CN103446965B - Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres - Google Patents
Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres Download PDFInfo
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- CN103446965B CN103446965B CN201310407123.2A CN201310407123A CN103446965B CN 103446965 B CN103446965 B CN 103446965B CN 201310407123 A CN201310407123 A CN 201310407123A CN 103446965 B CN103446965 B CN 103446965B
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- nickel
- alpha
- feooh
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- microspheres
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000004005 microsphere Substances 0.000 title abstract description 7
- 229910003145 α-Fe2O3 Inorganic materials 0.000 title abstract 4
- 238000000034 method Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 69
- 229910000859 α-Fe Inorganic materials 0.000 claims description 36
- 229910052759 nickel Inorganic materials 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 241000080590 Niso Species 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 229910002588 FeOOH Inorganic materials 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000012071 phase Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 239000003463 adsorbent Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- 239000000696 magnetic material Substances 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000012429 reaction media Substances 0.000 abstract 1
- 230000009466 transformation Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
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- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres. The preparation method comprises the following steps of firstly, carrying out low-temperature liquid phase reaction by using water as a reaction medium, FeCl3.6H2O as an iron source and urea as a precipitant under the condition of the existence of NiSO4.6H2O so as to obtain precursors, namely nickel-doped FeOOH microspheres with regular and controllable morphology; and then putting the dry nickel-doped FeOOH precursors in a muffle furnace, heating to 300-500 DEG C at a certain temperature rise rate, carrying out heat preservation for 30 minutes to two hours, decomposing nickel-doped FeOOH, and carrying out phase transformation so as to obtain the nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres. The nickel-doped FeOOH multi-level structure microspheres and the alpha-Fe2O3 multi-level structure spinous microspheres are controllable in size, morphology, structure and assembly manner and can be used as magnetic materials, catalysts for environmental purification, adsorbents and the like. The preparation method is low in reaction temperature, simple in process and convenient for industrial production.
Description
Technical field
The invention belongs to inorganic functional material preparation field, relate to a kind of nickel doped alpha-Fe
2o
3the preparation method of nanostructured, specifically, relates to a kind of nickel doped alpha-Fe
2o
3the preparation method of multilevel hierarchy thorn-like microballoon.
Background technology
α-Fe
2o
3be a kind of oxide that in the oxide of iron, character is the most stable, there is the advantages such as rich content, environmental sound, preparation cost be low, as semi-conducting material α-Fe
2o
3there is again the feature that energy gap is narrow.These make α-Fe
2o
3be widely used in a lot of field.Especially as conductor photocatalysis material and gas sensitive, α-Fe
2o
3cause increasing interest.But solar energy utilization ratio is low is a major issue of the development of restriction photocatalysis technology and application, and sensitivity low be one of major issue of restriction gas sensor exploitation.
Not enough in order to overcome these, the method for report focuses mostly at α-Fe at present
2o
3nanostructured morphologies design and ion doping two aspects.At α-Fe
2o
3nanostructured controls synthesis aspect, zero dimension (spherical particle and cubic granules etc.), one dimension (nanometer rods, nano wire, nanotube and nanobelt etc.), two dimension (as tabular, plate-like and film etc.) and three-dimensional (flower-shaped and dendrite etc.) various pattern α-Fe
2o
3the synthesis of nanostructured all has report.In ion doping, the α-Fe of many kinds of metal ions doping
2o
3all there are report (Cao Fuling etc., chemical journal, 2008,66:1405; Zhang Zhaozhi etc., artificial lens journal, 2010,39:1429; Wu Donghui etc., Materials Science and Engineering, 2006,24:101; Gajendra K.P.et al.ACS Appl.Mater.Interfaces, 2011,3:317).Lou Xiangdong etc. by 160 DEG C of hydro-thermal reaction 8h again 600 DEG C calcining 2h synthesis technique obtain Ni doping α-Fe
2o
3nano particle (Lou Xiangdong etc., electronic component and material, 2009,28:23).Chinese patent CN102321917A discloses a kind of Si doped alpha-Fe
2o
3the preparation method of super-lattice nanostructure.Chinese patent CN102610394A discloses one and prepares transient metal doped formula α-Fe by two-step reaction method
2o
3the preparation method of nano-stick array thin film.But above metal-doped α-Fe
2o
3preparation method mainly concentrate on α-Fe
2o
3on nano particle and film, seldom relate to the multilevel hierarchy α-Fe of metal ion mixing
2o
3the preparation of nano material, for improving α-Fe
2o
3the performance of nano material also has very large research space.
