CN103342396A - Method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material - Google Patents
Method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material Download PDFInfo
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Abstract
The invention discloses a method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material. The method comprises the following steps of: respectively dissolving soluble nickel salt and alkali reagent in hydrophilic reagent, after dissolving completely, jointly adding the solution into a reaction vessel according to that the molar ratio of monovalent nickel ions to hydroxyl ions in the mixed solution is 1: (1-8), stirring, condensing and reflowing under the condition of microwave stimulated heating, naturally cooling to room temperature, and then performing centrifugal separation; then, washing several times with deionized water and absolute ethyl alcohol, placing the material in a vacuum drying chamber, then, obtaining the two-dimensional nickel hydroxide nano material. The microwave liquid-phase synthesis method used in the invention is combined with the advantages of microwave rapid and even heating and liquid-phase synthesis, and is short in reaction period and high in reaction yield, the product prepared by the method is high in purity and free of other impurities. The method provided by the invention has the advantages of controllable preparation, large-volume synthesis and so on, and is suitable for industrial production and large-scale application.
Description
Technical field
The present invention relates to the method for the synthetic class Graphene two dimension of a kind of microwave liquid phase nickel hydroxide nano material, belong to class Graphene ultra-thin two-dimension nano material preparation technical field.
Background technology
The new important research field of nano material science and technology has been opened in the appearance of Graphene, to two dimension (2D) epoch, two scientist Andre K.Geim of Britain graceful Chester university and Konstantin S.Novoselov are also because being awarded Nobel Prize in physics in 2010 in the outstanding contributions of making aspect the Graphene preparation characterization low-dimension nano material scientific research band.As typical 2D nano structural material, Graphene has shown novel physics-chem characteristic, especially high specific surface area and surperficial carrier mobility, making it has unique application in fields such as electronics, photonics, spintronicss, in short several years just successful Application to LED display, support of the catalyst, novel energy store with converting apparatus on.The huge scientific research that Graphene shows and using value have caused that also the investigator has the concern of the 2D nano structural material of high surface atom ratio to other types, is mainly class graphene inorganic 2D nano structural material.The class Graphene 2D stratified material of extensively being paid close attention at present mainly contains transition metal chalcogenide, transition metal oxide, metal hydroxides etc.Because huge specific surface area and ultra-thin microtexture, these 2D nano structural materials have shown special surface tissue and characteristic electron, have excellent mechanics, electricity and optical property, be presented as ultra-thin, transparent and high-flexibility on the macroscopic view, can be widely used in fields such as opto-electronic device, biochemical sensor, catalyzer, ultracapacitor, lithium ion battery, fuel cell and solar cell, especially in the photoelectrochemistry reaction field that highly depends on the bill of material interface performance, the 2D material has shown superior performance especially.Yet the performance of these a series of innovations of 2D nano structural material and application but depend on the controlled scale preparation of material.The special performance of 2D nano structural material depends on its thickness and area, thereby designs the forward position research topic that synthetic new 2D nano material is considered to modern chemistry and Materials science by the regulation and control of nanoscale and appearance structure.In addition, 2D nickel hydroxide nano structured material has caused many scientific workers' interest, regulation and control under the material microscale are synthetic has done number of research projects, and has realized that it is in important potential application in aspect such as gas sensor, catalysis, lithium ion battery, ultracapacitor, fuel cell and Ni-based alkali formula batteries.
Preparing at present the extensive method that adopts of 2D nano structural material is chemical stripping, chemical gas phase heavy (CVD) and molecular beam epitaxial growth (MBE) etc.Though chemical stripping method output is big, have uncontrollable shortcoming, prepared 2D nano material size and the pattern that comes out is inhomogeneous, and especially thickness and area are not of uniform size.Though and chemical vapour deposition can be prepared high-quality 2D nano material, its output is lower, and highly depends on growing substrate, and cost is higher, is not suitable for industrial applications.Comparatively speaking, liquid phase method is the method for more promising synthetic 2D nano material, and the building-up process simple controllable is fit to industrialized developing and uses.
