CN103342396B - 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 a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material, belong to class Graphene ultra-thin two-dimension technical field of nanometer material preparation.
Background technology
The appearance of Graphene opens the new important research field of nano material science and technology, low-dimension nano material scientific research band to two dimension (2D) epoch, two scientist Andre K.Geim of graceful Chester university of Britain and Konstantin S.Novoselov are also because the outstanding contributions made in Graphene preparation characterization are awarded Nobel Prize in physics in 2010.As typical 2D nano structural material, Graphene shows novel physics-chem characteristic, especially high specific surface area and surface carrier mobility, make it there is unique application in fields such as electronics, photonics, spintronicss, in short several years, be just successfully applied to LED display, support of the catalyst, novel energy storage with on converting apparatus.The huge scientific research that Graphene shows and using value also result in investigator has the 2D nano structural material of high surface atom ratio concern to other types, are mainly class graphene inorganic 2D nano structural material.Extensively concerned class Graphene 2D stratified material mainly contains Transition-metal dichalcogenide, transition metal oxide, metal hydroxides etc. at present.Due to huge specific surface area and ultra-thin microtexture, these 2D nano structural materials show special surface tissue and characteristic electron, there is excellent mechanics, electricity and optical property, macroscopically be presented as ultra-thin, transparent and high-flexibility, the fields such as opto-electronic device, biochemical sensor, catalyzer, ultracapacitor, lithium ion battery, fuel cell and solar cell can be widely used in, especially in the photoelectrochemistry reaction field highly depending on bill of material interface performance, 2D material shows superior performance especially.But the performance and application of these a series of innovations of 2D nano structural material but depends on the controlled mass-producing preparation of material.The special performance of 2D nano structural material depends on its thickness and area, thus carrys out by the regulation and control of nanoscale and appearance structure the Some Questions To Be Researched that the new 2D nano material of design and synthesis is considered to modern chemistry and Materials science.In addition, 2D nickel hydroxide nano structured material causes the interest of many scientific workers, a large amount of research work is done in regulation and control synthesis under material microscale, and has achieved its potential application important in gas sensor, catalysis, lithium ion battery, ultracapacitor, fuel cell and Ni-based alkali formula battery etc.
The method that the current 2D of preparation nano structural material extensively adopts is chemical stripping, chemical gas phase heavy (CVD) and molecular beam epitaxial growth (MBE) etc.Although chemical stripping method output is large, there is uncontrollable shortcoming, prepared 2D nano material size out and pattern uneven, especially thickness and size differ.And although chemical vapour deposition can prepare 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 synthesis 2D nano material, and building-up process is simply controlled, is applicable to industrialized developing application.
Based on advanced microwave heating liquid-phase synthesis process, be used in recent years synthesize various nano material.A kind of method (China Patent Publication No. CNIO1864314A) that cutting edge of a knife or a sword etc. discloses synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase is learned in analogy, and obtained product grain size is even.Compared with traditional liquid-phase synthesis process, microwave liquid phase synthesizing method is a kind of material synthesis method of simple, environmental protection, can Reaction time shorten greatly, selectivity heating has the compound of different Microwave Absorption Properties, homogeneous heating, combined coefficient is high, is applicable to extensive preparation.According to the knowledge of the applicant, have no the method reported and utilize microwave liquid phase synthesis class Graphene ultra-thin 2D nickel hydroxide nano material up to now simultaneously.
Summary of the invention
The object of the invention is to meet output greatly to solve prior art simultaneously, and the problem that quality product is controlled, the method for a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material is provided.
The object of the invention is to be achieved through the following technical solutions.
The method of a kind of microwave liquid phase synthesis of the present invention class Graphene two dimension nickel hydroxide nano material, concrete steps are as follows:
Step one, nickel salt and alkaline reagents are dissolved in respectively in hydrophilic solvent, after dissolving, in solution, the volumetric molar concentration of monovalence nickel ion is 0.05 ~ 1.50mol/L, and the volumetric molar concentration of hydroxide ion is 0.20 ~ 6.00mol/L, for subsequent use after fully dissolving;
Step 2, by the mixing of two of step one gained kinds of solution, blending ratio is the mol ratio of monovalence nickel ion and hydroxide ion is 1:(1 ~ 8); Condensing reflux under microwave-excitation heating condition, after naturally cooling to room temperature, namely centrifugation obtains nano material;
After step 3, nano material priority deionized water step 2 obtained and absolute ethanol washing, after putting into vacuum drying oven drying, just obtain two-dimentional nickel hydroxide nano material.
Described nickel salt raw material is: nickelous nitrate, nickelous acetate, nickelous chloride, single nickel salt, nickelous oxalate, one or more the mixing salt in nickel hydroxide;
Described alkaline reagents is: potassium hydroxide, sodium hydroxide, ammoniacal liquor, urea, one or more the mixed base in quadrol;
Described hydrophilic solvent is: deionized water, ethanol, ethylene glycol, glycerol, isopropylcarbinol, acetone, benzene, vinylbenzene, one or more the mixing solutions in acetonitrile.