Summary of the invention
The object of the invention is to make up the deficiencies in the prior art, a kind of nickel doped alpha-Fe is provided
2o
3the preparation method of multilevel hierarchy thorn-like microballoon, had both considered the doping vario-property of metal ion, considered again α-Fe
2o
3the pattern of nanostructured designs, to exploitation α-Fe
2o
3the aspects such as the photocatalysis performance of nanostructured and air-sensitive performance are of great importance.
The present invention is realized by following technology path and measure, first prepares FeOOH multilevel hierarchy microballoon presoma, then obtains α-Fe by thermal decomposition and phase in version
2o
3nanostructured.Specifically:
1. by FeCl
36H
2o, NiSO
46H
2o, polyvinylpyrrolidone (PVP) and urea are dissolved in appropriate distilled water, and make its concentration be respectively 3-15mmol/L, 0.1-0.5mol/L, 5-10g/L and 0.05-0.2mol/L, solution mixes;
2. above-mentioned solution is reacted 3-24h at 80-95 DEG C, obtain the mixed liquor containing nickel doping alpha-feooh;
3. by above-mentioned containing nickel doping alpha-feooh mixed liquor take out, cooling after, centrifugal 5-10min under 2000-4000r/min rotating speed, outwell supernatant liquor, by the sediment water that obtains and ethanol repeated washing, put into 60-80 DEG C of drying box drier, after drying, obtain nickel doping alpha-feooh multilevel hierarchy thorn-like microballoon.
4. the nickel of drying doping alpha-feooh sample is warming up to 300-500 DEG C with the programming rate of 1-2 DEG C/min, then after being incubated 30min-2h, is cooled to room temperature, nickel doped alpha-Fe can be obtained
2o
3multilevel hierarchy thorn-like microballoon.
This process route has following characteristics: the nickel doped F eOOH microballoon obtained and nickel doped alpha-Fe
2o
3microballoon is the thorn-like microballoon with multilevel hierarchy assembled by nanometer burr, and morphosis is novel, namely embodies the pattern of nanostructured, dimensional effect, also combines the structure effect adulterating and bring.Not only contribute to improving its photocatalytic activity and air-sensitive performance, to exploitation α-Fe
2o
3base novel functional material is also significant.Meanwhile, the method technique is simple, and reaction condition is gentleer, prepared FeOOH multilevel hierarchy microballoon and α-Fe
2o
3the size of multilevel hierarchy micro-sphere structure, pattern, structure and assembling mode are controlled, and reaction temperature is low, has batch production feasibility.
Accompanying drawing explanation
Fig. 1 is the nickel doped alpha-Fe utilizing the method for the invention to prepare
2o
3thorn-like microballoon X-ray diffraction (XRD) collection of illustrative plates;
Fig. 2 a is the nickel doped alpha-Fe utilizing the method for the invention to prepare
2o
3sEM (SEM) photo of thorn-like microballoon;
Fig. 2 b is SEM (SEM) photo of the multiplication factor of Fig. 2 a.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail, but content of the present invention has more than and is limited to described embodiment.