Based on advanced microwave heating liquid-phase synthesis process, be used to synthetic various nano materials in recent years.Analogy cutting edge of a knife or a sword etc. discloses a kind of method (Chinese patent publication number CNIO1864314A) of synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase, prepared product even particle size.Compare with traditional liquid-phase synthesis process, the microwave liquid phase synthesizing method is a kind of material synthesis method of simple, environmental protection, can shorten the reaction times greatly, the compound that the selectivity heating has different microwave absorbing characteristics, homogeneous heating, the combined coefficient height is fit to mass preparation.While did not appear in the newspapers up to now and utilized the method for the synthetic ultra-thin 2D nickel hydroxide nano of the class Graphene material of microwave liquid phase according to the knowledge of the applicant.
Summary of the invention
The objective of the invention is that can't to satisfy output simultaneously big in order to solve prior art, and the problem of controllable product quality, the method for the synthetic class Graphene two dimension of a kind of microwave liquid phase nickel hydroxide nano material is provided.
The objective of the invention is to be achieved through the following technical solutions.
The method of the synthetic class Graphene two dimension of a kind of microwave liquid phase of the present invention nickel hydroxide nano material, concrete steps are as follows:
Step 3, the resulting nano material of step 2 successively used deionized water and absolute ethanol washing after, just obtain two-dimentional nickel hydroxide nano material after putting into the vacuum drying oven drying.
Described nickel salt raw material is: nickelous nitrate, nickelous acetate, nickelous chloride, single nickel salt, nickelous oxalate, the mixing salt of one or more in the nickel hydroxide;
Described alkaline reagents is: potassium hydroxide, sodium hydroxide, ammoniacal liquor, urea, the mixed base of one or more in the quadrol;
Described hydrophilic solvent is: deionized water, ethanol, ethylene glycol, glycerol, isopropylcarbinol, acetone, benzene, vinylbenzene, the mixing solutions of one or more in the acetonitrile.
Beneficial effect
1, the method for the synthetic class Graphene two dimension of a kind of microwave liquid phase of the present invention nickel hydroxide nano material, its microtexture shape characteristic is ultra-thin, big area, single sheet of disperseing, can reach 1nm when thickness is the thinnest, length and width are several microns, can be used for preparing metal-hydrogen nickel alkaline cell, electrode of super capacitor active material and catalyzer etc.
2, the method for the synthetic class Graphene two dimension of a kind of microwave liquid phase of the present invention nickel hydroxide nano material, simple to operate, with low cost, the reaction conditions gentleness, entire reaction course is carried out under normal pressure, and temperature of reaction is between 80~170 ℃, and the reaction times is 0.5~180 minute, product size and pattern are even, good dispersity.
3, the method for the synthetic class Graphene two dimension of a kind of microwave liquid phase of the present invention nickel hydroxide nano material, the microwave liquid-phase synthesis process that adopts combines microwave rapid and uniform heating and the synthetic advantage of liquid phase, reaction time is short, the reaction yield height, and the heating of the selectivity of microwave is beneficial to the generation that suppresses side reaction, therefore resulting product purity height does not have other impurity.Compare with the chemical stripping that generally the adopts method that vapour deposition prepares ultra-thin class Graphene two-dimensional nano material with high temperature, designed method of the present invention has controlled preparation, a large amount of advantage such as synthetic, is fit to suitability for industrialized production and mass-producing and uses.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of the prepared two-dimentional nickel hydroxide nano material of explanation case study on implementation 1;
Fig. 2 is the scanning electron microscope diagram of the prepared two-dimentional nickel hydroxide nano material of explanation case study on implementation 1;
Fig. 3 is the transmission electron microscope figure of the prepared two-dimentional nickel hydroxide nano material of explanation case study on implementation 1;
Fig. 4 is the high-resolution-ration transmission electric-lens figure of the prepared two-dimentional nickel hydroxide nano material of explanation case study on implementation 2;
Fig. 5 is the specific surface area test pattern of the prepared two-dimentional nickel hydroxide nano material of explanation case study on implementation 3;
Fig. 6 can spectrogram for the prepared two-dimentional nickel hydroxide nano material of explanation case study on implementation 4;
Fig. 7 is the scanning electron microscope diagram of the prepared two-dimentional nickel hydroxide nano material of explanation case study on implementation 8.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing and embodiment.
