CN101704558A - Preparation method of nickel oxide nano flake with uniform and mesoporous structure - Google Patents
Preparation method of nickel oxide nano flake with uniform and mesoporous structure Download PDFInfo
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- CN101704558A CN101704558A CN200910237799A CN200910237799A CN101704558A CN 101704558 A CN101704558 A CN 101704558A CN 200910237799 A CN200910237799 A CN 200910237799A CN 200910237799 A CN200910237799 A CN 200910237799A CN 101704558 A CN101704558 A CN 101704558A
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Abstract
The invention provides a preparation method of nickel oxide nano flake with uniform and mesoporous structure, which is implemented by (1) putting 0.05-0.15mol/L of aqueous inorganic salt solution containing nickel in a beaker, adding in surfactant with concentration being 5-10g/L, and performing magnetic stirring for 3h; dripping in ammonia water with the volume ratio of ammonia water to aqueous inorganic salt solution containing nickel being 0.01:1-0.015:1, and performing magnetic stirring for 3h; (2) placing the mixed solution obtained in step (1) in a stainless reaction kettle lined by polytetrafluoroethylene to be sealed, and heating for reaction in a muffle furnace for 12-20h with reaction temperature being 80-150 DEG C; (3) filtering, washing and drying the obtained nepheloid solution to obtain nickelhydroxide primer; (4) calcinating the nickelhydroxide primer obtained in step (3) at 350-500 DEG C for 2-4h to obtain porous structural nickel oxide nano flake. The inventive NiO nano flake has pore diameter of 30-40nm, diameter of 300-400nm, belongs to cubic system, high purity, and good quality.
Description
Technical field:
The present invention relates to a kind of preparation method of inorganic nano material, particularly a kind of evenly, the preparation method of nickel oxide (NiO) nano flake of central hole structure.
Background technology:
Nano-nickel oxide (NiO) is a kind of important semiconductor material, industrial main, become one of present worldwide research focus as producing battery electrode, catalyzer, magneticsubstance, semi-conductor (as pressure-sensitive, thermistor), nickel-zinc ferrite, fuel sensitization solar battery etc.Because these unique character intensive of nano NiO depend on their pattern and size, so synthetic numerous research workers' the very big interest that caused of the nano NiO of different-shape structure.According to the literature, and Han etc. (Powder Technology, 2004,147,113-116) adopt water-oily micella method to prepare the NiO nano particle.(J.Materials Letters, 2007, the NiO nano particle that 61-3174-3178) adopted improved Prepared by Sol Gel Method such as Wu.Yang etc. (J.Cryst.Growth Des, 2007,7,2716-2719) by nickel acetate at water and glycerine mixed solvent, hydrolysis has prepared the NiO nanostructured microsphere of carnation shape.Feng etc. (J.Am.Chem.Soc.2008,130, be that template has prepared NiO material bimodal distribution, order mesoporous with KIT-6 5262-5266).Kuang etc. (J.Phys.Chem.C, 2009,113,5508-5513) under the effect of anion surfactant, by Hydrothermal Preparation the NiO micron ball of novel laminate structure.Zhou (J.AM.CHEM.SOC.2009,131,2959-2964) adopt the hydrazine hydrate method to prepare the concave polyhedron NiO nano particle that nanometer sheet is formed.
In addition, porous material is owing to have equally distributed micropore or hole, porosity height, volume density are little, also have high specific surface area and unique physical surface properties thereof, and different porousness can change the physics and the chemical property of material, so porous structure material becomes a kind of functional materials with development prospect in biotechnology, environmental engineering, catalyzer and the sensor field.
Feng etc. (J.Am.Chem.Soc.2008,130, be that template has prepared bimodal distribution, orderly mesoporous NiO material with KIT-6 5262-5266).Up to the present, evenly, the synthetic bibliographical information that yet there are no of the nano NiO of central hole structure.
Summary of the invention:
The object of the present invention is to provide a kind of evenly, the preparation method of the nickel oxide nano flake of central hole structure, with technical barrier at suitability for industrialized production porous NiO nano-powder, the preparation method of the NiO nano flake of the vesicular structure that a kind of technology is simple, cost is low is provided, to prepare the NiO nano flake of highly purified vesicular structure, have theory and actual application value.
