CN102126762A - Method for preparing NiO nano flowerlike microspheres with surface topography controllable - Google Patents
Method for preparing NiO nano flowerlike microspheres with surface topography controllable Download PDFInfo
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Abstract
The invention discloses a method for preparing NiO nano flowerlike microspheres with surface topography controllable, belonging to the technical field of inorganic nano materials. The method is characterized by preparing the microspheres by a solvothermal method and comprises the following steps: dissolving a surfactant into a glycol solvent, respectively dissolving nickel nitrate and benzoic acid into the prepared solution, and later, adding a 2mol/L NaOH solution to form blue-green transparent mixed solution; putting the mixed solution into a stainless steel reactor with polytetrafluoroethylene lining to react; centrifuging the obtained turbid solution and then drying the obtained precipitate in a drying oven to obtain a nickel hydroxide precursor; and calcining the precursor in a muffle furnace to obtain the target products, namely NiO nano flowerlike microspheres. The microspheres prepared by the method have the characteristics of high specific surface area, multiple pore size distribution and high purity; and the preparation process is simple.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, relate to the preparation method of nickel oxide (NiO) the nano flower-like microballoon that a kind of surface topography can regulate and control continuously.
Background technology
Nano-nickel oxide (NiO) is a kind of important P-type semiconductor material, because its unique electricity, magnetics and catalysis characteristics, it is applied in fields such as catalytic field, smart window field, fuel cell field, field of magnetic material, gas sensor field, electroplating film field and active fibre widely, be a kind of up-and-coming functional material, become one of present worldwide research focus.Because these unique character intensive of nano NiO depend on its appearance structure and size, therefore the study on the synthesis to the nano NiO of different-shape structure has caused numerous scientific workers' very big attention.According to the literature, and Gui etc. (J.Phys.Chem.C, 2007,111,5622-5627), prepared and be hexagonal NiO nanometer lamellar body by nickel chloride aqueous solution and the reaction of hydrazine aqueous solution.Wang etc. (Chemical Physics Letters, 2002,362,119-122) by thermal decomposition method, adopt NaCl as fusing assistant, make nickelous carbonate that thermolysis take place under the 1173K temperature and obtain the NiO nanometer rod.Kuang etc. (J.Phys.Chem.C, 2009,113,5508-5513) by hydrothermal method, under the effect of anion surfactant, prepared the NiO micron ball of novel laminate structure.Zhu etc. (J.Phys.Chem.B, 2004,108,3488-3491) adopt nickel acetate as the nickel source, ammoniacal liquor is as alkaline complexing agent, by Hydrothermal Preparation monocrystalline NiO nanometer sheet.Feng etc. (J.Am.Chem.Soc.2008,130, be that template has prepared NiO material bimodal distribution, order mesoporous with KIT-6 5262-5266).
The NiO nano flower-like microballoon of the present invention's preparation has uniform distribution of sizes and multiple aperture characteristic distributions, have higher specific surface area and unique physical surface properties, and can purposively regulate and control its surface topography continuously by changing synthetic material proportion, and then change the physics and the chemical property of material.Therefore become a kind of functional materials in controlled NiO nano flower-like microballoon environmental engineering of this surface topography and the catalytic field with development prospect.Chen etc. (J.Phys.Chem.C, 2009,113,14440-14447) mix by nickel acetate aqueous solution and ammoniacal liquor, hydrolysis has prepared the NiO nano flower-like microballoon of carnation shape.Li Chunzhong etc. are raw material with vulkacit H, Nickelous nitrate hexahydrate and deionized water in patent " a kind of preparation method who spends the shape nickel oxide ", have gone out colored shape nickel oxide by Hydrothermal Preparation.But the synthetic bibliographical information that yet there are no of the NiO Nano microsphere that can regulate and control continuously of surface topography up to the present.
Summary of the invention
The solvent process for thermosynthesizing that the purpose of this invention is to provide a kind of nano NiO material.Further purpose of the present invention provides the method for preparing the NiO nano flower-like microballoon that a series of surface tissues can regulate and control continuously by solvent-thermal method.
