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
- Publication number
- CN102126762A CN102126762A CN 201110108760 CN201110108760A CN102126762A CN 102126762 A CN102126762 A CN 102126762A CN 201110108760 CN201110108760 CN 201110108760 CN 201110108760 A CN201110108760 A CN 201110108760A CN 102126762 A CN102126762 A CN 102126762A
- Authority
- CN
- China
- Prior art keywords
- solution
- nio
- microspheres
- flower
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000004005 microsphere Substances 0.000 title claims abstract description 7
- 238000012876 topography Methods 0.000 title description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 12
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims abstract description 11
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 239000004094 surface-active agent Substances 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims abstract 5
- 239000005711 Benzoic acid Substances 0.000 claims abstract 3
- 235000010233 benzoic acid Nutrition 0.000 claims abstract 3
- 238000004729 solvothermal method Methods 0.000 claims abstract 2
- 239000000047 product Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 7
- 229910000480 nickel oxide Inorganic materials 0.000 description 39
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 230000005291 magnetic effect Effects 0.000 description 12
- 238000013019 agitation Methods 0.000 description 11
- 238000002156 mixing Methods 0.000 description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 6
- -1 polyoxyethylene Polymers 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 5
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 229910018661 Ni(OH) Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229940078494 nickel acetate Drugs 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 235000009355 Dianthus caryophyllus Nutrition 0.000 description 1
- 240000006497 Dianthus caryophyllus Species 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004984 smart glass Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种表面形貌可控的NiO纳米花状微球的制备方法，属于无机纳米材料技术领域。通过溶剂热法制备，包括以下步骤：将表面活性剂溶解于乙二醇溶剂中，将硝酸镍和苯甲酸分别溶解于上述溶液中，之后加入浓度为2mol/L的NaOH溶液，形成蓝绿色透明的混合溶液；将上述混合溶液放置于聚四氟乙烯内衬的不锈钢反应釜内反应，得到的浑浊溶液进行离心处理，再置于烘箱中干燥得到氢氧化镍前驱物；将前驱物在马弗炉中煅烧得到目的产物纳米NiO花状微球。本发明所制得的表面形貌可控的NiO纳米花状微球具有高的比表面积、具有多孔径分布的特点、纯度高，制备工艺简单。The invention discloses a method for preparing NiO nano flower-like microspheres with controllable surface morphology, and belongs to the technical field of inorganic nanometer materials. Prepared by solvothermal method, including the following steps: dissolving surfactant in ethylene glycol solvent, dissolving nickel nitrate and benzoic acid in the above solution respectively, and then adding NaOH solution with a concentration of 2mol/L to form blue-green transparent The mixed solution; the above mixed solution is placed in a polytetrafluoroethylene-lined stainless steel reactor for reaction, and the obtained turbid solution is centrifuged, and then dried in an oven to obtain a nickel hydroxide precursor; the precursor is placed in a muffle Calcining in a furnace to obtain the target product nano NiO flower-like microspheres. The NiO nano-flower-shaped microspheres with controllable surface morphology prepared by the invention have high specific surface area, characteristics of multi-diameter distribution, high purity and simple preparation process.