Beneficial effect
1, the method for a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material of the present invention, its morphology is characterized as ultra-thin, big area, single dispersing sheet, 1nm can be reached when thickness is the thinnest, length and width are several micron, can be used for preparing metal-hydrogen nickel alkaline cell, electrode of super capacitor active material and catalyzer etc.
2, the method for a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material of the present invention, simple to operate, with low cost, reaction conditions is gentle, whole reaction process is carried out at ambient pressure, and temperature of reaction is between 80 ~ 170 DEG C, and the reaction times is 0.5 ~ 180 minute, Product size and pattern are even, good dispersity.
3, the method for a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material of the present invention, the microwave liquid-phase synthesis process adopted combines the advantage of microwave rapid and uniform heating and liquid phase synthesis, reaction time is short, reaction yield is high, and the selectivity heating of microwave is beneficial to the generation suppressing side reaction, therefore obtained product purity is high, without other impurity.The method preparing ultra-thin class Graphene two-dimension nano materials with the chemical stripping generally adopted and high temperature vapour deposition is compared, and the method designed by the present invention has the advantage such as controlled synthesis, a large amount of synthesis, is applicable to suitability for industrialized production and mass-producing application.
Accompanying drawing explanation
Fig. 1 is for illustrating the X-ray diffracting spectrum of the two-dimentional nickel hydroxide nano material prepared by case study on implementation 1;
Fig. 2 is for illustrating the scanning electron microscope diagram of the two-dimentional nickel hydroxide nano material prepared by case study on implementation 1;
Fig. 3 is for illustrating the transmission electron microscope figure of the two-dimentional nickel hydroxide nano material prepared by case study on implementation 1;
Fig. 4 is for illustrating the high-resolution-ration transmission electric-lens figure of the two-dimentional nickel hydroxide nano material prepared by case study on implementation 2;
Fig. 5 is for illustrating the specific surface area test pattern of the two-dimentional nickel hydroxide nano material prepared by case study on implementation 3;
Fig. 6 is for illustrating the energy spectrogram of the two-dimentional nickel hydroxide nano material prepared by case study on implementation 4;
Fig. 7 is for illustrating the scanning electron microscope diagram of the two-dimentional nickel hydroxide nano material prepared by case study on implementation 8.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention will be further described.
Embodiment 1
(1) nickelous nitrate and sodium hydroxide are dissolved in respectively in deionized water, the concentration of nickelous nitrate is 0.05mol/L, and the concentration of sodium hydroxide is 0.1mol/L, and magnetic agitation 30 minutes, to filling dissolving.
(2) be 1:4 by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, the solution getting above-mentioned nickelous nitrate and the sodium hydroxide prepared respectively to join in reaction vessel mix and blend 30 minutes, condensing reflux 60 minutes under the microwave-excitation heating condition that power is 700W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 100 DEG C of dryings in vacuum drying oven and after 12 hours, just obtain two-dimentional nickel hydroxide nano material.
Fig. 1 is the X ray diffracting spectrum of two-dimentional nickel hydroxide nano material, and obtained material is the nickel hydroxide of pure α phase six side laminate structure, do not have other as β phase or other impurity, and material crystalline is good.Fig. 2 is the scanning electron microscope diagram sheet of two-dimentional nickel hydroxide nano material, and obtained scantling and pattern evenly, are nano-sheet, favorable dispersity.Fig. 3 is the transmission electron micrograph of two-dimentional nickel hydroxide nano material, and obtained material is transparent superthin structure, is similar to Graphene, and its thickness is about 1nm.
Embodiment 2
(1) nickelous nitrate and potassium hydroxide are dissolved in respectively in 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, to filling dissolving.
(2) be 1:1 by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, the solution getting above-mentioned nickelous nitrate and the potassium hydroxide prepared respectively to join in reaction vessel mix and blend 30 minutes, condensing reflux 60 minutes under the microwave-excitation heating condition that power is 700W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 100 DEG C of dryings in vacuum drying oven and after 12 hours, just obtain two-dimentional nickel hydroxide nano material.
Fig. 4 is the high resolution transmission electron microscopy picture of two-dimentional nickel hydroxide nano material, and obtained material is typical class Graphene laminate structure, and is evenly individual layer, and its thickness is about 1.7nm.
Embodiment 3
(1) nickelous chloride and potassium hydroxide are dissolved in respectively in 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, to filling dissolving.
(2) be that solution that 1:8 gets above-mentioned nickelous chloride and the potassium hydroxide prepared respectively to join in reaction vessel mix and blend 30 minutes by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, condensing reflux 60 minutes under the microwave-excitation heating condition that power is 700W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 110 DEG C of dryings in vacuum drying oven and after 12 hours, just obtain two-dimentional nickel hydroxide nano material.
Fig. 5 is the specific surface area test pattern of two-dimentional nickel hydroxide nano material, and because obtained nickel hydroxide is class Graphene two-dimensional ultrathin nano material, have very high specific surface area, test result shows its specific surface area up to 190.15m
2/ g.
Embodiment 4
(1) be dissolved in deionized water and ethylene glycol respectively by single nickel salt and urea, the concentration of single nickel salt is 0.10mol/L, and the concentration of urea is 0.80mol/L, and magnetic agitation 30 minutes, to filling dissolving.
