. the nickel sheet in the reactor is taken out water and alcohol flushing, at last respectively ultrasonic cleaning in water and ethanol;
E. the product that steps d is obtained is put into 100 ℃ of baking ovens dries 6h, can obtain the nickel hydroxide nano sheet film of vertical ordering growth on the nickel foam sheet, and nickel hydroxide nano sheet particle diameter is the 0.7-1.5 micron, and the thickness degree is the 5-9 nanometer.
Its stereoscan photograph is referring to Fig. 6, and XRD is referring to Fig. 7, and capacitance characteristic, electric capacity cyclic voltammogram, electric capacity cycle graph and embodiment 1 are basically identical.
Embodiment 3
A. get the nickel foam sheet, put into the hydrochloric acid supersound washing, then be transferred in deionized water and the ethanol, respectively supersound washing;
B. preparing Nickelous nitrate hexahydrate concentration is that 0.25 mol/L and hexa concentration are the solution of 0.5 mol/L, fully stirs and obtains stable homogeneous solution;
C. the nickel foam sheet that step a is obtained is tilting to be put into 40 milliliters and has the teflon-lined autoclave, again solution among the step b is transferred in the reactor at 70 ℃ of lower hydro-thermal 6h, after reaction finishes with water quench to room temperature, cooling time was less than 15 minutes;
D. the nickel sheet in the reactor is taken out water and alcohol flushing, at last respectively ultrasonic cleaning in water and ethanol;
E. the product that steps d is obtained is put into 100 ℃ of baking ovens dries 6h, can obtain the nickel hydroxide nano sheet film of vertical ordering growth on the nickel foam sheet, and nickel hydroxide nano sheet particle diameter is the 0.7-1.5 micron, and the thickness degree is the 5-9 nanometer.
Its stereoscan photograph is referring to Fig. 8, and XRD, capacitance characteristic, electric capacity cyclic voltammogram and electric capacity cycle graph and embodiment 1 are basically identical.
Embodiment 4
A. get the nickel foam sheet, put into the hydrochloric acid supersound washing, then be transferred in deionized water and the ethanol, respectively supersound washing;
B. preparing Nickelous nitrate hexahydrate concentration is that 0.2 mol/L and hexa concentration are the solution of 0.4 mol/L, fully stirs and obtains stable homogeneous solution;
C. the nickel foam sheet that step a is obtained is tilting to be put into 40 milliliters and has the teflon-lined autoclave, again solution among the step b is transferred in the reactor at 120 ℃ of lower hydro-thermal 24h, after reaction finishes with water quench to room temperature, cooling time was less than 15 minutes;
D. the nickel sheet in the reactor is taken out water and alcohol flushing, at last respectively ultrasonic cleaning in water and ethanol;
E. the product that steps d is obtained is put into 100 ℃ of baking ovens dries 6h, can obtain the nickel hydroxide nano sheet film of vertical ordering growth on the nickel foam sheet, and nickel hydroxide nano sheet particle diameter is the 0.7-1.5 micron, and the thickness degree is the 5-9 nanometer.
Its stereoscan photograph is referring to Fig. 9, and XRD, capacitance characteristic, electric capacity cyclic voltammogram and electric capacity cycle graph and embodiment 1 are basically identical.
Claims (4)
1. a nickel hydroxide nano sheet film materials is characterized in that, the nickel hydroxide nano sheet vertically is grown in the nickel foam substrate in an orderly manner, and nickel hydroxide nano sheet particle diameter is the 0.7-1.5 micron, and thickness is the 5-9 nanometer.
2. in the preparation method of nickel foam sheet growth nickel hydroxide nano sheet film materials, it is characterized in that the method comprises the steps:
A. get the nickel foam substrate, put into the hydrochloric acid supersound washing, then be transferred in deionized water and the ethanol, respectively supersound washing;
B. soluble nickel salt and hexa are dissolved in the deionized water and obtain, be stirred well to settled solution, obtaining nickel salt concentration is the 0.05-0.25 mol/L, and hexa concentration is the solution of 0.05-0.5 mol/L;
C. the tilting reactor of putting into of the nickel foam sheet of step a being processed, again the solution that obtains among the step b is transferred to and carries out hydro-thermal reaction in the reactor, hydrothermal temperature is 70-140 ℃, and the reaction time is 6-48 hour, after reaction finishes with water quench to room temperature;
D. the nickel foam sheet in the reactor is taken out water, alcohol flushing, and water and respectively ultrasonic cleaning of ethanol;
E. the product that steps d is obtained is put into baking oven until dry the nickel hydroxide nano sheet film film that can obtain growing on the nickel foam.