Of the present invention a kind of evenly, the preparation method's of the NiO nano flake of central hole structure technical process as shown in Figure 1, concrete steps are as follows:
(1) the nickeliferous inorganic salt solution of a certain amount of 0.05～0.15mol/L is put into the beaker of 100mL, added tensio-active agent, surfactant concentrations is 5g/L～10g/L, behind the magnetic agitation 3h; Dropping ammonia, the volume ratio of ammoniacal liquor and nickeliferous inorganic salt solution are 0.01: 1～0.015: 1, and magnetic agitation 0.5～2h forms the transparent mixing solutions of blue-greenish colour;
(2) mixing solutions that step (1) is obtained is positioned in the teflon-lined stainless steel cauldron, and sealing is in retort furnace internal heating reaction 12～20h; Temperature of reaction is 80～150 ℃;
(3) turbid solution that step (2) is obtained filter, wash, drying, obtain the nickel hydroxide precursor;
(4) the nickel hydroxide precursor that step (3) is obtained obtains the NiO nano flake of vesicular structure at 350～500 ℃ of roasting 2～4h.
The chemical equation of entire reaction course can be expressed as follows:
NH
3·H
2O→NH
4 ++OH
-
Ni
2++2OH-→Ni(OH)
2
Ni(OH)
2→NiO+H
2O
Wherein, described nickeliferous inorganic salt are Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate.
Wherein, described tensio-active agent is hexadecyl brometo de amonio (CTAB) or polyvinylpyrrolidone (PVP).
Wherein, described NiO nano flake mesopore is evenly distributed, and the diameter in hole is 30～40nm.
Wherein, described evenly, the diameter of the NiO nano flake of central hole structure is 300～400nm, thickness is several nm.
Wherein, the NiO of described NiO nano flake becomes cube phase, degree of crystallinity height.
Under different concentration of the present invention and temperature of reaction condition, all can obtain cube phase evenly, the NiO nano flake of central hole structure, purity height, good product quality.
The NiO nano flake even, central hole structure of the present invention's preparation not only helps opening up particular performances of NiO own and application, and helps the development and application of other new nano structure device.
The present invention is a kind of evenly, the preparation method of the nickel oxide nano flake of central hole structure, and its advantage and effect are:
(1) prepared NiO nano flake has lotus-like vesicular structure and hole is evenly distributed.
(2) prepared evenly, the NiO nano flake purity height of central hole structure, do not contain the NiO of other pattern.
(3) prepared evenly, the NiO nano flake stable performance of central hole structure, volatility not in air.
(4) technology is simple, and is low for equipment requirements, and starting material are easy to get, and expense is cheap, can produce in enormous quantities.
(4) description of drawings
Fig. 1 is even, the preparation flow figure of the NiO nano flake of central hole structure.
Fig. 2 adopt present method preparation evenly, the X-ray diffraction spectrogram of the NiO nano flake of central hole structure.
Fig. 3 adopt present method preparation evenly, the stereoscan photograph of the NiO nano flake of central hole structure.
(5) embodiment:
The present invention will be further described below in conjunction with embodiment, but be not limited only to this.
Embodiment 1
(1) with 80mL, the aqueous solution of the Nickel dichloride hexahydrate of 0.05mol/L is put into the beaker of 100mL, adds the hexadecyl brometo de amonio (CTAB) of 0.5g, behind the magnetic agitation 3h; Drip 0.8mL ammoniacal liquor, magnetic agitation 2h forms the transparent mixing solutions of light green;
(2) mixing solutions that step (1) is obtained is positioned in the teflon-lined stainless steel cauldron, and sealing is in retort furnace internal heating reaction 15h; Temperature of reaction is 150 ℃;
(3) turbid solution that step (2) is obtained filter, wash, drying, obtain the nickel hydroxide precursor;
(4) the nickel hydroxide precursor that step (3) is obtained is at 500 ℃ of roasting 2h, obtaining NiO nano flake even, central hole structure. Fig. 2 is the X ray diffracting spectrum of the NiO nano flake of central hole structure, all diffraction peaks are all well corresponding to a cube phase NiO, diffraction peak intensity is high and sharp-pointed, interpret sample degree of crystallinity height.