Above-mentioned purpose of the present invention reaches by following technical proposals and measure:
The preparation method of the NiO nano flower-like microballoon that surface topography of the present invention is controlled is characterized in that, by the solvent-thermal method preparation, specifically may further comprise the steps:
(1) with surfactant dissolves in ethylene glycol solvent, be mixed with volumetric concentration and be 2%～6% solution; Nickelous nitrate and phenylformic acid are dissolved in respectively in the above-mentioned solution, and wherein the concentration of nickelous nitrate is 0.03mol/L～0.3mol/L, and benzoic concentration is 0.03mol/L～0.15mol/L, magnetic agitation 1h; Dropwise adding concentration afterwards is the NaOH solution of 2mol/L, and the volume ratio of NaOH solution and mixing solutions is 0.02: 1～0.05: 1, and magnetic agitation 0.5h forms the transparent mixing solutions of blue-greenish colour.
(2) above-mentioned mixing solutions is positioned in the teflon-lined stainless steel cauldron sealing, reacting by heating 8～14h in baking oven; Temperature of reaction is 160～220 ℃.
(3) turbid solution that step (2) is obtained carries out centrifugal treating, and the throw out that obtains is cleaned repeatedly with dehydrated alcohol and deionized water, places that drying obtains the nickel hydroxide precursor under 60～100 ℃ of temperature of baking oven again.
(4) the nickel hydroxide precursor that step (3) is obtained 300～550 ℃ of calcinings in retort furnace obtained the flower-shaped microballoon of purpose product nano NiO in 2～6 hours.
The chemical equation of entire reaction course can be expressed as follows:
Ni
2++2OH-→Ni(OH)
2
Ni(OH)
2→NiO+H
2O
Wherein, described nickelous nitrate is a Nickelous nitrate hexahydrate, and tensio-active agent is polyoxyethylene glycol (PEG-400).
In entire reaction course, ethylene glycol be solvent also be reductive agent, stop the Ni in the solution
2+Be oxidized to Ni
3+Polyoxyethylene glycol is as tensio-active agent, as nanometer Ni (OH)
2During generation, polyoxyethylene glycol can be coated on its surface by hydrogen bond or affinity interaction, prevents the nanoparticle coagulation, increases its dispersiveness, strengthens the stability of solution.Phenylformic acid helps to strengthen the packaging efficiency of the flower-shaped microballoon of nano NiO as soft template.
The NiO nano flower-like microballoon that the surface topography of the present invention's preparation can be regulated and control continuously not only helps opening up particular performances of NiO own and application, and helps the development and application of other new nano structure devices.
The preparation method of the NiO nano flower-like microballoon that a kind of surface topography of the present invention can be regulated and control continuously, its advantage and effect are:
(1) prepared NiO nano flower-like microballoon, its surface topography can change proportioning raw materials and reach purposive carrying out and regulate and control continuously.
(2) the controlled NiO nano flower-like microballoon of prepared surface topography has high specific surface area.Its specific surface area can reach 10～80 meters squared per gram, and can regulate and control continuously in this scope.
(3) the controlled NiO nano flower-like microballoon of prepared surface topography has the characteristics of multiple aperture distribution and large pore volume.
(4) the controlled NiO nano flower-like microballoon purity height of prepared surface topography does not contain the NiO of other pattern.
(5) the controlled NiO nano flower-like microballoon stable performance of prepared surface topography, volatility not in air, and still can keep original appearance through its pattern of high-temperature calcination.
(6) preparation technology is simple, to equipment require lowly, the prices of raw and semifnished materials are cheap, obtain easily, can produce in enormous quantities.
Description of drawings
Fig. 1. the X-ray diffraction spectrogram of the nano flower-like microballoon A of embodiment 1.
Fig. 2. the stereoscan photograph of the nano flower-like microballoon A of embodiment 1.
Fig. 3. the X-ray diffraction spectrogram of the nano flower-like microballoon B of embodiment 2.
Fig. 4. the stereoscan photograph of the nano flower-like microballoon B of embodiment 2.
Fig. 5. the X-ray diffraction spectrogram of the nano flower-like microballoon C of embodiment 3.
Fig. 6. the stereoscan photograph of the nano flower-like microballoon C of embodiment 3.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
(1) 30mL ethylene glycol is put into the beaker of 50mL, added 0.6mL polyoxyethylene glycol (PEG-400), behind the magnetic agitation 2h; Add 10mmol Nickelous nitrate hexahydrate and 1mmol phenylformic acid, behind the magnetic agitation 1h; Dripping 0.6mL concentration is the NaOH solution of 2mol/L, and magnetic agitation 0.5h forms the transparent mixing solutions of blue-greenish colour.