Embodiment one:
1. by FeCl
36H
2o, NiSO
46H
2o, polyvinylpyrrolidone and urea are dissolved in appropriate distilled water, and make its concentration be respectively 3.7mmol/L, 0.3mol/L, 10g/L and 0.05mol/L, solution mixes;
2. above-mentioned solution is reacted 5h at 90 DEG C, obtain the mixed liquor containing nickel doping alpha-feooh;
3. by above-mentioned containing nickel doping alpha-feooh mixed liquor but after, under 4000r/min rotating speed, centrifugal 5min, outwells supernatant liquor, by the sediment water that obtains and ethanol repeated washing, put into 70 DEG C of drying boxes drier, after drying, obtain nickel doping alpha-feooh multilevel hierarchy thorn-like microballoon.
4. the nickel of drying doping alpha-feooh sample is warming up to 300 DEG C with the programming rate of 1 DEG C/min, then after being incubated 30min, is cooled to room temperature, nickel doped alpha-Fe can be obtained
2o
3multilevel hierarchy thorn-like microballoon.
Embodiment two:
1. by FeCl
36H
2o, NiSO
46H
2o, polyvinylpyrrolidone and urea are dissolved in appropriate distilled water, and make its concentration be respectively 7.4mmol/L, 0.3mol/L, 10g/L and 0.1mol/L, solution mixes;
2. above-mentioned solution is reacted 5h at 90 DEG C, obtain the mixed liquor containing nickel doping alpha-feooh;
3. by after the above-mentioned mixed liquor cooling containing nickel doping alpha-feooh, under 4000r/min rotating speed, centrifugal 5min, outwells supernatant liquor, by the sediment water that obtains and ethanol repeated washing, put into 70 DEG C of drying boxes drier, after drying, obtain nickel doping alpha-feooh multilevel hierarchy thorn-like microballoon.
4. the nickel of drying doping alpha-feooh sample is warming up to 400 DEG C with the programming rate of 1 DEG C/min, then after being incubated 30min, is cooled to room temperature, nickel doped alpha-Fe can be obtained
2o
3multilevel hierarchy thorn-like microballoon.
Embodiment three:
1. by FeCl
36H
2o, NiSO
46H
2o, polyvinylpyrrolidone and urea are dissolved in appropriate distilled water, and make its concentration be respectively 7.4mmol/L, 0.4mol/L, 10g/L and 0.2mol/L, solution mixes;
1. above-mentioned solution is reacted 12h at 90 DEG C, obtain the mixed liquor containing nickel doping alpha-feooh;
2. by after the above-mentioned mixed liquor cooling containing nickel doping alpha-feooh, under 4000r/min rotating speed, centrifugal 5min, outwells supernatant liquor, by the sediment water that obtains and ethanol repeated washing, put into 70 DEG C of drying boxes drier, after drying, obtain nickel doping alpha-feooh multilevel hierarchy thorn-like microballoon.
4. the nickel of drying doping alpha-feooh sample is warming up to 400 DEG C with the programming rate of 1 DEG C/min, then after being incubated 1h, is cooled to room temperature, nickel doped alpha-Fe can be obtained
2o
3multilevel hierarchy thorn-like microballoon.
Fig. 1 is for utilizing the Fe that described in the embodiment of the present invention one prepared by method
2o
3the XRD collection of illustrative plates of sample, the diffraction maximum in figure can turn to six side phase α-Fe according to standard card (card No.33-0664) index
2o
3diffraction maximum, in the indices of crystallographic plane mark that each diffraction maximum is corresponding and figure.In figure, diffraction peaks broadening obviously illustrates α-Fe
2o
3sample crystal grain is tiny.
α-the Fe that Fig. 2 is prepared for utilizing method described in the embodiment of the present invention one
2o
3sEM photo under sample different multiples.Can find out what sample was mainly made up of the microballoon of a large amount of 300-400nm from Fig. 2 a, domain size distribution is more even.α-Fe can be found out from Fig. 2 b multiplication factor photo
2o
3microballoon has burr shape multilevel hierarchy, is that the nanometer burr being less than 10nm by diameter assembles.
