CN104030371A - Method for synthesizing NiO microsphere consisting of mesoporous sheet structures by soft template process - Google Patents
Method for synthesizing NiO microsphere consisting of mesoporous sheet structures by soft template process Download PDFInfo
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- CN104030371A CN104030371A CN201410267424.4A CN201410267424A CN104030371A CN 104030371 A CN104030371 A CN 104030371A CN 201410267424 A CN201410267424 A CN 201410267424A CN 104030371 A CN104030371 A CN 104030371A
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Abstract
The invention relates to a method for synthesizing NiO microsphere consisting of mesoporous sheet structures by a soft template process. The method comprises the following specific steps of (1) preparing 0.34 mol/L liquor by using nickel nitrate hexahydrate NiNO3.6H2O, and then adding urea; and dissolving a segmented copolymer P123 in mixed liquor of alcohol and water, and stirring to prepare mixed liquor; (2), placing the mixed liquor obtained in the step (1) in a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 8-24 hours at 80-200 DEG C under a hydrothermal condition, and cooling to the room temperature; (3), centrifuging turbid liquor obtained in the step (2), respectively washing by water and alcohol, and then drying to obtain a nickel hydroxide precursor; and (4), roasting for the nickel hydroxide precursor for 2-4 hours at 300-600 DEG C to obtain the NiO microsphere consisting of mesoporous sheet structures. The method disclosed by the invention is simple in process, low in equipment requirement, easily available in materials, low in cost, and capable of carrying out mass production; the NiO microsphere is beneficial to developing performances and application of the NiO body.
Description
[technical field]
The present invention relates to the preparation field of inorganic nano material, particularly the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method.
[background technology]
Nano-nickel oxide (NiO) is a kind of important transition metal, is a kind of P-type semiconductor material.Due to the special electricity of nickel oxide, magnetics and catalysis characteristics, be widely used in fields such as capacitor material, magneticsubstance, catalystic material, sensor materials, become one of current worldwide study hotspot.Also because the special character of nano-nickel oxide relies on its pattern and size strongly, so the research of nano-nickel oxide, sign and the correlated performance of synthetic different-shape and structure is subject to investigator's extensive concern.Mesoporous material has just evoked countless scholars' strong interest from birth, the synthetic focus with being applied to current research of mesoporous material.The application of mesoporous material is limited to unordered mesoporous material more, but ordered mesoporous material has more advantage.Utilize the nano material with order mesoporous structure that synthesizes that block polymer P123 can be easy.
Nano-nickel oxide has been synthesized out different morphologies, as nano-powder, nano wire, nanotube, nanometer ball etc.Its preparation method mostly is vapor phase process, liquid phase method and solid phase method.According to the literature, Gui etc. (J.phys.Chem.C, 2007,111,5622-5627), by nickel chloride aqueous solution and the reaction of fat aqueous solution, have prepared and have been hexagonal NiO nanometer lamellar body.Feng etc. (J.Am.Chem.Soc.2008,130,5262-5266) have prepared NiO material bimodal distribution, order mesoporous taking KIT-6 as template.China Patent Publication No. is that CNI01269850A relates to a kind of preparation method who spends shape nickel oxide, prepare by hydrothermal method, taking vulkacit H, Nickelous nitrate hexahydrate and deionized water as raw material, be mixed with mixing solutions, after stirring, above-mentioned mixing solutions is placed in reactor, in 80-150 DEG C of baking oven, heats 4-20h.Through centrifugation, washing, oven dry and calcination process, obtain flower shape nickel oxide again.China Patent Publication No. is the preparation method of the controlled NiO nano flower-like microballoon of a kind of surface topography of relating to of CNI02126762A, prepare by solvent-thermal method, comprise the following steps: by surfactant dissolves in ethylene glycol, nickelous nitrate and phenylformic acid are dissolved in respectively as in above-mentioned solution, adding afterwards concentration is that the NaOH solution of 2mol/L is positioned over above-mentioned mixing solutions in reactor, at 160-220 DEG C, react 8-14h, then obtain the flower-shaped microballoon of product nano NiO through centrifugal, dry and calcination processing.
