CN106365208B - One kind prepares spherical Fe3O4The method of nano-magnetic powder particle - Google Patents
One kind prepares spherical Fe3O4The method of nano-magnetic powder particle Download PDFInfo
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- CN106365208B CN106365208B CN201610817714.0A CN201610817714A CN106365208B CN 106365208 B CN106365208 B CN 106365208B CN 201610817714 A CN201610817714 A CN 201610817714A CN 106365208 B CN106365208 B CN 106365208B
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- 239000002245 particle Substances 0.000 title claims abstract description 39
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 30
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000009413 insulation Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 15
- 230000005291 magnetic effect Effects 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000005415 magnetization Effects 0.000 description 5
- 239000011858 nanopowder Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- 239000011324 bead Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000003780 insertion Methods 0.000 description 3
- 230000037431 insertion Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/72—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables
- G01N27/82—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws
- G01N27/83—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws by investigating stray magnetic fields
- G01N27/84—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws by investigating stray magnetic fields by applying magnetic powder or magnetic ink
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses one kind to prepare spherical Fe3O4The method of nano-magnetic powder particle, including step：Weigh FeCl3•6H2O and NaAc 3H2O room temperatures in solvent；In stainless steel cauldron, 195 205 DEG C of 10 15h of insulation are calorified；Cool down, after separation of solid and liquid, wash and dry obtained spherical Fe3O4Magnetic powder particle；It is described to be cooled to air cooling or water cooling or frozen water cooling.The spherical Fe of different-diameter size is prepared by solvent thermal reaction the invention provides one kind3O4Nano-magnetic powder particle, the present invention change in the prior art generally using furnace cooling by the way of, instead air cooling, water cooling or frozen water cooling mode, can but obtain the less spherical Fe of particle diameter3O4Nano-magnetic powder particle, and the mode that under equal conditions frozen water cools down is smaller compared with the particle that air cooling obtains, and is easy to mass produce, obtained Fe3O4Nano-magnetic powder particle is free of any other impurity, has the wide prospect of marketing.
Description
Technical field
The present invention relates to one kind to prepare the spherical Fe of different-diameter size3O4The method of nano-magnetic powder particle, belongs to Magnetic testing
With the preparation field of material.
Background technology
Magnetic testing is after being magnetized using ferromagnetic workpiece, due to the presence of discontinuity so that workpiece surface and near
The line of magnetic induction on surface occurs local distortion and produces stray field, and absorption is applied to the magnetic of workpiece surface, therefore magnetic conduct
The sensor of stray field, detect discontinuous position, size and Orientation is particularly important.Usual magnetic should be by different shape group
Into spherical magnetic can provide good mobility, can jump towards aggregation at stray field.Generally, different-diameter size
Spherical Fe3O4Magnetic powder particle preparation method is mainly by controlling the concentration of primitive reaction thing, controlling instead using solvent thermal reaction
The time answered realizes that these methods need to consume more material, add energy consumption, and cost is higher, and it is big to be unfavorable for different-diameter
Small spherical Fe3O4The large-scale production of magnetic powder particle.
Chinese patent CN1645530A discloses a kind of method for synthesizing serial monodisperse ferrate nanometer magnetic bead, and it includes
Following steps：Soluble ferric ion salt is added in ethylene glycol solution, is made into 0.05-0.4mol/l settled solution
In, then the solution is put into airtight heating device, solvent thermal reaction, heat time 8- are carried out under the conditions of 200-300 DEG C
72 hours, products therefrom is washed with deionized, in 40-80 DEG C of drying, single dispersing Fe is made3O4Nanometer magnetic bead.This system
Standby different-diameter size Fe3O4The main method of nanosphere is by controlling to adjust the heating furnace reaction time, obtaining different size
Fe3O4Nanometer magnetic bead, the energy consumption that this method needs is higher, and the reaction time is longer, uneconomical environmental protection.Chinese patent
CN101381109A discloses spherical Fe3O4The preparation method of nano-powder, this method are characterized mainly in that：Configure ferrous salt
The aqueous solution, heat, stirring, adjust pH value 4.0-8.0, then add equipped with gas distributor reactor in, stirring, be passed through
NH is added after air 5-15min4NO2Or NaNO2, adjust reaction pH value be 8-14 after, react 1.0-5.0h, separation of solid and liquid
Afterwards, it is washed with deionized, dries and spherical Fe is made3O4Nano-powder.But this method needs to add catalyst n H4NO2Or
NaNO2, prepared spherical Fe3O4A diameter of 100nm of nano-powder or so, it is unfavorable for preparing the spherical of different-diameter size
Fe3O4Nano-powder.