3. according to the preparation method of claim 2, it is characterized in that soluble nickel salt is Nickelous nitrate hexahydrate among the step b, single nickel salts, Nickel dichloride hexahydrate.
4. a kind of nickel hydroxide nano sheet film materials of claim 1 is as super capacitor material.
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Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103101981A (en) * | 2013-02-02 | 2013-05-15 | 山东理工大学 | Method for preparing Ni(OH)2 nanosheet array film by hydrothermal method |
| CN104201380A (en) * | 2014-08-19 | 2014-12-10 | 北京科技大学 | Preparation method of nano Ni3S2 material with lamellar structure |
| CN104226330A (en) * | 2013-06-07 | 2014-12-24 | 北京化工大学 | Au/Co(OH)2 nano-array structured catalyst |
| CN104291386A (en) * | 2014-10-10 | 2015-01-21 | 九江学院 | Preparation method of two-dimensional nickel hydroxide ultrathin nano-film |
| CN105033241A (en) * | 2015-06-04 | 2015-11-11 | 北京化工大学 | Ultrathin metallic nickel nanosheet, manufacturing method thereof and application of nanosheets as electrode materials |
| CN105347406A (en) * | 2015-12-04 | 2016-02-24 | 厦门大学 | Preparation method for nickel hydroxide ultrathin nanosheet |
| CN105469901A (en) * | 2015-11-20 | 2016-04-06 | 燕山大学 | In-situ-growth-based method for preparing nickel hydroxide-nickel oxide film electrode |
| CN105720236A (en) * | 2016-03-27 | 2016-06-29 | 华南理工大学 | Foamed nickel self-supported flake-shaped Ni3P/C composite material for sodium ion battery negative electrode and preparation method for composite material |
| CN106082364A (en) * | 2016-06-18 | 2016-11-09 | 合肥松雷信息科技有限公司 | A kind of preparation method of β nickel hydroxide nano sheet |
| CN106848278A (en) * | 2017-01-10 | 2017-06-13 | 广西大学 | The preparation method of metallic compound nano structural membrane material |
| CN107758750A (en) * | 2017-10-19 | 2018-03-06 | 郑州比克电池有限公司 | A kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape |
| CN109590000A (en) * | 2019-01-23 | 2019-04-09 | 中国科学院过程工程研究所 | It is a kind of for being catalyzed the catalyst and preparation method thereof of hydrogen peroxide oxidation NO |
| CN109637825A (en) * | 2018-12-13 | 2019-04-16 | 广东工业大学 | A kind of nanometer nickel sulfide piece/carbon quantum dot composite material and preparation method and application |
| CN109659143A (en) * | 2018-11-23 | 2019-04-19 | 暨南大学 | A kind of nickel hydroxide/three nickel of curing/foam nickel composite and the preparation method and application thereof |
| CN109830380A (en) * | 2019-02-18 | 2019-05-31 | 南阳理工学院 | A kind of electrode material for super capacitor, preparation method and application |
| CN110038577A (en) * | 2019-05-20 | 2019-07-23 | 南昌航空大学 | Synthetic method of the one step growth in situ in the class alpha-phase nickel hydroxide nanometer sheet of carbon cloth substrate |
| CN110040792A (en) * | 2019-03-04 | 2019-07-23 | 天津大学 | Preparation method of nickel hydroxide nanosheet array material growing on surface of foamed nickel |
| CN110129815A (en) * | 2019-04-24 | 2019-08-16 | 北京大学深圳研究生院 | Modified TM-LDH nano material, preparation method and application |
| CN110327930A (en) * | 2019-06-20 | 2019-10-15 | 武汉理工大学 | Low crystallization classification hydroxy nickel oxide nano-chip arrays and its preparation method and application |
| CN111276337A (en) * | 2019-12-13 | 2020-06-12 | 湖北大学 | Based on β -Ni (OH)2Manufacturing method of flexible solid-state supercapacitor |
| CN111943286A (en) * | 2020-08-18 | 2020-11-17 | 中国人民解放军空军预警学院雷达士官学校 | Nickel-nickel hydroxide composite film electrode and preparation method and application thereof |