(1) nickelous nitrate and sodium hydroxide are dissolved in respectively in the deionized water, the concentration of nickelous nitrate is 0.05mol/L, and concentration sodium hydroxide is 0.1mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be 1:4 by the mol ratio of mixing back monovalence nickel ion and hydroxide ion, the solution of getting the above-mentioned nickelous nitrate for preparing and sodium hydroxide respectively joins to mix in the reaction vessel and stirred 30 minutes, be condensing reflux 60 minutes under the microwave-excitation heating condition of 700W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 100 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 12 hours.
Fig. 1 is the X ray diffracting spectrum of two-dimentional nickel hydroxide nano material, and prepared material is the pure α nickel hydroxide of six side's laminate structures mutually, does not have other to exist as β phase or other impurity mutually, and the material well-crystallized.Fig. 2 is the scanning electron microscope diagram sheet of two-dimentional nickel hydroxide nano material, and prepared scantling and pattern are even, are nano-sheet, favorable dispersity.Fig. 3 is the transmission electron micrograph of two-dimentional nickel hydroxide nano material, and prepared material is transparent superthin structure, is similar to Graphene, and its thickness is about 1nm.
(1) nickelous nitrate and potassium hydroxide are dissolved in respectively in the deionized water, the concentration of nickelous nitrate is 0.10mol/L, and the concentration of potassium hydroxide is 0.10mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be 1:1 by the mol ratio of mixing back monovalence nickel ion and hydroxide ion, the solution of getting the above-mentioned nickelous nitrate for preparing and potassium hydroxide respectively joins to mix in the reaction vessel and stirred 30 minutes, be condensing reflux 60 minutes under the microwave-excitation heating condition of 700W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 100 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 12 hours.
Fig. 4 is the high resolution transmission electron microscopy picture of two-dimentional nickel hydroxide nano material, and prepared material is typical class Graphene stratiform structure, and evenly is individual layer, and its thickness is about 1.7nm.
Embodiment 3
(1) nickelous chloride and potassium hydroxide are dissolved in respectively in the deionized water, the concentration of nickelous chloride is 0.20mol/L, and the concentration of potassium hydroxide is 0.80mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be that solution that 1:8 gets the above-mentioned nickelous chloride for preparing and potassium hydroxide respectively joins and mixes stirring 30 minutes in the reaction vessel by mixing back monovalence nickel ion and the mol ratio of hydroxide ion, be condensing reflux 60 minutes under the microwave-excitation heating condition of 700W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 110 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 12 hours.
Fig. 5 is the specific surface area test pattern of two-dimentional nickel hydroxide nano material, because prepared nickel hydroxide is class Graphene two dimension ultrathin nanometer material, has very high specific surface area, and test result shows that its specific surface area is up to 190.15m
2/ g.
Embodiment 4
(1) single nickel salt and urea are dissolved in respectively in deionized water and the ethylene glycol, the concentration of single nickel salt is 0.10mol/L, and the concentration of urea is 0.80mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be that solution that 1:4 gets the above-mentioned single nickel salt for preparing and urea respectively joins and mixes stirring 30 minutes in the reaction vessel by mixing back monovalence nickel ion and the mol ratio of hydroxide ion, be condensing reflux 30 minutes under the microwave-excitation heating condition of 900W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 80 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 12 hours.