The content of the invention
The invention provides one kind to prepare spherical Fe3O4Nano-magnetic powder preparation method of granules, raw material of the present invention are easy to get, reaction
Time is short, reduces the energy consumption in course of reaction, and the present invention proposes one kind and is different from the prior art mainly by controlling original
The concentration of beginning reactant, extend the reaction time to regulate and control spherical Fe3O4The diameter of magnetic powder particle it is new prepare it is spherical
Fe3O4The method of nano-magnetic powder particle.
One kind of the present invention prepares spherical Fe3O4The method of nano-magnetic powder particle, comprises the steps：
(1) 1.8~3.6gFeCl is weighed3·6H2O and 6~12gNaAc3H2O is in solvent；
(2) step (1) resulting solution is stirred at room temperature；
(3) by step (2) resulting solution in stainless steel cauldron, 195-205 DEG C of insulation 10-15h is calorified；
(4) reaction solution is cooled down, after separation of solid and liquid, be washed with deionized 2~5 times, dried and spherical Fe is made3O4Magnetic
Powder particles；It is described to be cooled to air cooling or water cooling or frozen water cooling.
Preferably, one kind described above prepares spherical Fe3O4In the method for nano-magnetic powder particle, the solvent is ethylene glycol.
Preferably, one kind described above prepares spherical Fe3O4In the method for nano-magnetic powder particle, in the step (2)
Speed is stirred at room temperature as 2000~2500 revs/min, stirs 25-35min.
Preferably, one kind described above prepares spherical Fe3O4In the method for nano-magnetic powder particle, add in the step (3)
Heat is incubated 12h in 200 DEG C.
Preferably, one kind described above prepares spherical Fe3O4In the method for nano-magnetic powder particle, done in the step (4)
Dry is in 45~50 DEG C of dry 8-12h.
The spherical Fe of different-diameter size is prepared by solvent thermal reaction the invention provides one kind3O4Nano-magnetic powder particle, can
Reached using the type of cooling different in course of reaction and prepare spherical Fe3O4The requirement of nano-magnetic powder particle diameter size, and
The present invention change in the prior art generally using furnace cooling by the way of, instead air cooling, water cooling or frozen water cooling mode,
But the less spherical Fe of particle diameter can be obtained3O4Nano-magnetic powder particle, and under equal conditions the mode of frozen water cooling obtains compared with air cooling
The particle arrived is smaller, and its saturation magnetization is also higher；Meanwhile preparation process of the present invention is convenient, preparation condition is simple, consumption
Resource is few, and cost is low, environmentally safe without any additive such as catalyst etc. and large-scale precision instrument, is easy to extensive
Production, obtained Fe3O4Nano-magnetic powder particle is free of any other impurity, has the wide prospect of marketing.