(2) above-mentioned mixing solutions is positioned in the teflon-lined stainless steel cauldron of 50ml sealing, reacting by heating 8h in baking oven; Temperature of reaction is 160 ℃.
(3) the tetrafluoroethylene pressurized vessel is taken out, be cooled to normal temperature.Reaction solution is taken out, the 50ml centrifuge tube of packing into is isolated the precipitated product in the reaction solution with the method for centrifugation, and is cleaned repeatedly 3 times with dehydrated alcohol and deionized water, place 60 ℃ of baking ovens dry the precipitated product that obtains, promptly obtain nickel hydroxide precursor powder.
(4) nickel hydroxide precursor roasting in retort furnace that step (3) is obtained (1 ℃/min of temperature rise rate is incubated 2 hours down at 350 ℃) can obtain purpose product nano flower-like microballoon A powder.Fig. 1 is the X ray diffracting spectrum of nano flower-like microballoon A, and all diffraction peaks are all well corresponding to a cube phase NiO, and diffraction peak intensity is high and sharp-pointed, interpret sample degree of crystallinity height.Fig. 2 is the scanning electron microscope collection of illustrative plates of nano flower-like microballoon A, and nano flower-like microballoon A size evenly is of a size of about 2 μ m.All there is distribution in the aperture of nano flower-like microballoon A at 3.5nm, 10nm, 80nm and 180nm place.
Embodiment 2
(1) 30mL ethylene glycol is put into the beaker of 50mL, added 1.2mL polyoxyethylene glycol (PEG-400), behind the magnetic agitation 2h; Add 6mmol Nickelous nitrate hexahydrate and 3mmol phenylformic acid, behind the magnetic agitation 1h; Dripping 0.9mL concentration is the NaOH solution of 2mol/L, and magnetic agitation 0.5h forms the transparent mixing solutions of blue-greenish colour.
(2) above-mentioned mixing solutions is positioned in the teflon-lined stainless steel cauldron of 50ml sealing, reacting by heating 10h in baking oven; Temperature of reaction is 180 ℃.
(3) the tetrafluoroethylene pressurized vessel is taken out, be cooled to normal temperature.Reaction solution is taken out, the 50ml centrifuge tube of packing into is isolated the precipitated product in the reaction solution with the method for centrifugation, and is cleaned repeatedly 3 times with dehydrated alcohol and deionized water, place 80 ℃ of baking ovens dry the precipitated product that obtains, promptly obtain nickel hydroxide precursor powder.
(4) nickel hydroxide precursor roasting in retort furnace that step (3) is obtained (1 ℃/min of temperature rise rate is incubated 4 hours down at 450 ℃) can obtain purpose product NiO-B nano flower-like microballoon powder.Fig. 3 is the X ray diffracting spectrum of nano flower-like microballoon B, and all diffraction peaks are all well corresponding to a cube phase NiO, and diffraction peak intensity is high and sharp-pointed, interpret sample degree of crystallinity height.Fig. 4 is the scanning electron microscope collection of illustrative plates of nano flower-like microballoon B, and the size of nano flower-like microballoon B evenly is of a size of about 8 μ m.All there is distribution in the aperture of nano flower-like microballoon B at 2nm, 4nm, 7nm, 70nm and 280nm place.
Embodiment 3
(1) 30mL ethylene glycol is put into the beaker of 50mL, added 1.8mL polyoxyethylene glycol (PEG-400), behind the magnetic agitation 2h; Add 1mmol Nickelous nitrate hexahydrate and 5mmol phenylformic acid, behind the magnetic agitation 1h; Dripping 1.5mL concentration is the NaOH solution of 2mol/L, and magnetic agitation 0.5h forms the transparent mixing solutions of blue-greenish colour.
(2) above-mentioned mixing solutions is positioned in the teflon-lined stainless steel cauldron of 50ml sealing, reacting by heating 14h in baking oven; Temperature of reaction is 220 ℃.
(3) the tetrafluoroethylene pressurized vessel is taken out, be cooled to normal temperature.Reaction solution is taken out, the 50ml centrifuge tube of packing into is isolated the precipitated product in the reaction solution with the method for centrifugation, and is cleaned repeatedly 3 times with dehydrated alcohol and deionized water, place 100 ℃ of baking ovens dry the precipitated product that obtains, promptly obtain nickel hydroxide precursor powder.