The preparation method of the nano-nickel oxide providing in above-mentioned document, condition harshness, consuming time long, undesirable without meso-hole structure or meso-hole structure.Therefore,, from the viewpoint of controlling of production process and energy-conserving and environment-protective, need the preparation method who seeks a kind of easy synthesis of nano meso-hole structure NiO badly.
[summary of the invention]
The object of the invention is to overcome the deficiencies in the prior art, the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method is provided; To be directed to the mesoporous NiO microballoon process complexity of preparation, the undesirable difficult problem of meso-hole structure, provide the preparation method of the NiO microballoon of the simple order mesoporous structure nano sheet composition of a kind of technique.Prepare high dispersive, there is the NiO microballoon that mesoporous sheet structure forms.
The object of the invention is to be achieved through the following technical solutions:
A method for the NiO microballoon of the synthesising mesoporous sheet structure composition of soft template method, its concrete steps are:
(1) get Nickelous nitrate hexahydrate NiNO
36H
2o is configured to the solution of 0.34mol/L, then adds urea; Get in the mixing solutions that segmented copolymer P123 is dissolved in ethanol and water, and stir, make mixing solutions;
Segmented copolymer P123 is specially PEO20-PPO70-PEO20, and Chinese is: polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer;
NiNO
36H
2the proportioning of O and urea is 1mmol: 1～2mmol;
NiNO
36H
2the proportioning of O and P123 is 1mmol: 0.3～0.4g;
(2) mixing solutions step (1) being obtained is positioned in teflon-lined stainless steel cauldron, under 80～200 DEG C of hydrothermal conditions, reacts 8～24h, is cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, water and ethanol wash respectively, then dry, both nickel hydroxide presoma;
(4), by nickel hydroxide presoma roasting 2～4h under 300～600 DEG C of conditions, obtain the NiO microballoon of mesoporous sheet structure composition.
The diameter of the NiO microballoon of described mesoporous sheet structure composition is 1.2～1.8 μ m, and the nanometer sheet thickness of this meso-hole structure is about 60nm, and in this nanometer sheet, is evenly distributed with the hole that diameter is 20～25nm, and NiO becomes Emission in Cubic, and degree of crystallinity is high.
Compared with prior art, positively effect of the present invention is:
(1) micro-nano structure that the NiO microballoon of prepared meso-porous nano sheet composition is made up of mesoporous nanometer sheet.
(2) the NiO microballoon purity of prepared mesoporous shape nanometer sheet composition is high, does not contain the NiO of other pattern.
(3) the NiO microballoon stable performance of prepared lotus-like nanometer sheet composition, volatility not in air.
(4) segmented copolymer P123 in building-up process as structure directing agent, also as pore-creating agent.
(5) technique is simple, low for equipment requirements, and starting material are easy to get, and expense is cheap, can produce in enormous quantities.
(6) the NiO microballoon of the mesoporous sheet structure composition that prepared by the present invention is conducive to open up performance and the application that NiO itself is unique.
[accompanying drawing and explanation thereof]
Fig. 1 is the preparation flow figure of the NiO microballoon of mesoporous sheet structure composition.
Fig. 2 is the X-ray diffraction spectrogram of NiO microballoon in the time that differing temps is calcined that adopts mesoporous sheet structure composition prepared by present method.
Fig. 3 is the stereoscan photograph of the NiO microballoon of the mesoporous sheet structure composition of embodiment 1.
Fig. 4 is the stereoscan photograph of the NiO microballoon of the mesoporous sheet structure composition of embodiment 2.
Fig. 5-1 is the stereoscan photograph of the NiO microballoon of the mesoporous sheet structure composition of embodiment 3.
Fig. 5-2 are the transmission electron microscope photo of the NiO microballoon of the mesoporous sheet structure composition of embodiment 3.
[embodiment]
The embodiment of the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method of the present invention is below provided.