Embodiment 2
(1) with 80mL, the aqueous solution of the Nickel dichloride hexahydrate of 0.75mol/L is put into the beaker of 100mL, adds the polyvinylpyrrolidone (PVP) of 0.5g, behind the magnetic agitation 3h; Drip 0.8mL ammoniacal liquor, magnetic agitation 2h forms the transparent mixing solutions of light green;
(2) mixing solutions that step (1) is obtained is positioned in the teflon-lined stainless steel cauldron, and sealing is in retort furnace internal heating reaction 18h; Temperature of reaction is 120 ℃;
(3) turbid solution that step (2) is obtained filter, wash, drying, obtain the nickel hydroxide precursor;
(4) the nickel hydroxide precursor that step (3) is obtained obtains NiO nano flake even, central hole structure at 400 ℃ of roasting 3h.Fig. 3 is the scanning electron microscope collection of illustrative plates of the NiO nano flake of central hole structure, and NiO nano flake mesopore is evenly distributed, and the diameter in hole is 30～40nm; Evenly, the diameter of the NiO nano flake of central hole structure is 300～400nm, thickness is several nm.
Embodiment 3
(1) with 80mL, the aqueous solution of the Nickelous nitrate hexahydrate of 0.15mol/L is put into the beaker of 100mL, adds the polyvinylpyrrolidone (PVP) of 0.7g, behind the magnetic agitation 3h; Drip 1.0mL ammoniacal liquor, magnetic agitation 2h forms the transparent mixing solutions of light green;
(2) mixing solutions that step (1) is obtained is positioned in the teflon-lined stainless steel cauldron, and sealing is in retort furnace internal heating reaction 20h; Temperature of reaction is 80 ℃;
(3) turbid solution that step (2) is obtained filter, wash, drying, obtain the nickel hydroxide precursor;
(4) the nickel hydroxide precursor that step (3) is obtained obtains NiO nano flake even, central hole structure at 350 ℃ of roasting 4h.
Claims (6)
- One kind evenly, the preparation method of the nickel oxide nano flake of central hole structure, be characterised in that: concrete steps are as follows:(1) the nickeliferous inorganic salt solution of a certain amount of 0.05～0.15mol/L is put into beaker, add tensio-active agent, surfactant concentrations is 5g/L～10g/L, behind the magnetic agitation 3h; Dropping ammonia, the volume ratio of ammoniacal liquor and nickeliferous inorganic salt solution are 0.01: 1～0.015: 1, and magnetic agitation 0.5～2h forms the transparent mixing solutions of blue-greenish colour;(2) mixing solutions that step (1) is obtained is positioned in the teflon-lined stainless steel cauldron, and sealing is in retort furnace internal heating reaction 12～20h; Temperature of reaction is 80～150 ℃;(3) turbid solution that step (2) is obtained filter, wash, drying, obtain the nickel hydroxide precursor;(4) the nickel hydroxide precursor that step (3) is obtained obtains the nickel oxide nano flake of vesicular structure at 350～500 ℃ of roasting 2～4h.
- 2. according to claim 1 evenly, the preparation method of the nickel oxide nano flake of central hole structure, be characterised in that: described nickeliferous inorganic salt are Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate.
- 3. according to claim 1 evenly, the preparation method of the nickel oxide nano flake of central hole structure, be characterised in that: described tensio-active agent is hexadecyl brometo de amonio or polyvinylpyrrolidone.
- 4. according to claim 1 evenly, the preparation method of the nickel oxide nano flake of central hole structure, be characterised in that: described nickel oxide nano flake mesopore is evenly distributed, the diameter in hole is 30～40nm.
- 5. according to claim 1 evenly, the preparation method of the nickel oxide nano flake of central hole structure, be characterised in that: described evenly, the diameter of the nickel oxide nano flake of central hole structure is 300～400nm, thickness is several nm.
