CN102992408B - Preparation method of ferroferric oxide magnetic nanocrystal - Google Patents
Preparation method of ferroferric oxide magnetic nanocrystal Download PDFInfo
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- CN102992408B CN102992408B CN201310004392.4A CN201310004392A CN102992408B CN 102992408 B CN102992408 B CN 102992408B CN 201310004392 A CN201310004392 A CN 201310004392A CN 102992408 B CN102992408 B CN 102992408B
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- ferroferric oxide
- oxide magnetic
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- cyclodextrin
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Abstract
The invention relates to a preparation method of a ferroferric oxide magnetic nanocrystal, in particular to a method for preparing the ferroferric oxide magnetic nanocrystal of a hexagonal piece-shaped structure in a hydrothermal mode. The preparation method comprises the steps of dissolving a certain amount of beta-cyclodextrin and carbamide into deionized water, and heating reactant while performing stirring to enable the reactant to form transparent solution; and adding a certain amount of FeCl3 into the transparent solution, stirring for 30 minutes to enable the reactant to achieve full mixing, and regulating pH of the mixture into a certain range. The mixture is transferred into a hydrothermal kettle to perform hydrothermal reaction for a period of time. The synthesized ferroferric oxide magnetic nanocrystal is of the hexagonal piece-shaped structure, the dimension of the ferroferric oxide magnetic nanocrystal is 500nm, the thickness is 30-50nm, the dispersity is good, the saturation magnetization is larger than 60.0emu/g, and the coercive force is smaller than 200Oe. The ferroferric oxide magnetic nanocrystal is simple in preparation processing, low in cost and capable of performing large-scale preparation easily.
Description
Technical field
The present invention relates to a kind of preparation method of ferroferric oxide magnetic nano crystalline substance, especially a kind of hydro-thermal is prepared the method that pattern is the ferriferrous oxide nano crystalline substance of hexagonal flake structure.
Technical background
In recent years, Fe
3o
4nanocrystalline because its excellent performance has important application prospect in fields such as information storage, biosensor, pharmaceutical carrier and absorbing materials; As everyone knows, except elementary composition, the physical features such as structure, shape, size also have very large impact to the magnetic performance of material; Therefore, design has just become a very important research topic with synthesizing to have the magneticsubstance of different nanostructures and to study its magnetic property; Up to now, the researchists of region of chemistry, material supply section educational circles and Condensed Matter Physics circle are own synthesizes the various Fe with controllable appearance through having designed a lot of methods
3o
4magnetic Nano structure, although people have synthesized the different nanostructures such as nano particle, nanometer rod, nano-sheet, nano wire and nanotube, the magnetic property that controlled synthetic of On A New has the material of special construction and study it remains the difficult problem that researchists face.
Hexagonal plate Fe
3o
4nano particle is because its special structure has caused the broad interest of Chinese scholars, up to now, and at present about hexagonal plate Fe
3o
4the synthetic also rarely seen report of nano particle; Zhang etc. utilize FeCl
3as precursor, in glycerol-water mixed solvent, adopt simple polyvalent alcohol legal system for Fe with hydrazine hydrate
3o
4hexagonal nanometer sheet, mean sizes is 100-200nm, prepared Fe
3o
4hexagonal nanometer sheet is at magnetic fluid, and information storage and medical field will have potential application (Solid State Sci., 2010,12:99 – 104).Li etc. be take ferrocene as source of iron, supercritical CO
2as solvent and oxygen source, utilize supercritical fluid technology to synthesize Fe
3o
4hexagonal nanometer sheet, nanometer sheet mean diameter is 200nm, mean thickness is 20-30nm(J. Am. Chem. Soc., 2010,132:12540 – 12541); Zhou etc. are usingd citric acid, sodium-acetate and sodium hypophosphite as additive, utilize microwave assisted synthesizing method to synthesize the Fe that the average length of side is 80nm
3o
4hexagonal nanometer sheet (Chem. Lett., 2005,34:240 – 241), yet there are no and utilize hydrothermal method to synthesize Fe
3o
4the report of hexagonal nanometer sheet.
Summary of the invention
The present invention relates to a kind of preparation method of ferroferric oxide magnetic nano crystalline substance, especially a kind of hydro-thermal is prepared the method that pattern is the ferriferrous oxide nano crystalline substance of hexagonal flake structure.
The present invention realizes by following steps:
Beta-cyclodextrin and urea are dissolved in deionized water, and the mass ratio of beta-cyclodextrin and urea is 0.75 ~ 2.5: reacting by heating thing while stirring in dissolution process, makes it to form clear solution; Add FeCl
3precursor in above-mentioned clear solution, FeCl
3with beta-cyclodextrin mass ratio be 1:4 ~ 10, being stirred to reactant fully mixes, regulate afterwards mixture pH value to 9-11, mixture is proceeded to 180-200 ℃ of hydro-thermal reaction 2-4 h in water heating kettle, after reaction finishes, water heating kettle is naturally cooled to room temperature, with magnet, collect product, distilled water wash 2-3 time, the ferriferrous oxide nano that obtains hexagonal flake structure is brilliant.
Described Heating temperature is 40 ~ 60 ℃.
The purity of product and crystalline structure are by X-ray diffraction (XRD, instrument model: RegakuD/Max, CuK α is X source, λ=0.15406nm), by transmission electron microscope (TEM, instrument model: Philips Tecnai-12) to the pattern of product and microstructure analysis, magnetic property characterizes (VSM, instrument model by vibrating sample magnetometer; The HH-15 of Nanjing University type).
