CN104891580A - Preparation method of nickel hydroxide ultrathin nanosheet assemblies - Google Patents
Preparation method of nickel hydroxide ultrathin nanosheet assemblies Download PDFInfo
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- CN104891580A CN104891580A CN201510225312.7A CN201510225312A CN104891580A CN 104891580 A CN104891580 A CN 104891580A CN 201510225312 A CN201510225312 A CN 201510225312A CN 104891580 A CN104891580 A CN 104891580A
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Abstract
The invention discloses a preparation method of nickel hydroxide ultrathin nanosheet assemblies, which belongs to the technical field of inorganic function material preparation. The preparation method is characterized in that a precipitating agent is added in a soluble solution of nickel salt, and compound precipitation is obtained by controlling the reaction time and reaction parameter ratio. The nickel hydroxide ultrathin nanosheet assemblies can be prepared by steps of filtering, washing by water and drying. The preparation method has the advantages that 1)the rapid preparation method of Ni(OH)2 ultrathin nanosheet assemblies can be provided; 2) Ni(OH)2 ultrathin nanosheet assemblies prepared by the method can control the products morphology through an experiment parameter ratio; and 3)the provided method has the advantages of simple process, mild condition and short flow, and is suitable for industrial production.
Description
Technical field
The invention belongs to inorganic functional material preparing technical field, particularly a kind of preparation method of nickel hydroxide ultrathin nanometer sheet assembly.
Background technology
Low-dimension nano material because of its size little, percent by volume shared by surface atom is large, surfaceness increases, and forms rough atomic steps, improves the contact surface of chemical reaction, can catalytic efficiency be significantly improved as catalystic material, have broad prospects at catalytic field.People utilize solid phase method, liquid phase method and vapor phase process prepare and have modified various low-dimension nano material, in the fields such as the energy, environment, information, biology, show huge application prospect, have become one of research field enlivened the most in the world.
Ni (OH)
2be a kind of important inorganic non-noble metallic materials, its 3d track electron rich oxygen, has very strong adsorption, to a lot of reducing gas as H
2there is certain activation capacity with CO, and to the oxidation of these gases, there is good katalysis.The Ni (OH) of current multiple different-shape
2nano material is in the news, comprises porous nano microballoon, nano flower, nanometer sheet and nanofiber etc.CN102897852A describes a kind of preparation method of nickel hydroxide hierarchy microballoon of nanometer sheet packaging assembly, hierarchy is assembled by the spiral mode of being layering by flake nano unit, has good application prospect in fields such as battery electrode material, catalysis, air-sensitives.CN102826617A provides a kind of ultracapacitor ball-shape nickel hydroxide electrode materials and preparation method thereof, has good chemical property.
At present, about Ni (OH)
2the report of the research of the low-dimensional materials such as ultrathin nanometer sheet is less, and preparation method is comparatively harsh.Therefore, develop a kind of simplification, method that is rapid, gentlenessization prepares Ni (OH)
2ultrathin nanometer sheet, and prepare Ni (OH) by Control release parameter
2ultrathin nanometer sheet assembly and realize the challenge subjects that its Morphological control is still materials science field.
Summary of the invention
The present invention is without the need to adding any template, tensio-active agent, and by simple solvent-thermal process method, regulation and control synthesize the transition metal hydroxide nano material with flaky nanometer structure.The object of the invention is to propose a kind of simple for process, experiment flow is short, the preparation method of the nickel hydroxide ultrathin nanometer sheet assembly of mild condition.
Technical scheme of the present invention is: first in soluble nickel salt, add urea, after fully stirring, reacts 2-30h at a certain temperature, and through centrifugal, dry obtained nickel hydroxide ultrathin nanometer sheet assembly, concrete preparation process is:
Under normal temperature, compound concentration is the soluble nickel salt of 0.001-2.0mol/L, magnetic agitation 20-60min, add 0.0001-0.05mol urea under agitation, continue to stir 10-40min, again this mixed system is moved in reactor, temperature controlled at 60-280 DEG C of insulation 2-30h, filtration washing, then obtains Ni (OH) at 40-120 DEG C after dry 4-36h
2ultrathin nanometer sheet assembly.