Fig. 6 is the energy spectrogram of two-dimentional nickel hydroxide nano material, except the Si and C element that come from test base, only detects Ni and O element, does not have other impurity elements and occurs, and illustrates that prepared nickel hydroxide purity is higher.
Embodiment 5
(1) nickel acetate and ammoniacal liquor are dissolved in respectively in the deionized water, the concentration of nickel acetate is 0.25mol/L, and the concentration of ammoniacal liquor is 1.00mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be that solution that 1:3 gets the above-mentioned nickel acetate for preparing and ammoniacal liquor respectively joins and mixes stirring 30 minutes in the reaction vessel by mixing back monovalence nickel ion and the mol ratio of hydroxide ion, be condensing reflux 180 minutes under the microwave-excitation heating condition of 200W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 120 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 10 hours.
(1) nickelous oxalate and sodium hydroxide are dissolved in respectively in the ethylene glycol, the concentration of nickelous oxalate is 0.05mol/L, and concentration sodium hydroxide is 1.20mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be that solution that 1:8 gets the above-mentioned nickelous oxalate for preparing and sodium hydroxide respectively joins and mixes stirring 30 minutes in the reaction vessel by mixing back monovalence nickel ion and the mol ratio of hydroxide ion, be condensing reflux 30 seconds under the microwave-excitation heating condition of 1500W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 120 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 10 hours.
Embodiment 7
(1) nickel hydroxide and potassium hydroxide are dissolved in respectively in the mixing solutions of water that volume ratio is 1:5 and ethylene glycol, the concentration of nickel hydroxide is 0.05mol/L, and the concentration of potassium hydroxide is 1.20mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be that solution that 1:8 gets the above-mentioned nickel hydroxide for preparing and potassium hydroxide respectively joins and mixes stirring 30 minutes in the reaction vessel by mixing back monovalence nickel ion and the mol ratio of hydroxide ion, be condensing reflux 120 minutes under the microwave-excitation heating condition of 1500W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 120 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 10 hours.
(1) with in nickelous nitrate, nickelous chloride and the water-soluble solution of potassium hydroxide difference, the concentration of nickelous nitrate is 0.025mol/L, and the concentration of nickelous chloride is 0.025mol/L, and the concentration of potassium hydroxide is 1.20mol/L, and magnetic agitation 30 minutes is to filling dissolving.
(2) be that solution that 1:8 gets the above-mentioned nickelous nitrate, nickelous chloride and the potassium hydroxide that prepare respectively joins and mixes stirring 30 minutes in the reaction vessel by mixing back monovalence nickel ion and the mol ratio of hydroxide ion, be condensing reflux 120 minutes under the microwave-excitation heating condition of 1500W at power, naturally cool to room temperature after centrifugation namely obtain nano material.
(3) will go up after the step, the nano material that obtains was successively used deionized water and absolute ethanol washing, put into that 120 ℃ of dryings just obtain two-dimentional nickel hydroxide nano material in the vacuum drying oven after 10 hours.
Fig. 7 is the scanning electron microscope diagram of two-dimentional nickel hydroxide nano material, and prepared scantling and pattern are even, is the super-thin sheet-shaped structure, favorable dispersity.
Claims (4)
1. the method for the synthetic class Graphene two dimension of microwave liquid phase nickel hydroxide nano material, it is characterized in that: concrete steps are as follows:
Step 1, nickel salt and alkaline reagents are dissolved in respectively in the hydrophilic solvent, the volumetric molar concentration of monovalence nickel ion is 0.05~1.50mol/L in the solution of dissolving back, and the volumetric molar concentration of hydroxide ion is 0.20~6.00mol/L, and fully the dissolving back is standby;
Step 2, two kinds of solution of step 1 gained are mixed, blending ratio is that the mol ratio of monovalence nickel ion and hydroxide ion is 1:(1~8); Condensing reflux under the microwave-excitation heating condition, naturally cool to room temperature after centrifugation namely obtain nano material;
Step 3, the resulting nano material of step 2 successively used deionized water and absolute ethanol washing after, just obtain two-dimentional nickel hydroxide nano material after putting into the vacuum drying oven drying.
