CN103193280B - Based on the method that double-template prepares nickel oxide nano-crystal combination electrode material - Google Patents
Based on the method that double-template prepares nickel oxide nano-crystal combination electrode material Download PDFInfo
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- CN103193280B CN103193280B CN201310149598.6A CN201310149598A CN103193280B CN 103193280 B CN103193280 B CN 103193280B CN 201310149598 A CN201310149598 A CN 201310149598A CN 103193280 B CN103193280 B CN 103193280B
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Abstract
The present invention is to provide the method for preparing nickel oxide nano-crystal combination electrode material based on double-template, 1 3g glucose is dissolved in a certain amount of distilled water, absolute ethyl alcohol and multi-walled carbon nano-tubes is added after ultrasonic dissolution, ultrasonic 10min, mixed solution is placed in 50mL polytetrafluoro liner, naturally cools to room temperature after hydro-thermal reaction.Centrifugation product, dries after distillation water washing, that is, obtains double-template.A certain amount of double-template is dissolved in the ethanol solution of nickel salt, centrifugation after ultrasound, dries after using distilled water and absolute ethanol washing respectively.By products therefrom, in air atmosphere, roasting obtains product.The technical characteristic of the present invention is to adsorb Ni using glucose in nanotube surface carbonization2+, preparing that monodispersed NiO is nanocrystalline, the preparation of the double-template of glucose carbonization in the preparation process of whole material is crucial, the generation of nickel oxide precursor does not need precipitating reagent and surfactant, environment is friendly, and chemical property is good, has preferable application prospect and actual application value.
Description
Technical field
The invention belongs to the method for preparing nickel oxide nano-crystal combination electrode material based on double-template.
Background technology
Transition metal oxide nano is brilliant in electrochemistry, is catalyzed, has a wide range of applications in terms of gas sensing property and energy conversion,
Become the focus of current research.Conventional method can synthesize the porous monocrystalline metal oxide of nano-scale range, and Su etc. is in table
The graded structure being prepared for being assembled by nano particle under the activating agent auxiliary of face is nanocrystalline, the side that Cheah etc. is evaporated using molten drop
Method assembles gold nanocrystals, and is scattered in the template of specific morphology.But the high-ratio surface energy due to nano crystal material, holds
The problems such as easily causing particle agglomeration and irregular pattern, greatly limit its application in each field.In this regard, in the urgent need to exploitation
A kind of single dispersing, the preparation method of the controlled metallic oxide nanocrystal of pattern unification.
The invention provides a kind of be based on CNT（MWCNTs）Transition gold is prepared with glucose carburization zone for bimodulus version
The method of category oxide nanocrystalline, solves transition metal oxide and is difficult to the difficulty that same carbon nano tube surface functional group combines
Topic, reduces crystal particle diameter size, and the crystal of raising is dispersed, meanwhile, CNT has good charge conductibility, can be significantly
Improve the capacitive property of electrode.The method is simple, energy-conservation, and environmental protection need not add in the preparation process of whole composite
Plus any surfactant and precipitating reagent, this is provided with application for the brilliant industrialized production of transition metal oxide nano can
Energy.（Yang, P. D.; Zhao, D. Y.; Margolese, D. I.; Chmelka, B. F.;Stucky, G. D.
Nature 1998, 396, 152. Ba, J.H.; Polleux, J.;Antonietti,M.;Niederberger,
M.Adv.Mater.2005, 17, 2509. Yang, X. Y.; Li, Y.; Tendeloo, G. V.; Xiao, F.
S.; Su, B. L. Adv. Mater. 2009, 21, 1368. Lou, X. W.; Archer, L. A.; Yang, Z.
C. Adv. Mater. 2008, 20, 3971.）.
Content of the invention
The purpose of the present invention is to prepare monodispersed transition metal oxide/carbon electrode composite.
Technical scheme is as follows：
1-3g glucose is dissolved in 10-20mL distilled water in conical flask, add after ultrasonic dissolution 4-7mL absolute ethyl alcohol and
30-40mg multi-walled carbon nano-tubes, ultrasonic 10min, mixed solution are placed in 50mL polytetrafluoro liner, 170-210 DEG C of hydro-thermal reaction
4-8h, naturally cools to room temperature after reaction.
Centrifugation product, dries after distillation water washing, that is, obtains double-template.
40-80mg double-template is dissolved in the ethanol solution of nickel salt, centrifugation after ultrasound, respectively with distilled water and anhydrous
After ethanol washs three times, 80 DEG C dry 12h.
By products therefrom, roasting obtains product under the conditions of 300-600 DEG C.
Description of the drawings：
The TEM photo of the MWCNTs after Fig. 1 glucose carbon-coating cladding.
The TEM photo of Fig. 2 MWCNTs@NiO nano composite material.