Accompanying drawing explanation
The Fe that Fig. 1 is prepared according to embodiment 1 condition
3o
4the XRD spectra of nanoparticle; Can find out, the sample of preparing by present method is Fe
3o
4pure phase;
The Fe that Fig. 2 is prepared according to embodiment 1 condition
3o
4the TEM photo of nanoparticle; Prepared Fe
3o
4nanocrystalline pattern is hexagonal flake structure, is of a size of 200-500 nm, and thickness is 30-50 nm;
The Fe that Fig. 3 is prepared according to embodiment 1 condition
3o
4curve of Magnetic Hysteresis Loop under nanoparticle room temperature condition; Prepared Fe
3o
4saturation magnetization is greater than 60.0 emu/g, and coercive force is less than 200Oe.
embodiment 1
The beta-cyclodextrin of 1.42 g and 1.20g urea are dissolved in deionized water, and in whipping process, 50 ℃ of reacting by heating things, make it to form clear solution; The FeCl that adds 0.27g
3precursor is in above-mentioned clear solution, stir 30min, reactant is fully mixed, regulate afterwards mixture pH value to 10, mixture is proceeded to 200 ℃ of hydro-thermal reaction 2 h in water heating kettle, after reaction finishes, water heating kettle is naturally cooled to room temperature, with magnet, collect product, distilled water wash 2-3 time, the ferriferrous oxide nano that obtains hexagonal flake structure is brilliant.
embodiment 2
The beta-cyclodextrin of 2.27 g and 1.20g urea are dissolved in deionized water, and in whipping process, 60 ℃ of reacting by heating things, make it to form clear solution, add the FeCl of 0.27g
3precursor is in above-mentioned solution, stir 30min, reactant is fully mixed, regulate afterwards mixture pH value to 11, mixture is proceeded to 180 ℃ of hydro-thermal reaction 4h in water heating kettle, after reaction finishes, water heating kettle is naturally cooled to room temperature, with magnet, collect product, distilled water wash 2-3 time, the ferriferrous oxide nano that obtains hexagonal flake structure is brilliant.
embodiment 3
The beta-cyclodextrin of 1.42 g and 1.50g urea are dissolved in deionized water, and in whipping process, 40 ℃ of reacting by heating things, make it to form clear solution, add the FeCl of 0.27g
3precursor is in above-mentioned solution, stir 30min, reactant is fully mixed, regulate afterwards mixture pH value to 9, mixture is proceeded to 200 ℃ of hydro-thermal reaction 2h in water heating kettle, after reaction finishes, water heating kettle is naturally cooled to room temperature, with magnet, collect product, distilled water wash 2-3 time, the ferriferrous oxide nano that obtains hexagonal flake structure is brilliant.
Claims (2)
1. the preparation method of a ferroferric oxide magnetic nano crystalline substance, described nanocrystalline pattern is hexagonal flake structure, be of a size of 200-500 nm, thickness is 30-50 nm, saturation magnetization is greater than 60.0 emu/g, and coercive force is less than 200Oe, it is characterized in that comprising the steps: beta-cyclodextrin and urea are dissolved in deionized water, the mass ratio of beta-cyclodextrin and urea is 0.75 ~ 2.5: reacting by heating thing while stirring in dissolution process, makes it to form clear solution; Add FeCl
3precursor in above-mentioned clear solution, FeCl
3with beta-cyclodextrin mass ratio be 1:4 ~ 10, being stirred to reactant fully mixes, regulate afterwards mixture pH value to 9-11, mixture is proceeded to 180-200 ℃ of hydro-thermal reaction 2-4 h in water heating kettle, after reaction finishes, water heating kettle is naturally cooled to room temperature, with magnet, collect product, distilled water wash 2-3 time, the ferriferrous oxide nano that obtains hexagonal flake structure is brilliant.
2. the preparation method of a kind of ferroferric oxide magnetic nano crystalline substance as claimed in claim 1, is characterized in that: described Heating temperature is 40 ~ 60 ℃.
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| CN103395845B (en) * | 2013-08-06 | 2015-02-25 | 肇庆学院 | Magnetic nanoparticle for rapid screening of estradiol |
| CN106587167B (en) * | 2016-12-15 | 2018-01-26 | 陕西科技大学 | A kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials |
| CN107162063B (en) * | 2017-07-05 | 2018-08-17 | 合肥学院 | A kind of size tunable Fe3O4The preparation method of nano powder and its application in water-oil separating |
| CN108190967B (en) * | 2018-01-24 | 2020-03-27 | 合肥学院 | Ferroferric oxide nanosheet and preparation method thereof |
Citations (1)
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| CN102424427A (en) * | 2011-09-06 | 2012-04-25 | 合肥学院 | Simple preparation method of magnetic Fe3O4 nano-material |
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| CN102424427A (en) * | 2011-09-06 | 2012-04-25 | 合肥学院 | Simple preparation method of magnetic Fe3O4 nano-material |
Non-Patent Citations (4)
| Title |
|---|
| An easy fabrication of monodisperese oleic acid-coated Fe3O4 nanoparticals;Di Li等;《Materials Letters》;20100810;摘要 * |
| Di Li等.An easy fabrication of monodisperese oleic acid-coated Fe3O4 nanoparticals.《Materials Letters》.2010,摘要. |
| 刘奕等.磁性Fe3O4六方片状晶体和单晶纳米棒的水热合成.《人工晶体学报》.2005,摘要. |
| 磁性Fe3O4六方片状晶体和单晶纳米棒的水热合成;刘奕等;《人工晶体学报》;20051031;摘要 * |
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