The above embodiment is the present invention's preferably embodiment; but the specific embodiment of the present invention is not restricted to the described embodiments; do not deviate from do under principle of the present invention and technical process other any change, substitute, simplification etc.; be the displacement of equivalence, all should be included within protection scope of the present invention.
Claims (1)
1. a nickel doped alpha-Fe
2o
3the preparation method of multilevel hierarchy thorn-like microballoon, is characterized in that, described method comprises the steps:
(1) by FeCl
36H
2o, NiSO
46H
2o, polyvinylpyrrolidone and urea are dissolved in appropriate distilled water, and make its concentration be respectively 3-15mmol/L, 0.1-0.5mol/L, 5-10g/L and 0.05-0.2mol/L, solution mixes;
(2) mixed solution is reacted 3-24h at 80-95 DEG C, obtain the mixed liquor containing nickel doping alpha-feooh;
(3) by after the above-mentioned mixed liquor cooling containing nickel doping alpha-feooh, centrifugal, outwell supernatant liquor, by the sediment water that obtains and ethanol repeated washing, after drying, obtain nickel doping alpha-feooh multilevel hierarchy thorn-like microballoon;
(4) nickel of drying doping alpha-feooh sample is warming up to 300-500 DEG C with the programming rate of 1-2 DEG C/min, then after being incubated 0.5-2h, is cooled to room temperature, nickel doped alpha-Fe can be obtained
2o
3multilevel hierarchy thorn-like microballoon.
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| CN108217751B (en) * | 2018-02-09 | 2020-04-24 | 青岛大学 | Preparation method of hexagonal prism α -FeOOH nanorod |
| CN109148828B (en) * | 2018-07-12 | 2020-10-27 | 华南师范大学 | Comprises cluster Co-Fe of rice straw2O3Electrode of nano composite material and preparation method thereof |
| CN110844940A (en) * | 2019-11-11 | 2020-02-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of α -ferric oxide nano material doped with nickel atoms, product and application thereof |
| CN112657555B (en) * | 2020-12-01 | 2022-06-17 | 南昌航空大学 | Monodisperse Fe-O cluster doped Ni-based metal organic framework composite photocatalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312224A (en) * | 2000-10-16 | 2001-09-12 | 童忠良 | Liquid phase synthesis process of producing nanometer iron oxide red |
| CN102161500A (en) * | 2011-02-24 | 2011-08-24 | 西北工业大学 | Preparation method of cobalt-doped zinc oxide nano-material |
| CN103232049A (en) * | 2013-03-17 | 2013-08-07 | 青岛科技大学 | Preparation method of alpha-Al2O3 cage-structure hollow microspheres |
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| WO2011069771A1 (en) * | 2009-12-09 | 2011-06-16 | Evonik Degussa Gmbh | Heat-expandable microcapsules comprising magnetic metal oxide particles |
| JP2011214144A (en) * | 2010-03-17 | 2011-10-27 | Nippon Steel Chem Co Ltd | Method for production of nickel nanoparticle |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312224A (en) * | 2000-10-16 | 2001-09-12 | 童忠良 | Liquid phase synthesis process of producing nanometer iron oxide red |
| CN102161500A (en) * | 2011-02-24 | 2011-08-24 | 西北工业大学 | Preparation method of cobalt-doped zinc oxide nano-material |
| CN103232049A (en) * | 2013-03-17 | 2013-08-07 | 青岛科技大学 | Preparation method of alpha-Al2O3 cage-structure hollow microspheres |
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Effective date of registration: 20191127 Address after: 221300, Jiangsu City, Xuzhou province Pizhou Town Industrial Park Patentee after: XUZHOU XINBEIKE ELECTRIC POWER EQUIPMENT CO., LTD. Address before: 266061 Shandong Province, Qingdao city Laoshan District Songling Road No. 99 Patentee before: Qingdao University of Science & Technology |