(4) nickel hydroxide precursor roasting in retort furnace that step (3) is obtained (1 ℃/min of temperature rise rate is incubated 6 hours down at 550 ℃) can obtain purpose product nano flower-like microballoon C powder.Fig. 5 is the X ray diffracting spectrum of nano flower-like microballoon C, and all diffraction peaks are all well corresponding to a cube phase NiO, and diffraction peak intensity is high and sharp-pointed, interpret sample degree of crystallinity height.Fig. 6 is the scanning electron microscope collection of illustrative plates of nano flower-like microballoon C, and the size of nano flower-like microballoon C evenly is of a size of about 4 μ m.All there is distribution in the aperture of nano flower-like microballoon C at 2.5nm, 20nm, 110nm and 250nm place.
Form 1 is the nitrogen adsorption desorption characterization data of three kinds of prepared NiO nano flower-like microballoons of embodiment 1-3 and industrial oxidation nickel catalyzator.This character can greatly be brought into play its catalytic performance, form 2 is the catalytic performance data of prepared three kinds of NiO nano flower-like microballoons of embodiment 1-3 and industrial oxidation nickel catalyzator, catalyzed reaction is selected the CO burning reaction, and all the catalytic performance than industrial oxidation nickel catalyzator is good for the catalytic performance of the NiO nano flower-like microballoon of the preparation of the present invention as a result.
Form 1
Form 2
Claims (1)
1. the preparation method of the controlled NiO nano flower-like microballoon of surface topography is characterized in that, by the solvent-thermal method preparation, specifically may further comprise the steps:
(1) with surfactant dissolves in ethylene glycol solvent, be mixed with volumetric concentration and be 2%～6% solution; Nickelous nitrate and phenylformic acid are dissolved in respectively in the above-mentioned solution, and wherein the concentration of nickelous nitrate is 0.03mol/L～0.3mol/L, and benzoic concentration is 0.03mol/L～0.15mol/L, magnetic agitation 1h; Dropwise adding concentration afterwards is the NaOH solution of 2mol/L, and the volume ratio of NaOH solution and mixing solutions is 0.02: 1～0.05: 1, and magnetic agitation 0.5h forms the transparent mixing solutions of blue-greenish colour;
(2) above-mentioned mixing solutions is positioned in the teflon-lined stainless steel cauldron sealing, reacting by heating 8～14h in baking oven; Temperature of reaction is 160～220 ℃;
(3) turbid solution that step (2) is obtained carries out centrifugal treating, and the throw out that obtains is cleaned repeatedly with dehydrated alcohol and deionized water, places that drying obtains the nickel hydroxide precursor under 60～100 ℃ of temperature of baking oven again;
(4) the nickel hydroxide precursor that step (3) is obtained 300～550 ℃ of calcinings in retort furnace obtained the flower-shaped microballoon of purpose product nano NiO in 2～6 hours.
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| CN102489303A (en) * | 2011-11-14 | 2012-06-13 | 青岛科技大学 | Preparation method of cerium-doped NiO microsphere with hierarchical structure |
| CN102891008A (en) * | 2011-07-21 | 2013-01-23 | 北京化工大学 | Nickel hydroxide nanosheet thin-film material as well as preparation method and application thereof |
| CN103387268A (en) * | 2013-07-30 | 2013-11-13 | 浙江大学 | Preparation method of nano-nickel oxide for electrode material of supercapacitor, and nano-nickel oxide prepared by method |
| CN103482668A (en) * | 2013-09-09 | 2014-01-01 | 青岛科技大学 | Co-production preparation method of CeO2 microspheres and Ni(OH)2 microspheres |
| CN103482712A (en) * | 2013-09-06 | 2014-01-01 | 浙江大学 | Method for preparing beta-Ni(OH)2 flower-like microsphere |
| CN103818974A (en) * | 2014-02-20 | 2014-05-28 | 浙江大学 | Preparation method and product of colloid NiO nanocrystal |
| CN103833076A (en) * | 2012-11-27 | 2014-06-04 | 王泰林 | Nickel oxide-titanium dioxide nano composite material |
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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 |
| CN106745133A (en) * | 2017-01-24 | 2017-05-31 | 武汉工程大学 | A kind of preparation method of water insoluble hydroxide |
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