| CN114558465A (en) * | 2020-11-27 | 2022-05-31 | 中国科学院大连化学物理研究所 | Preparation and application of porous nickel hydroxide ion screening membrane |
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| CN103101981A (en) * | 2013-02-02 | 2013-05-15 | 山东理工大学 | Method for preparing Ni(OH)2 nanosheet array film by hydrothermal method |
| CN103101981B (en) * | 2013-02-02 | 2016-06-15 | 山东理工大学 | Hydro-thermal method prepares Ni (OH)2The method of nano-chip arrays thin film |
| CN104226330A (en) * | 2013-06-07 | 2014-12-24 | 北京化工大学 | Au/Co(OH)2 nano-array structured catalyst |
| CN104226330B (en) * | 2013-06-07 | 2017-09-29 | 北京化工大学 | A kind of Au/Co (OH)2Nano array structure catalyst |
| CN104201380A (en) * | 2014-08-19 | 2014-12-10 | 北京科技大学 | Preparation method of nano Ni3S2 material with lamellar structure |
| CN104291386B (en) * | 2014-10-10 | 2016-04-06 | 九江学院 | A kind of preparation method of two-dimentional nickel hydroxide ultrathin nanometer film |
| CN104291386A (en) * | 2014-10-10 | 2015-01-21 | 九江学院 | Preparation method of two-dimensional nickel hydroxide ultrathin nano-film |
| CN105033241A (en) * | 2015-06-04 | 2015-11-11 | 北京化工大学 | Ultrathin metallic nickel nanosheet, manufacturing method thereof and application of nanosheets as electrode materials |
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| CN106082364A (en) * | 2016-06-18 | 2016-11-09 | 合肥松雷信息科技有限公司 | A kind of preparation method of β nickel hydroxide nano sheet |
| CN106848278A (en) * | 2017-01-10 | 2017-06-13 | 广西大学 | The preparation method of metallic compound nano structural membrane material |
| CN107758750A (en) * | 2017-10-19 | 2018-03-06 | 郑州比克电池有限公司 | A kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape |
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| CN110040792A (en) * | 2019-03-04 | 2019-07-23 | 天津大学 | Preparation method of nickel hydroxide nanosheet array material growing on surface of foamed nickel |
| CN110040792B (en) * | 2019-03-04 | 2021-08-27 | 天津大学 | Preparation method of nickel hydroxide nanosheet array material growing on surface of foamed nickel |
| CN110129815B (en) * | 2019-04-24 | 2020-10-16 | 北京大学深圳研究生院 | Modified TM-LDH nano material, preparation method and application thereof |
| CN110129815A (en) * | 2019-04-24 | 2019-08-16 | 北京大学深圳研究生院 | Modified TM-LDH nano material, preparation method and application |
| CN110038577A (en) * | 2019-05-20 | 2019-07-23 | 南昌航空大学 | Synthetic method of the one step growth in situ in the class alpha-phase nickel hydroxide nanometer sheet of carbon cloth substrate |
| CN110327930A (en) * | 2019-06-20 | 2019-10-15 | 武汉理工大学 | Low crystallization classification hydroxy nickel oxide nano-chip arrays and its preparation method and application |
| CN110327930B (en) * | 2019-06-20 | 2022-02-18 | 武汉理工大学 | Low-crystallization graded nickel oxyhydroxide nanosheet array and preparation method and application thereof |
| CN111276337A (en) * | 2019-12-13 | 2020-06-12 | 湖北大学 | Based on β -Ni (OH)2Manufacturing method of flexible solid-state supercapacitor |
| CN111943286A (en) * | 2020-08-18 | 2020-11-17 | 中国人民解放军空军预警学院雷达士官学校 | Nickel-nickel hydroxide composite film electrode and preparation method and application thereof |
| CN114558465A (en) * | 2020-11-27 | 2022-05-31 | 中国科学院大连化学物理研究所 | Preparation and application of porous nickel hydroxide ion screening membrane |
| CN114558465B (en) * | 2020-11-27 | 2022-11-15 | 中国科学院大连化学物理研究所 | Preparation and application of porous nickel hydroxide ion screening membrane |
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