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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101087600A CN102126762B (en) | 2011-04-28 | 2011-04-28 | Method for preparing NiO nano flowerlike microspheres with surface topography controllable |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101087600A CN102126762B (en) | 2011-04-28 | 2011-04-28 | Method for preparing NiO nano flowerlike microspheres with surface topography controllable |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102126762A true CN102126762A (en) | 2011-07-20 |
| CN102126762B CN102126762B (en) | 2012-07-04 |
Family
ID=44265087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101087600A Expired - Fee Related CN102126762B (en) | 2011-04-28 | 2011-04-28 | Method for preparing NiO nano flowerlike microspheres with surface topography controllable |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102126762B (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103482712A (en) * | 2013-09-06 | 2014-01-01 | 浙江大学 | A kind of method for preparing β-Ni(OH)2 flower-like microspheres |
| CN103482668A (en) * | 2013-09-09 | 2014-01-01 | 青岛科技大学 | A kind of coproduction preparation method of CeO2 microsphere and Ni(OH)2 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 |
| CN104610998A (en) * | 2013-12-19 | 2015-05-13 | 北京林业大学 | Method for preparing biodiesel by employing flower-like nickel-based catalyst material |
| CN104743617A (en) * | 2015-03-16 | 2015-07-01 | 沈阳化工大学 | Preparation method and application of nano-sheet assembled flower-like NiO microsphere |
| 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 |
| CN106807379A (en) * | 2015-11-27 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of flower ball-shaped nickel cobalt oxide oxygen-separating catalyst and its preparation method and application |
| CN108144616A (en) * | 2018-01-18 | 2018-06-12 | 太原理工大学 | A kind of low-temperature catalyzed decomposition N2The preparation method of the porous NiO nano flakes catalyst of O |
| CN109205681A (en) * | 2018-09-12 | 2019-01-15 | 嘉兴学院 | A kind of three-dimensional hierarchical structure metal oxide and preparation method thereof |
| CN109374687A (en) * | 2018-11-02 | 2019-02-22 | 华中科技大学 | A NO2 gas sensor based on NiO nanocrystal and its preparation method |
| CN110745800A (en) * | 2019-11-07 | 2020-02-04 | 南京师范大学 | A kind of nitrogen-doped nickel phosphide nanoflower, preparation method and application thereof |
| CN111226985A (en) * | 2020-01-20 | 2020-06-05 | 曲阜师范大学 | Ni/Ni3S2Nano antibacterial agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269850A (en) * | 2008-05-06 | 2008-09-24 | 华东理工大学 | A kind of preparation method of flower-shaped nickel oxide |
| CN101985367A (en) * | 2010-07-28 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing multi-level α-Ni(OH)2 or NiO nanocrystals by microwave solvothermal method |
-
2011
- 2011-04-28 CN CN2011101087600A patent/CN102126762B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269850A (en) * | 2008-05-06 | 2008-09-24 | 华东理工大学 | A kind of preparation method of flower-shaped nickel oxide |
| CN101985367A (en) * | 2010-07-28 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing multi-level α-Ni(OH)2 or NiO nanocrystals by microwave solvothermal method |
Non-Patent Citations (1)
| Title |
|---|
| 《J. Phys. Chem. C》 20090701 Bin Zhao et al. Synthesis of Flower-Like NiO and Effects of Morphology on Its Catalytic Properties 第14440-14447页 1 第113卷, 第32期 2 * |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102489303A (en) * | 2011-11-14 | 2012-06-13 | 青岛科技大学 | Preparation method of cerium-doped NiO microsphere with hierarchical structure |
| CN102489303B (en) * | 2011-11-14 | 2013-04-17 | 青岛科技大学 | A kind of preparation method of cerium-doped NiO hierarchical structure microsphere |
| CN103833076A (en) * | 2012-11-27 | 2014-06-04 | 王泰林 | Nickel oxide-titanium dioxide nano composite material |
| 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 |
| CN103482712A (en) * | 2013-09-06 | 2014-01-01 | 浙江大学 | A kind of method for preparing β-Ni(OH)2 flower-like microspheres |
| CN103482668A (en) * | 2013-09-09 | 2014-01-01 | 青岛科技大学 | A kind of coproduction preparation method of CeO2 microsphere and Ni(OH)2 microsphere |
| CN104610998B (en) * | 2013-12-19 | 2017-07-04 | 北京林业大学 | A kind of method that biodiesel is prepared using flower-shaped nickel catalyst agent material |
| CN104610998A (en) * | 2013-12-19 | 2015-05-13 | 北京林业大学 | Method for preparing biodiesel by employing flower-like nickel-based catalyst material |
| CN103818974A (en) * | 2014-02-20 | 2014-05-28 | 浙江大学 | Preparation method and product of colloid NiO nanocrystal |
| CN103818974B (en) * | 2014-02-20 | 2015-06-03 | 浙江大学 | Preparation method and product of colloid NiO nanocrystal |