Brief description of the drawings
Fig. 1 is comparative example 1, embodiment 1, in embodiment 2 as heating furnace cools down, cools down three in cooling, frozen water in air
The XRD diffraction patterns that the kind type of cooling obtains, wherein (a) is as heating furnace cools down, (b) is to be cooled down in air, cold in (c) frozen water
But, the spherical Fe that as can be seen from the figure prepared by three kinds of types of cooling3O4The XRD diffraction of magnetic powder particle meets card JCPDS
Card no.85-1436, it is spinel structure, crystallization quality is preferable, the diffraction maximum and Fe occurred3O4Diffraction maximum it is consistent,
Illustrate that prepared powder is Fe3O4Magnetic is single-phase, without any impurity phase；
Fig. 2 is that the SEM obtained by comparative example 1 cools down with heating furnace schemes, wherein insertion figure is the SEM figures of multiplication factor,
As can be seen from the figure prepared spherical Fe3O4Nano-magnetic powder particle diameter is in 700nm or so；
Fig. 3 is the SEM figures obtained by being cooled down in the air of embodiment 1, wherein insertion figure is the SEM figures of multiplication factor, from figure
In it can be seen that prepared spherical Fe3O4Magnetic powder particle diameter is in 600nm or so；
Fig. 4 is the SEM figures obtained by being cooled down in the frozen water of embodiment 2, wherein insertion figure is the SEM figures of multiplication factor, from figure
In it can be seen that prepared spherical Fe3O4Nano-magnetic powder particle diameter is in 500nm or so；
Fig. 5 is comparative example 1, embodiment 1, in embodiment 2 as heating furnace cools down, cools down three in cooling, frozen water in air
The VSM collection of illustrative plates that kind of the type of cooling obtains, wherein (a)~(c) correspond to respectively with heating furnace cools down, in air in cooling, frozen water
Cooling, it can be seen that the spherical Fe that three kinds of types of cooling obtain3O4Nano-magnetic powder saturation magnetization is respectively
82.6193emu/g、97.8481emu/g、99.033emu/g。
Embodiment
Following embodiments are further explanations for present invention using as the explaination to the technology of the present invention content, but
The present invention substantive content be not limited in described in following embodiments, one of ordinary skill in the art can with and should know appoint
What simple change or replacement based on true spirit all should belong to protection domain of the presently claimed invention.
Comparative example 1
Weigh 3.6gFeCl3·6H2O and 12gNaAC3H2O is dissolved in 90ml ethylene glycol solutions, 2000-2500 turns/
30min is stirred at room temperature under conditions of minute, then pours into solution in the stainless steel cauldron of 150ml polytetrafluoroethyllining linings,
200 DEG C of insulation 12h of heating, reactor furnace cooling after separation of solid and liquid, is washed with deionized 2-5 times, 40-45 DEG C of condition
Lower dry 12h, it is about 700nmFe that can obtain diameter3O4Magnetic powder particle.
Embodiment 1
Weigh 3.6gFeCl3·6H2O and 12gNaAC3H2O is dissolved in 90ml ethylene glycol solutions, 2000-2500 turns/
30min is stirred at room temperature under conditions of minute, then pours into solution in the stainless steel cauldron of 150ml polytetrafluoroethyllining linings,
200 DEG C of insulation 12h of heating, reactor is cooled down in atmosphere, after separation of solid and liquid, is washed with deionized 2-5 times, 40-45 DEG C
Under the conditions of dry 12h, it is about 600nmFe that can obtain diameter3O4Magnetic powder particle.
Embodiment 2
Weigh 3.6gFeCl3·6H2O and 12gNaAC3H2O is dissolved in 90ml ethylene glycol solutions, 2000-2500 turns/
30min is stirred at room temperature under conditions of minute, then pours into solution in the stainless steel cauldron of 150ml polytetrafluoroethyllining linings,
200 DEG C of insulation 12h of heating, reactor is cooled down in frozen water, after separation of solid and liquid, is washed with deionized 2-5 times, 40-45 DEG C
Under the conditions of dry 12h, it is about 500nmFe that can obtain diameter3O4Magnetic powder particle.