2. a kind of microwave liquid phase as claimed in claim 1 is synthesized the method for class Graphene two dimension nickel hydroxide nano material, and it is characterized in that: described nickel salt raw material is: nickelous nitrate, nickelous acetate, nickelous chloride, single nickel salt, nickelous oxalate, the mixing salt of one or more in the nickel hydroxide.
3. a kind of microwave liquid phase as claimed in claim 1 is synthesized the method for class Graphene two dimension nickel hydroxide nano material, it is characterized in that: described alkaline reagents is: potassium hydroxide, sodium hydroxide, ammoniacal liquor, urea, the mixed base of one or more in the quadrol.
4. a kind of microwave liquid phase as claimed in claim 1 is synthesized the method for class Graphene two dimension nickel hydroxide nano material, it is characterized in that: described hydrophilic solvent is: deionized water, ethanol, ethylene glycol, glycerol, isopropylcarbinol, acetone, benzene, vinylbenzene, the mixing solutions of one or more in the acetonitrile.
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Cited By (5)
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CN105060284A (en) * | 2015-08-14 | 2015-11-18 | 扬州大学 | Preparation method for graphene powder with micro-nano structure |
CN105161314A (en) * | 2015-08-26 | 2015-12-16 | 西南石油大学 | Nano nickel oxide/nickel/graphene composite material and preparation method and application thereof |
CN107248572A (en) * | 2017-08-28 | 2017-10-13 | 北京理工大学 | A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery |
CN108039470A (en) * | 2017-12-11 | 2018-05-15 | 宁波高新区锦众信息科技有限公司 | A kind of preparation method of alkaline secondary cell graphene-nickel hydroxide composite material |
CN112390298A (en) * | 2019-08-19 | 2021-02-23 | Tcl集团股份有限公司 | Modified metal oxide, preparation method thereof and quantum dot light-emitting diode |
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CN1724390A (en) * | 2005-06-30 | 2006-01-25 | 上海交通大学 | Process for preparing alpha-phase nickel hydroxide by microwave water heating method |
CN101676441A (en) * | 2008-09-16 | 2010-03-24 | 中国科学院福建物质结构研究所 | Single-layer beta phase nickel hydroxide two dimensional nano single chip and synthesizing method thereof |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1724390A (en) * | 2005-06-30 | 2006-01-25 | 上海交通大学 | Process for preparing alpha-phase nickel hydroxide by microwave water heating method |
CN101676441A (en) * | 2008-09-16 | 2010-03-24 | 中国科学院福建物质结构研究所 | Single-layer beta phase nickel hydroxide two dimensional nano single chip and synthesizing method thereof |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105060284A (en) * | 2015-08-14 | 2015-11-18 | 扬州大学 | Preparation method for graphene powder with micro-nano structure |
CN105161314A (en) * | 2015-08-26 | 2015-12-16 | 西南石油大学 | Nano nickel oxide/nickel/graphene composite material and preparation method and application thereof |
CN105161314B (en) * | 2015-08-26 | 2018-09-11 | 四川天策聚材科技有限公司 | Nano-nickel oxide/nickel/graphene composite material and its preparation method and application |
CN107248572A (en) * | 2017-08-28 | 2017-10-13 | 北京理工大学 | A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery |
CN108039470A (en) * | 2017-12-11 | 2018-05-15 | 宁波高新区锦众信息科技有限公司 | A kind of preparation method of alkaline secondary cell graphene-nickel hydroxide composite material |
CN112390298A (en) * | 2019-08-19 | 2021-02-23 | Tcl集团股份有限公司 | Modified metal oxide, preparation method thereof and quantum dot light-emitting diode |
CN112390298B (en) * | 2019-08-19 | 2022-08-23 | Tcl科技集团股份有限公司 | Modified metal oxide, preparation method thereof and quantum dot light-emitting diode |
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