| CN104743617A (en) * | 2015-03-16 | 2015-07-01 | 沈阳化工大学 | Preparation method and application of nano-sheet assembled flower-like NiO microsphere |
| 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 |
| 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 |
| CN106807379A (en) * | 2015-11-27 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of flower ball-shaped nickel cobalt oxide oxygen-separating catalyst and its preparation method and application |
| CN106745133A (en) * | 2017-01-24 | 2017-05-31 | 武汉工程大学 | A kind of preparation method of water insoluble hydroxide |
| CN106745133B (en) * | 2017-01-24 | 2018-03-20 | 武汉工程大学 | A kind of preparation method of hydroxide not soluble in water |
| CN108144616A (en) * | 2018-01-18 | 2018-06-12 | 太原理工大学 | A kind of low-temperature catalyzed decomposition N2The preparation method of the porous NiO nano flakes catalyst of O |
| CN108144616B (en) * | 2018-01-18 | 2020-11-06 | 太原理工大学 | Low-temperature catalytic decomposition of N2Preparation method of porous NiO nano flake catalyst of O |
| CN109205681A (en) * | 2018-09-12 | 2019-01-15 | 嘉兴学院 | A kind of three-dimensional hierarchical structure metal oxide and preparation method thereof |
| CN109374687A (en) * | 2018-11-02 | 2019-02-22 | 华中科技大学 | A NO2 gas sensor based on NiO nanocrystal and its preparation method |
| CN110745800A (en) * | 2019-11-07 | 2020-02-04 | 南京师范大学 | A kind of nitrogen-doped nickel phosphide nanoflower, preparation method and application thereof |
| CN111226985A (en) * | 2020-01-20 | 2020-06-05 | 曲阜师范大学 | Ni/Ni3S2Nano antibacterial agent and preparation method thereof |
| CN111226985B (en) * | 2020-01-20 | 2021-04-20 | 曲阜师范大学 | A kind of Ni/Ni3S2 nanometer antibacterial agent and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102126762B (en) | 2012-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102126762A (en) | Method for preparing NiO nano flowerlike microspheres with surface topography controllable | |
| CN104538145B (en) | Multi-scale uniform and single-dispersion magnetic microsphere and preparation method thereof | |
| CN101723436B (en) | Self-assembly zinc oxide hollow sphere and preparation method thereof | |
| CN111420664B (en) | Preparation method of sheet-like cuprous oxide/cobalt oxide nanocomposite material and its application in catalyzing ammonia borane hydrolysis to produce hydrogen | |
| CN102942165B (en) | Graphene and ferrum diselenide composite material and method for preparing same | |
| CN104003448B (en) | A kind of alpha-phase ferricoxide porous core-shell particles and controlledly synthesis preparation method thereof | |
| CN105060351B (en) | Flower-like cobaltosic oxide material composed of nanoparticles and preparation method thereof | |
| CN101597085B (en) | Mesoporous manganese oxide nano granule and preparation method thereof | |
| CN108706637B (en) | Preparation method of a magnetic iron oxide mesocrystalline material with uniform and adjustable size | |
| CN103387258A (en) | Cuprous oxide nano hollow spheres as well as synthetic method and application method thereof | |
| CN104030371B (en) | A method for synthesizing NiO microspheres with mesoporous sheet structure by soft template method | |
| CN108840313B (en) | A kind of preparation method of multi-level spherical nickel diselenide | |
| CN113786856A (en) | Preparation method of bamboo-like nitrogen-doped carbon nanotube loaded with metal monoatomic atoms and nanoparticles | |
| WO2021104087A1 (en) | Metal oxide nanoparticles, and preparation method therefor and application thereof | |
| CN102502886B (en) | Method for preparing cobalt sulfide nanocrystallines by hydrothermal or solvent-thermal method | |
| Liu et al. | Superior thermochemical energy storage performance of the Co3O4/CoO redox couple with a cubic micro-nanostructure | |
| CN105289688A (en) | Method for preparing oxygen reduction catalyst transition metallic oxide/nitrogen-doped carbon composite material | |
| CN111804303B (en) | Preparation method of cerium dioxide/cobalt aluminum hydrotalcite material with core-shell structure | |
| CN107857300A (en) | A kind of preparation method of β types bismuth oxide | |
| CN105668606B (en) | A kind of preparation method of square nano-sheet cerium oxide | |
| CN101475201A (en) | Preparation of Gd(OH)3 and Gd2O3 nano-tubu | |
| CN109273289A (en) | Preparation of nickel-based magnesium cobaltate composite material by solvent method and application thereof | |
| CN106881118B (en) | A kind of method of ion-exchange synthesis heterojunction photocatalyst | |
| CN109133144A (en) | A kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline | |
| CN105948106B (en) | A kind of preparation method of narrow band gap tin ash semiconductor nano material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120704 Termination date: 20160428 |