CN104030371B - The method of the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method - Google Patents
The method of the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method Download PDFInfo
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- CN104030371B CN104030371B CN201410267424.4A CN201410267424A CN104030371B CN 104030371 B CN104030371 B CN 104030371B CN 201410267424 A CN201410267424 A CN 201410267424A CN 104030371 B CN104030371 B CN 104030371B
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Abstract
The present invention relates to the method for the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method, concrete steps are: (1) gets Nickelous nitrate hexahydrate NiNO
36H
2o is configured to the solution of 0.34mol/L, then adds urea; Get segmented copolymer P123 to be dissolved in the mixing solutions of ethanol and water, and stir, obtained mixing solutions; (2) mixing solutions that step (1) obtains is positioned in teflon-lined stainless steel cauldron, under 80 ~ 200 DEG C of hydrothermal conditions, reacts 8 ~ 24h, be cooled to room temperature; (3) step (2) gained turbid solution is carried out centrifugal, wash respectively with water and ethanol, then dry, both obtained nickel hydroxide presoma; (4) by nickel hydroxide presoma roasting 2 ~ 4h under 300 ~ 600 DEG C of conditions, the NiO microballoon of mesoporous sheet structure composition is obtained.Present invention process is simple, and low for equipment requirements, starting material are easy to get, low cost, batch production, and NiO microballoon is beneficial to the performance and application of developing NiO itself.
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 electricity, magnetics and catalysis characteristics that nickel oxide is special, be widely used in fields such as capacitor material, magneticsubstance, catalystic material, sensor materials, become one of current worldwide study hotspot.Also because special its pattern of character strong depend-ence of nano-nickel oxide and size, so the research of the nano-nickel oxide of synthesis different-shape and structure, sign and correlated performance is subject to the extensive concern of investigator.Mesoporous material has just evoked the strong interest of countless scholar from being born, and the Synthesis and application of mesoporous material has become the focus of current research.The application of mesoporous material is limited to unordered mesoporous material more, but ordered mesoporous material has more advantage.What utilize that block polymer P123 can be easy synthesizes the nano material with ordered mesopore structure.
Nano-nickel oxide is 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 been prepared in hexagonal NiO nanometer lamellar body.Feng etc. (J.Am.Chem.Soc.2008,130,5262-5266) take KIT-6 as Template preparation bimodal distribution, order mesoporous NiO material.China Patent Publication No. is that CNI01269850A relates to a kind of preparation method spending shape nickel oxide, prepared by hydrothermal method, with vulkacit H, Nickelous nitrate hexahydrate and deionized water for 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.Again through centrifugation, washing, oven dry and calcination process, obtain flower shape nickel oxide.China Patent Publication No. is the preparation method relating to the controlled NiO nano flower-like microballoon of a kind of surface topography of CNI02126762A, prepared by solvent-thermal method, comprise the following steps: by surfactant dissolves in ethylene glycol, nickelous nitrate and phenylformic acid are dissolved in respectively in above-mentioned solution, adding concentration is afterwards that above-mentioned mixing solutions is positioned in reactor by the NaOH solution of 2mol/L, at 160-220 DEG C, react 8-14h, then obtain product nano NiO flower-like microsphere through centrifugal, dry and calcination process.
The preparation method of the nano-nickel oxide provided in above-mentioned document, condition is harsh, consuming time longer, without meso-hole structure or meso-hole structure undesirable.Therefore, from the viewpoint of controlling of production process and energy-conserving and environment-protective, need the preparation method seeking 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 difficult problem that the mesoporous NiO microballoon process of preparation is complicated, meso-hole structure is undesirable, provide the preparation method of the NiO microballoon of the simple ordered mesopore structure nanometer sheet composition of a kind of technique.Prepare high dispersive, there is the NiO microballoon of mesoporous sheet structure composition.
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) Nickelous nitrate hexahydrate NiNO is got
36H
2o is configured to the solution of 0.34mol/L, then adds urea; Get segmented copolymer P123 to be dissolved in the mixing solutions of ethanol and water, and stir, obtained 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 that step (1) obtains is positioned in teflon-lined stainless steel cauldron, under 80 ~ 200 DEG C of hydrothermal conditions, reacts 8 ~ 24h, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, wash respectively with water and ethanol, then dry, both obtained nickel hydroxide presoma;
(4) by nickel hydroxide presoma roasting 2 ~ 4h under 300 ~ 600 DEG C of conditions, the NiO microballoon of mesoporous sheet structure composition is obtained.
The diameter of the NiO microballoon of described mesoporous sheet structure composition is 1.2 ~ 1.8 μm, and the nanometer sheet thickness of this meso-hole structure is about 60nm, and in this nanometer sheet, be 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 that the meso-porous nano sheet obtained by forms is made up of mesoporous nanometer sheet.