(2) be that solution that 1:4 gets above-mentioned single nickel salt and the urea prepared respectively to join in reaction vessel mix and blend 30 minutes by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, condensing reflux 30 minutes under the microwave-excitation heating condition that power is 900W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 80 DEG C of dryings in vacuum drying oven and after 12 hours, just obtain two-dimentional nickel hydroxide nano material.
Fig. 6 be two-dimentional nickel hydroxide nano material can spectrogram, except the Si that comes from test base and C element, Ni and O element only detected, occur without other impurity elements, the nickel hydroxide purity prepared by explanation is higher.
Embodiment 5
(1) nickel acetate and ammoniacal liquor are dissolved in respectively in 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, to filling dissolving.
(2) be that solution that 1:3 gets above-mentioned nickel acetate and the ammoniacal liquor prepared respectively to join in reaction vessel mix and blend 30 minutes by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, condensing reflux 180 minutes under the microwave-excitation heating condition that power is 200W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 120 DEG C of dryings in vacuum drying oven and after 10 hours, just obtain two-dimentional nickel hydroxide nano material.
Embodiment 6
(1) nickelous oxalate and sodium hydroxide are dissolved in respectively in ethylene glycol, the concentration of nickelous oxalate is 0.05mol/L, and the concentration of sodium hydroxide is 1.20mol/L, and magnetic agitation 30 minutes, to filling dissolving.
(2) be that solution that 1:8 gets above-mentioned nickelous oxalate and the sodium hydroxide prepared respectively to join in reaction vessel mix and blend 30 minutes by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, condensing reflux 30 seconds under the microwave-excitation heating condition that power is 1500W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 120 DEG C of dryings in vacuum drying oven and after 10 hours, just obtain two-dimentional nickel hydroxide nano material.
Embodiment 7
(1) nickel hydroxide and potassium hydroxide being dissolved in respectively volume ratio is that in the water of 1:5 and the mixing solutions of 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, to filling dissolving.
(2) be that solution that 1:8 gets above-mentioned nickel hydroxide and the potassium hydroxide prepared respectively to join in reaction vessel mix and blend 30 minutes by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, condensing reflux 120 minutes under the microwave-excitation heating condition that power is 1500W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 120 DEG C of dryings in vacuum drying oven and after 10 hours, just obtain two-dimentional nickel hydroxide nano material.
Embodiment 8
(1) by nickelous nitrate, nickelous chloride and potassium hydroxide respectively water-soluble solution, 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, to filling dissolving.
(2) be that solution that 1:8 gets above-mentioned nickelous nitrate, nickelous chloride and the potassium hydroxide prepared respectively to join in reaction vessel mix and blend 30 minutes by the mol ratio of monovalence nickel ion and hydroxide ion after mixing, condensing reflux 120 minutes under the microwave-excitation heating condition that power is 1500W, after naturally cooling to room temperature, namely centrifugation obtains nano material.
(3), after the nano material priority deionized water upper step obtained and absolute ethanol washing, put into 120 DEG C of dryings in vacuum drying oven and after 10 hours, just obtain two-dimentional nickel hydroxide nano material.
Fig. 7 is the scanning electron microscope diagram of two-dimentional nickel hydroxide nano material, and obtained scantling and pattern evenly, are super-thin sheet-shaped structure, favorable dispersity.
Claims (4)
1. a method for microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material, is characterized in that: concrete steps are as follows:
Step one, nickel salt and alkaline reagents are dissolved in respectively in hydrophilic solvent, after dissolving, in solution, the volumetric molar concentration of monovalence nickel ion is 0.05 ~ 1.50mol/L, and the volumetric molar concentration of hydroxide ion is 0.20 ~ 6.00mol/L, for subsequent use after fully dissolving;
Step 2, by the mixing of two of step one gained kinds of solution, blending ratio is the mol ratio of monovalence nickel ion and hydroxide ion is 1:(1 ~ 8); Condensing reflux under microwave-excitation heating condition, after naturally cooling to room temperature, namely centrifugation obtains nano material;
After step 3, nano material priority deionized water step 2 obtained and absolute ethanol washing, after putting into vacuum drying oven drying, just obtain two-dimentional α nickel hydroxide nano material.
2. the method for a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material as claimed in claim 1, it is characterized in that: described nickel salt raw material is: nickelous nitrate, nickelous acetate, nickelous chloride, single nickel salt, one or more the mixing salt in nickelous oxalate.
3. the method for a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material as claimed in claim 1, it is characterized in that: described alkaline reagents is: potassium hydroxide, sodium hydroxide, ammoniacal liquor, urea, one or more the mixed base in quadrol.
4. the method for a kind of microwave liquid phase synthesis class Graphene two dimension nickel hydroxide nano material as claimed in claim 1, it is characterized in that: described hydrophilic solvent is: deionized water, ethanol, ethylene glycol, glycerol, isopropylcarbinol, acetone, benzene, vinylbenzene, one or more the mixing solutions in acetonitrile.
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| 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 |
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