Embodiment 1
(1) 2.4g Nickelous nitrate hexahydrate is dissolved in the water of 25mL and adds again 0.5g urea; 2.5g P123 is added in the ethanol of 25mL, ultrasonic, stirring is fully dissolved it; Mix above-mentioned two kinds of solution;
(2) mixing solutions in step (1) is positioned in teflon-lined stainless steel cauldron, after sealing, under the condition of 120 DEG C, reacts 24h, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, water and ethanol wash respectively, then dry, both nickel hydroxide presoma;
(4), by nickel hydroxide presoma roasting 2h under 500 DEG C of conditions, obtain the NiO microballoon of mesoporous sheet structure composition.
Embodiment 2
(1) 2.4g Nickelous nitrate hexahydrate is dissolved in the water of 25mL and adds again 0.5g urea; 2.5g P123 is added in the ethanol of 25mL, ultrasonic, stirring is fully dissolved it; Mix above-mentioned two kinds of solution;
(2) mixing solutions in step (1) is positioned in teflon-lined stainless steel cauldron, after sealing, under the condition of 180 DEG C, reacts 6h, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, water and ethanol wash respectively, then dry, both nickel hydroxide presoma;
(4), by nickel hydroxide presoma roasting 2h under 300 DEG C of conditions, obtain the NiO microballoon of mesoporous sheet structure composition.
Embodiment 3
(1) 2.9g Nickelous nitrate hexahydrate is dissolved in the water of 29mL and adds again 0.6g urea; 2.9g P123 is added in the ethanol of 29mL, ultrasonic, stirring is fully dissolved it; Mix above-mentioned two kinds of solution;
(2) mixing solutions in step (1) is positioned in teflon-lined stainless steel cauldron, after sealing, under the condition of 180 DEG C, reacts 24h, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, water and ethanol wash respectively, then dry, both nickel hydroxide presoma;
(4), by nickel hydroxide presoma roasting 2h under 600 DEG C of conditions, obtain the NiO microballoon of mesoporous sheet structure composition.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (6)
1. a method for the NiO microballoon of the synthesising mesoporous sheet structure composition of soft template method, is characterized in that, its concrete steps are:
(1) get Nickelous nitrate hexahydrate NiNO
36H
2o is configured to the solution of 0.34mol/L, then adds urea; Get in the mixing solutions that segmented copolymer P123 is dissolved in ethanol and water, and stir, make mixing solutions;
(2) mixing solutions step (1) being obtained is positioned in teflon-lined stainless steel cauldron, under 80～200 DEG C of hydrothermal conditions, reacts 8～24h, is cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, water and ethanol wash respectively, then dry, both nickel hydroxide presoma;
(4), by nickel hydroxide presoma roasting 2～4h under 300～600 DEG C of conditions, obtain the NiO microballoon of mesoporous sheet structure composition.
2. the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method as claimed in claim 1, is characterized in that, in described step (1), and NiNO
36H
2the proportioning of O and urea is 1mmol: 1～2mmol.
3. the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method as claimed in claim 1, is characterized in that, in described step (1), and NiNO
36H
2the proportioning of O and P123 is 1mmol: 0.3～0.4g.
4. the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method as claimed in claim 1, is characterized in that, the diameter of the NiO microballoon of described mesoporous sheet structure composition is 1.2～1.8 μ m.
5. the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method as claimed in claim 1, is characterized in that, the nanometer sheet thickness of this described meso-hole structure is about 60nm, and in this nanometer sheet, is evenly distributed with the hole that diameter is 20～25nm.
6. the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method as claimed in claim 1, is characterized in that, described NiO becomes Emission in Cubic, and degree of crystallinity is high.