Described soluble nickel salt comprises: one or more in the nitrate of nickel, vitriol, halogenide, phosphoric acid salt, organic carboxylate.
The solvent of described mixing solutions comprises: water, ethanol, ethylene glycol, glycerol, one or more in butantetraol.
The invention has the advantages that: 1) provide a kind of Ni (OH)
2the fast preparation method of ultrathin nanometer sheet assembly; 2) with Ni (OH) prepared by method provided by the invention
2ultrathin nanometer sheet assembly, can realize the control to product morphology by parameter ratio by experiment; 3) simple with method reaction process provided by the invention, mild condition, flow process are short, are applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the Ni (OH) that the invention process case 1 obtains
2the stereoscan photograph of ultrathin nanometer sheet assembly.
Fig. 2 is the Ni (OH) that the invention process case 2 obtains
2the stereoscan photograph of ultrathin nanometer sheet assembly.
Fig. 3 is the Ni (OH) that the invention process case 3 obtains
2the stereoscan photograph of ultrathin nanometer sheet assembly.
Embodiment
Below in conjunction with concrete embodiment, technical scheme of the present invention is described further.
Case study on implementation 1
The nickel nitrate solution that 15mL concentration is 0.06mol/L is prepared under normal temperature, wherein the volume ratio of water and ethylene glycol is 1:1, add the urea of 0.004mol under agitation, continue to stir 30min, then move into reactor, at 120 DEG C, be incubated 6h, after naturally cooling, centrifugal, washing, then obtains Ni (OH) at 60 DEG C after dry 12h
2ultrathin nanometer sheet assembly (flower-like structure), the scanned photograph of product as shown in Figure 1.
Case study on implementation 2
The nickel nitrate solution that 15mL concentration is 0.017mol/L is prepared under normal temperature, wherein the volume ratio of water and ethylene glycol is 1:1, add the urea of 0.001mol under agitation, continue to stir 30min, then move into reactor, at 120 DEG C, be incubated 5h, after naturally cooling, centrifugal, washing, then obtains Ni (OH) at 60 DEG C after dry 12h
2ultrathin nanometer sheet assembly (stacked structure), the scanned photograph of product as shown in Figure 2.
Case study on implementation 3
The nickel nitrate solution that 15mL concentration is 0.06mol/L is prepared under normal temperature, wherein the volume ratio of water and ethylene glycol is 1:9, add the urea of 0.004mol under agitation, continue to stir 30min, then move into reactor, at 120 DEG C, be incubated 5h, after naturally cooling, centrifugal, dry, then at 60 DEG C, obtain Ni (OH) after dry 12h
2ultrathin nanometer sheet assembly (ball-like structure), the scanned photograph of product as shown in Figure 3.
Claims (3)
1. the preparation method of a nickel hydroxide ultrathin nanometer sheet assembly, it is characterized in that first in soluble nickel salt, adding urea, after fully stirring, react 2-30h at a certain temperature, through centrifugal, dry obtained nickel hydroxide ultrathin nanometer sheet assembly, concrete preparation process is:
Under normal temperature, compound concentration is the soluble nickel salt of 0.001-2.0mol/L, magnetic agitation 20-60min, add 0.0001-0.05mol urea under agitation, continue to stir 10-40min, again this mixed system is moved in reactor, temperature controlled at 60-280 DEG C of insulation 2-30h, filtration washing, then obtains Ni (OH) at 40-120 DEG C after dry 4-36h
2ultrathin nanometer sheet assembly.
2. the preparation method of a kind of nickel hydroxide ultrathin nanometer sheet assembly as claimed in claim 1, is characterized in that described soluble nickel salt comprises: one or more in the nitrate of nickel, vitriol, halogenide, phosphoric acid salt, organic carboxylate.