Comparative example 2
Weigh 1.8gFeCl3·6H2O and 6gNaAC3H2O is dissolved in 90ml ethylene glycol solutions, 2000-2500 turns/
30min is stirred at room temperature under conditions of minute, then pours into solution in the stainless steel cauldron of 150ml polytetrafluoroethyllining linings,
200 DEG C of insulation 12h of heating, by reactor as heating furnace cools down, after separation of solid and liquid, are washed with deionized 2-5 times, 0-45 DEG C
Under the conditions of dry 12h, Fe of the diameter in 350nm or so can be obtained3O4Magnetic powder particle, saturation magnetization 84.728emu/g.
Embodiment 3
Weigh 1.8gFeCl3·6H2O and 6gNaAC3H2O is dissolved in 90ml ethylene glycol solutions, 2000-2500 turns/
30min is stirred at room temperature under conditions of minute, then pours into solution in the stainless steel cauldron of 150ml polytetrafluoroethyllining linings,
200 DEG C of insulation 12h of heating, reactor is cooled down (remove out heating furnace) respectively, after separation of solid and liquid, be washed with deionized water in atmosphere
Wash 2-5 times, 12h is dried under the conditions of 40-45 DEG C, Fe of the diameter in 290nm or so can be obtained3O4Magnetic powder particle, saturation magnetization are
88.457emu/g。
Embodiment 4
Weigh 1.8gFeCl3·6H2O and 6gNaAC3H2O is dissolved in 90ml ethylene glycol solutions, 2000-2500 turns/
30min is stirred at room temperature under conditions of minute, then pours into solution in the stainless steel cauldron of 150ml polytetrafluoroethyllining linings,
200 DEG C of insulation 12h of heating, reactor is cooled down, after separation of solid and liquid, be washed with deionized 2-5 times, 40- in frozen water respectively
12h is dried under the conditions of 45 DEG C, Fe of the diameter in 200nm or so can be obtained3O4Magnetic powder particle, saturation magnetization 90.651emu/
g。
Claims (3)
1. one kind prepares spherical Fe3O4The method of nano-magnetic powder particle, comprises the steps：
（1）Weigh 1.8 ~ 3.6gFeCl3•6H2O and 6 ~ 12gNaAc 3H2O is in solvent；
（2）Step is stirred at room temperature（1）Resulting solution；Speed is stirred at room temperature as 2000 ~ 2500 revs/min, stirs 25-35min；
（3）By step（2）Resulting solution calorifies 200 DEG C of insulation 12h in stainless steel cauldron；
（4）Reaction solution is cooled down, after separation of solid and liquid, is washed with deionized 2 ~ 5 times, dries and spherical Fe is made3O4Magnetic
Grain；It is described to be cooled to air cooling or water cooling or frozen water cooling.
2. spherical Fe is prepared as claimed in claim 13O4The method of nano-magnetic powder particle, it is characterised in that the solvent is second two
Alcohol.
3. spherical Fe is prepared as claimed in claim 13O4The method of nano-magnetic powder particle, it is characterised in that the step（4）In
Drying is in 45 ~ 50 DEG C of dry 8-12h.
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| CN109095510A (en) * | 2018-09-14 | 2018-12-28 | 江苏省家禽科学研究所 | Ferroferric oxide nano granules and preparation method thereof and the application in inhibition salmonella proliferation |
| CN109502653A (en) * | 2018-12-10 | 2019-03-22 | 南京邮电大学 | One kind having flower-shaped Core-shell Structure Nanoparticles and preparation method thereof |
| CN109777396B (en) * | 2019-03-06 | 2022-05-31 | 安徽省特种设备检测院 | Phosphorescent magnetic powder, preparation method thereof and phosphorescent magnetic powder detection liquid |
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| CN105883934A (en) * | 2016-04-18 | 2016-08-24 | 吉林师范大学 | Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres |
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| Title |
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| "醋酸钠诱导的空心Fe3O4磁粒制备及表征";贺全国等;《功能材料》;20151030;第46卷(第20期);第20145页第4-5段以及图1（a） * |
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