(2) the NiO microballoon purity of the mesoporous shape nanometer sheet composition obtained by is high, the NiO not containing other pattern.
(3) the NiO microballoon stable performance of the lotus-like nanometer sheet composition obtained by, in atmosphere not volatility.
(4) segmented copolymer P123 in building-up process namely as structure directing agent, also as pore-creating agent.
(5) technique is simple, and low for equipment requirements, starting material are easy to get, low cost, can produce in enormous quantities.
(6) the NiO microballoon that the mesoporous sheet structure that prepared by the present invention forms is conducive to opening up the unique performance and application of NiO itself.
[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 when differing temps is calcined of the mesoporous sheet structure composition adopting present method to prepare.
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 is 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 0.5g urea again; Added by 2.5gP123 in the ethanol of 25mL, ultrasonic, stirring makes it fully dissolve; Mix above-mentioned two kinds of solution;
(2) mixing solutions in step (1) is positioned in teflon-lined stainless steel cauldron, under the condition of 120 DEG C, reacts 24h after sealing, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, wash respectively with water and ethanol, then dry, both obtained nickel hydroxide presoma;
(4) by nickel hydroxide presoma roasting 2h under 500 DEG C of conditions, the NiO microballoon of mesoporous sheet structure composition is obtained.
Embodiment 2
(1) 2.4g Nickelous nitrate hexahydrate is dissolved in the water of 25mL and adds 0.5g urea again; Added by 2.5gP123 in the ethanol of 25mL, ultrasonic, stirring makes it fully dissolve; Mix above-mentioned two kinds of solution;
(2) mixing solutions in step (1) is positioned in teflon-lined stainless steel cauldron, under the condition of 180 DEG C, reacts 6h after sealing, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, wash respectively with water and ethanol, then dry, both obtained nickel hydroxide presoma;
(4) by nickel hydroxide presoma roasting 2h under 300 DEG C of conditions, the NiO microballoon of mesoporous sheet structure composition is obtained.
Embodiment 3
(1) 2.9g Nickelous nitrate hexahydrate is dissolved in the water of 29mL and adds 0.6g urea again; Added by 2.9gP123 in the ethanol of 29mL, ultrasonic, stirring makes it fully dissolve; Mix above-mentioned two kinds of solution;
(2) mixing solutions in step (1) is positioned in teflon-lined stainless steel cauldron, under the condition of 180 DEG C, reacts 24h after sealing, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, wash respectively with water and ethanol, then dry, both obtained nickel hydroxide presoma;
(4) by nickel hydroxide presoma roasting 2h under 600 DEG C of conditions, the NiO microballoon of mesoporous sheet structure composition is obtained.
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 (5)
1. a method for the NiO microballoon of the synthesising mesoporous sheet structure composition of soft template method, it is characterized in that, its concrete steps are:
(1) Nickelous nitrate hexahydrate Ni (NO is got
3)
26H
2o is configured to the solution of 0.34mol/L, then adds urea; Get segmented copolymer P123 to be dissolved in the mixing solutions of ethanol and water, and stir, obtained mixing solutions;
(2) mixing solutions that step (1) obtains is positioned in teflon-lined stainless steel cauldron, under 80 ~ 200 DEG C of hydrothermal conditions, reacts 8 ~ 24h, be cooled to room temperature;
(3) step (2) gained turbid solution is carried out centrifugal, wash respectively with water and ethanol, then dry, both obtained nickel hydroxide presoma;
(4) by nickel hydroxide presoma roasting 2 ~ 4h under 300 ~ 600 DEG C of conditions, the NiO microballoon of mesoporous sheet structure composition is obtained;
The diameter of the NiO microballoon of described mesoporous sheet structure composition is 1.2 ~ 1.8 μm.
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 Ni (NO
3)
26H
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 Ni (NO
3)
26H
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, it is characterized in that, the nanometer sheet thickness of this described meso-hole structure is about 60nm, and in this nanometer sheet, be evenly distributed with the hole that diameter is 20 ~ 25nm.
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, it is characterized in that, described NiO becomes Emission in Cubic, and degree of crystallinity is high.
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| 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 |
| 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 |
| CN105834446B (en) * | 2016-04-12 | 2017-12-26 | 同济大学 | A kind of synthetic method of ultra-thin stratiform NiO CoOx nanometer sheets load NiCo nano compositions |
| 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 |
| CN108007998B (en) * | 2017-11-10 | 2020-07-17 | 东北电力大学 | Nickel oxide non-enzymatic glucose electrochemical sensor |
| 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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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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