3. the preparation method of a kind of nickel hydroxide ultrathin nanometer sheet assembly as claimed in claim 1, is characterized in that the solvent of described mixing solutions comprises: water, ethanol, ethylene glycol, glycerol, one or more in butantetraol.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105947995A (en) * | 2016-04-22 | 2016-09-21 | 国家纳米科学中心 | NiSe2 nanosheet with selenium enriched on surface, preparation method thereof, and application thereof |
CN106865628A (en) * | 2017-03-10 | 2017-06-20 | 长春理工大学 | One kind is used for room temperature H2S gas sensing materials nickel oxide and preparation method thereof |
CN107954483A (en) * | 2017-12-28 | 2018-04-24 | 济南大学 | A kind of class alpha-phase nickel hydroxide ultrathin nanometer piece and preparation method thereof |
CN110085434A (en) * | 2019-04-10 | 2019-08-02 | 南京航空航天大学 | Helical form Ni (OH)2Nanometer sheet/nitrogen-doped graphene/carbon pipe composite membrane preparation method and application |
CN113512737A (en) * | 2021-04-01 | 2021-10-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
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CN101618895A (en) * | 2008-07-04 | 2010-01-06 | 中国科学院福建物质结构研究所 | Multi-level structure alpha type nickel hydroxide prepared by microwave auxiliary and method thereof |
KR20120035331A (en) * | 2010-10-05 | 2012-04-16 | 한국원자력연구원 | A METHOD FOR PREPARING Α-METAL HYDROXIDE USING GAMMA RAY, AND α-METAL HYDROXIDE PREPARED THEREBY |
CN102826617A (en) * | 2012-09-21 | 2012-12-19 | 中国科学院过程工程研究所 | Spherical nickel hydroxide material and preparation method thereof |
CN104291386A (en) * | 2014-10-10 | 2015-01-21 | 九江学院 | Preparation method of two-dimensional nickel hydroxide ultrathin nano-film |
-
2015
- 2015-05-05 CN CN201510225312.7A patent/CN104891580A/en active Pending
Patent Citations (4)
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CN101618895A (en) * | 2008-07-04 | 2010-01-06 | 中国科学院福建物质结构研究所 | Multi-level structure alpha type nickel hydroxide prepared by microwave auxiliary and method thereof |
KR20120035331A (en) * | 2010-10-05 | 2012-04-16 | 한국원자력연구원 | A METHOD FOR PREPARING Α-METAL HYDROXIDE USING GAMMA RAY, AND α-METAL HYDROXIDE PREPARED THEREBY |
CN102826617A (en) * | 2012-09-21 | 2012-12-19 | 中国科学院过程工程研究所 | Spherical nickel hydroxide material and preparation method thereof |
CN104291386A (en) * | 2014-10-10 | 2015-01-21 | 九江学院 | Preparation method of two-dimensional nickel hydroxide ultrathin nano-film |
Non-Patent Citations (2)
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WENXIU HE ET AL.: "Hydrothermal synthesis and characterization of nano-petal nickel hydroxide", 《RARE METALS》, vol. 34, no. 9, 20 July 2013 (2013-07-20) * |
孙海峰等: "水热法合成纳米花瓣状β-Ni(OH)2", 《稀有金属》, vol. 34, no. 3, 31 May 2010 (2010-05-31) * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105947995A (en) * | 2016-04-22 | 2016-09-21 | 国家纳米科学中心 | NiSe2 nanosheet with selenium enriched on surface, preparation method thereof, and application thereof |
CN106865628A (en) * | 2017-03-10 | 2017-06-20 | 长春理工大学 | One kind is used for room temperature H2S gas sensing materials nickel oxide and preparation method thereof |
CN107954483A (en) * | 2017-12-28 | 2018-04-24 | 济南大学 | A kind of class alpha-phase nickel hydroxide ultrathin nanometer piece and preparation method thereof |
CN110085434A (en) * | 2019-04-10 | 2019-08-02 | 南京航空航天大学 | Helical form Ni (OH)2Nanometer sheet/nitrogen-doped graphene/carbon pipe composite membrane preparation method and application |
CN113512737A (en) * | 2021-04-01 | 2021-10-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
CN113512737B (en) * | 2021-04-01 | 2022-07-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
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