- 6. according to claim 1 evenly, the preparation method of the nickel oxide nano flake of central hole structure, be characterised in that: the nickel oxide of described nickel oxide nano flake becomes cube phase.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905904A (en) * | 2010-07-22 | 2010-12-08 | 北京航空航天大学 | Preparation method of nickel oxide microspheres consisting of lotus root-like nanosheets |
| CN102677129A (en) * | 2012-06-13 | 2012-09-19 | 西北有色金属研究院 | Ni-base NiO nanosheet array film electrode and preparation method thereof |
| CN105174320A (en) * | 2015-10-15 | 2015-12-23 | 齐鲁工业大学 | Hexagonal flake-shaped mesoporous nickel oxide and preparation method and application thereof |
| CN106186089A (en) * | 2016-07-11 | 2016-12-07 | 淮北师范大学 | A kind of preparation method with hole two-dimensional structure nickel hydroxide nano sheet |
| CN107381663A (en) * | 2017-06-16 | 2017-11-24 | 上海交通大学 | A kind of nickel oxide nano flake gas sensor and preparation method based on aluminium doping |
| 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 |
| CN108622946A (en) * | 2018-05-09 | 2018-10-09 | 华北电力大学 | Three-dimensional regular cube structure nano-nickel oxide and preparation method thereof and a kind of lithium battery |
| CN109755029A (en) * | 2019-01-31 | 2019-05-14 | 燕山大学 | A kind of preparation method of flower piece shape nano-nickel oxide |
| CN111653768A (en) * | 2020-05-25 | 2020-09-11 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| CN112062170A (en) * | 2020-09-09 | 2020-12-11 | 中国海洋大学 | Hydrothermal preparation method of nickel oxide electrochromic film with graded porous morphology and structure |
-
2009
- 2009-11-19 CN CN200910237799A patent/CN101704558A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905904A (en) * | 2010-07-22 | 2010-12-08 | 北京航空航天大学 | Preparation method of nickel oxide microspheres consisting of lotus root-like nanosheets |
| CN102677129A (en) * | 2012-06-13 | 2012-09-19 | 西北有色金属研究院 | Ni-base NiO nanosheet array film electrode and preparation method thereof |
| CN102677129B (en) * | 2012-06-13 | 2014-07-02 | 西北有色金属研究院 | Ni-base NiO nanosheet array film electrode and preparation method thereof |
| CN105174320A (en) * | 2015-10-15 | 2015-12-23 | 齐鲁工业大学 | Hexagonal flake-shaped mesoporous nickel oxide and preparation method and application thereof |
| CN105174320B (en) * | 2015-10-15 | 2017-03-22 | 齐鲁工业大学 | Hexagonal flake-shaped mesoporous nickel oxide and preparation method and application thereof |
| CN106186089A (en) * | 2016-07-11 | 2016-12-07 | 淮北师范大学 | A kind of preparation method with hole two-dimensional structure nickel hydroxide nano sheet |
| CN107381663A (en) * | 2017-06-16 | 2017-11-24 | 上海交通大学 | A kind of nickel oxide nano flake gas sensor and preparation method based on aluminium doping |
| CN107381663B (en) * | 2017-06-16 | 2019-05-14 | 上海交通大学 | A kind of nickel oxide nano flake gas sensor and preparation method based on aluminium doping |
| 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 |
| CN108622946A (en) * | 2018-05-09 | 2018-10-09 | 华北电力大学 | Three-dimensional regular cube structure nano-nickel oxide and preparation method thereof and a kind of lithium battery |
| CN109755029A (en) * | 2019-01-31 | 2019-05-14 | 燕山大学 | A kind of preparation method of flower piece shape nano-nickel oxide |
| CN111653768A (en) * | 2020-05-25 | 2020-09-11 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| CN112062170A (en) * | 2020-09-09 | 2020-12-11 | 中国海洋大学 | Hydrothermal preparation method of nickel oxide electrochromic film with graded porous morphology and structure |
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Open date: 20100512 |