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Cited By (8)
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| CN105044175A (en) * | 2015-07-14 | 2015-11-11 | 湘潭大学 | Preparation method of electrochemical sensor based on carbon-nitrogen-doped nickel oxide microsphere |
| CN105174320A (en) * | 2015-10-15 | 2015-12-23 | 齐鲁工业大学 | Hexagonal flake-shaped mesoporous nickel oxide and preparation method and application thereof |
| CN105502519A (en) * | 2015-12-16 | 2016-04-20 | 安徽建筑大学 | Two-dimensional oversized mint-leaf-shaped nickel oxide nano material and preparation method thereof |
| CN105834446A (en) * | 2016-04-12 | 2016-08-10 | 同济大学 | Synthetic method for ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite |
| CN106248744A (en) * | 2016-07-15 | 2016-12-21 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of micro porous hollow nickel oxide gas-sensitive sensor device for formaldehyde selective absorption and preparation and application |
| CN108007998A (en) * | 2017-11-10 | 2018-05-08 | 东北电力大学 | Nickel oxide non-enzymatic glucose electrochemical sensor |
| CN111333127A (en) * | 2020-03-05 | 2020-06-26 | 西北工业大学 | Hierarchical porous honeycomb nickel oxide microsphere and preparation method thereof |
| CN114054042A (en) * | 2021-11-11 | 2022-02-18 | 重庆邮电大学 | Preparation method of Ag-doped nickel oxide nano-microsphere with mesopores and product thereof |
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| CN102385998A (en) * | 2011-12-08 | 2012-03-21 | 南开大学 | NiO electrode material with high specific capacitance and preparation method thereof |
| CN102757101A (en) * | 2012-02-22 | 2012-10-31 | 太原理工大学 | Method for preparing large-specific-surface-area porous nickel oxide microspheres |
| CN102824912A (en) * | 2012-09-05 | 2012-12-19 | 中国石油天然气集团公司 | High-specific surface area mesoporous nickel oxide hydrogenation catalyst and preparation method thereof |
| CN102887550A (en) * | 2012-10-09 | 2013-01-23 | 四川大学 | Method for producing mesoporous nickel oxide |
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| WO2009112046A1 (en) * | 2008-03-10 | 2009-09-17 | Jacobs University Bremen Gmbh | Nio nanosheet structure possessing the (111) crystallographic planes with hexagonal holes, method for preparing the same and uses thereof |
| CN102385998A (en) * | 2011-12-08 | 2012-03-21 | 南开大学 | NiO electrode material with high specific capacitance and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105044175A (en) * | 2015-07-14 | 2015-11-11 | 湘潭大学 | Preparation method of electrochemical sensor based on carbon-nitrogen-doped nickel oxide microsphere |
| CN105044175B (en) * | 2015-07-14 | 2018-01-23 | 湘潭大学 | A kind of preparation method for the electrochemical sensor that nickel oxide microballoon is mixed based on carbon nitrogen |
| CN105174320A (en) * | 2015-10-15 | 2015-12-23 | 齐鲁工业大学 | Hexagonal flake-shaped mesoporous nickel oxide and preparation method and application thereof |
| CN105174320B (en) * | 2015-10-15 | 2017-03-22 | 齐鲁工业大学 | Hexagonal flake-shaped mesoporous nickel oxide and preparation method and application thereof |
| CN105502519B (en) * | 2015-12-16 | 2017-03-22 | 安徽建筑大学 | Two-dimensional oversized mint-leaf-shaped nickel oxide nano material and preparation method thereof |
| CN105502519A (en) * | 2015-12-16 | 2016-04-20 | 安徽建筑大学 | Two-dimensional oversized mint-leaf-shaped nickel oxide nano material and preparation method thereof |
| CN105834446A (en) * | 2016-04-12 | 2016-08-10 | 同济大学 | Synthetic method for ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite |
| CN106248744A (en) * | 2016-07-15 | 2016-12-21 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of micro porous hollow nickel oxide gas-sensitive sensor device for formaldehyde selective absorption and preparation and application |
| CN108007998A (en) * | 2017-11-10 | 2018-05-08 | 东北电力大学 | Nickel oxide non-enzymatic glucose electrochemical sensor |
| CN108007998B (en) * | 2017-11-10 | 2020-07-17 | 东北电力大学 | Nickel oxide non-enzymatic glucose electrochemical sensor |
| CN111333127A (en) * | 2020-03-05 | 2020-06-26 | 西北工业大学 | Hierarchical porous honeycomb nickel oxide microsphere and preparation method thereof |
| CN111333127B (en) * | 2020-03-05 | 2021-04-23 | 西北工业大学 | Hierarchical porous honeycomb nickel oxide microsphere and preparation method thereof |
| CN114054042A (en) * | 2021-11-11 | 2022-02-18 | 重庆邮电大学 | Preparation method of Ag-doped nickel oxide nano-microsphere with mesopores and product thereof |
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