Specific embodiment：
Technical scheme and effect are further described with reference to embodiment.But, used is concrete
Method, formula and explanation are not limitation of the present invention.
Embodiment 1：
1.687g glucose is dissolved in 11.2mL distilled water in conical flask, after ultrasonic dissolution, 5.6mL absolute ethyl alcohol is added,
With 33.8mg multi-walled carbon nano-tubes, ultrasonic 10min, mixed solution be placed in 50mL polytetrafluoro liner, 190 DEG C of hydro-thermal reactions 6h,
Room temperature is naturally cooled to after reaction.Centrifugation product, after distilled water washes four times, 80 DEG C dry 12h, that is, obtain double-template.
60mg double-template is dissolved in 20mL 0.2mol L-1Nickel nitrate（Ni(NO)3·6H2O）In ethanol solution, centrifugation point after ultrasound
From respectively with after distilled water and absolute ethanol washing three times, 80 DEG C dry 12h.By products therefrom under the conditions of 300-600 DEG C
Roasting obtains product.
Embodiment 2：
The glucose for being added is 1-3g, and the temperature and time of hydro-thermal reaction is respectively 170-210 DEG C and 4-8h, obtained
Glucose carbonization template layer thickness be 10-40nm.
Embodiment 3：
Nickel nitrate in embodiment 1 is changed to other nickel salts for being dissolved in ethanol, its addition is 0.002-0.006mol, its
Its experiment condition with embodiment 1, can also obtain monodispersed NiO nanocrystalline/charcoal combination electrode material.
Embodiment 4：
Dried powder is heated to 300-600 DEG C with the heating rate of 5-10 DEG C/min, and under air conditionses, roasting 3 is little
When.
Claims (4)
1. the method for nickel oxide nano-crystal combination electrode material being prepared based on double-template, it is characterised in that preparation process is as follows：Will
1-3g glucose is dissolved in 10-20mL distilled water in conical flask, adds a certain amount of absolute ethyl alcohol and many walls carbon after ultrasonic dissolution
Nanotube, ultrasonic 10min, mixed solution are placed in 50mL polytetrafluoro liner, 170-210 DEG C of hydro-thermal reaction 4-8h, after reaction certainly
Room temperature be so cooled to, centrifugation product, dry after distillation water washing, that is, double-template is obtained, 40-80mg double-template is dissolved in nickel
In the ethanol solution of salt, centrifugation after ultrasound, respectively with after distilled water and absolute ethanol washing three times, 80 DEG C dry 12h, will
Products therefrom roasting under the conditions of 300-600 DEG C obtains product.
2. the method for preparing nickel oxide nano-crystal combination electrode material based on double-template according to claim 1, is characterized in that
The glucose for being added is 1-3g, and the temperature and time of hydro-thermal reaction is respectively 170-210 DEG C and 4-8h, obtained glucose
The thickness of carbonization template layer is 10-40nm.
3. the method for preparing nickel oxide nano-crystal combination electrode material based on double-template according to claim 1, is characterized in that
Nickel salt is dissolved in the nickel salt of ethanol for nickel nitrate, nickel sulfate and nickel chloride, and its addition is 0.002-0.006mol.
4. the method for according to claim 1 nickel oxide nano-crystal combination electrode material being prepared based on double-template, dried
Powder is heated to 300-600 DEG C with the heating rate of 5-10 DEG C/min, roasting 3 hours under air conditionses.
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| CN103193280B true CN103193280B (en) | 2017-03-08 |
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| CN106442689B (en) * | 2016-09-29 | 2018-03-02 | 青岛大学 | The preparation and application of Dopamine Sensor based on nickel oxide CNT |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101455975A (en) * | 2007-12-14 | 2009-06-17 | 北京化工大学 | Porous carbon nanometer fiber-supported nanocrystal catalyst and preparation method thereof |
| TW201107236A (en) * | 2009-08-26 | 2011-03-01 | Guo Chun Ying | Carbon nanotube composite material and manufacturing method thereof |
| CN102992411A (en) * | 2012-09-25 | 2013-03-27 | 安徽建筑工业学院 | Hollow silkworm cocoon-shaped porous nickel oxide nano material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101455975A (en) * | 2007-12-14 | 2009-06-17 | 北京化工大学 | Porous carbon nanometer fiber-supported nanocrystal catalyst and preparation method thereof |
| TW201107236A (en) * | 2009-08-26 | 2011-03-01 | Guo Chun Ying | Carbon nanotube composite material and manufacturing method thereof |
| CN102992411A (en) * | 2012-09-25 | 2013-03-27 | 安徽建筑工业学院 | Hollow silkworm cocoon-shaped porous nickel oxide nano material and preparation method thereof |
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