CN1631587A - Method for manufacturing nanometer iron - Google Patents

Method for manufacturing nanometer iron Download PDF

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Publication number
CN1631587A
CN1631587A CN 200410084285 CN200410084285A CN1631587A CN 1631587 A CN1631587 A CN 1631587A CN 200410084285 CN200410084285 CN 200410084285 CN 200410084285 A CN200410084285 A CN 200410084285A CN 1631587 A CN1631587 A CN 1631587A
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iron
solution
nanometer
irradiation
concentration
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CN 200410084285
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周瑞敏
何林锋
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN 200410084285 priority Critical patent/CN1631587A/en
Publication of CN1631587A publication Critical patent/CN1631587A/en
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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention relates to an iron super-micro particle preparation technique, belongs to radiation chemical nanometer material production technique. The technique of the invention is that: nanometer material preparation: obtain iron hydroxide colloid solution by using iron sulfate as raw material and ammonia liquor as precipitant; control the crystal core accumulating speed and the particle size by hydrophilic surface-activator polyvinyl alcohol with isopropyl alcohol as free radical scavenger and in radiation chemistry principles; develop the radiation chemical reaction by the bunch of electrons generated by industrial electron accelerator; the radiated solution produces nanometer triple iron quadoxide which deoxidated with high purity hydrogen to obtain nanometer iron powder. The advantages of the invention are that: simple technical processes, short production cycle, non-pollution, the obtained particles are of uniform diameter and finely divided. The nanometer iron produced in above ways is of higher satiating hard magnetism and coercive force which is applicable on high intensity magnetic recording material..

Description

The manufacture method of nanometer iron
Technical field
The present invention relates to a kind of preparation method of iron ultramicron, belong to radiation chemistry and make the nano material technology field.
Background technology
In recent years, because the extensive prospect of magnetic nano-particle in the reagent practical application, the preparation method of relevant magnetic nano-particle and the research of character are subjected to very big attention, aspect magnetic recording material, magnetic nano-particle is expected to replace traditional micron order magnetic, is used for the high density magnetic recording material; At biological field, be that carrier is made directed agents with it, can make the part that is gathered under the effect of medicine outside magnetic field in the body, thereby the drug therapy of high concentration is carried out in the pathology position, being particularly suitable for cancer, tuberculosis etc. has the fixedly disease of focus.
Synthetic magnetic nanoparticle with superparamagnetism is realized the evenly compound of magnetic particle and macromolecular material, and preparation has the magnetic microsphere of various functional groups, can be widely used in separation, mark and the medical diagnosis on disease of biomolecule.
Use the radiation chemistry method to prepare nano material, more widely used at present method is the gamma-rays radiation method, still, seldom has electron accelerator to prepare nano material as radiation source both at home and abroad.
Summary of the invention
The object of the present invention is to provide and adopt another kind of radiation source, the electron beam that promptly adopts high-frequency and high-voltage industrial electronic accelerator to produce comes the synthesis of nano metallic iron as radiation source method.
A kind of manufacture method of nanometer iron adopts the radiation chemistry method to prepare nano material, it is characterized in that the processing step of this method is as follows:
A) adopting ferric sulfate is raw material, and it is dissolved in the distilled water, and the concentration of iron ion is 0.005-0.02mol/100ml in the solution;
B) add hydrophilic surfactant active's polyvinyl alcohol then, its concentration is 0.4-1.0g/100ml;
C) add isopropyl alcohol again as oxidative free radical OH scavenger; Its concentration is 15-30ml/100ml, and adds ammoniacal liquor again, forms ferric hydroxide colloid solution;
D) the above-mentioned mixed solution for preparing is packed in the irradiation vessel, and charge into nitrogen, seal irradiation vessel then to get rid of the oxygen in the solution;
E) adopting high-frequency and high-voltage industrial electronic accelerator, is to carry out irradiation with different irradiation doses under ground that meter electron accelerator of 2.0MeV, 10mA in working range, and dosage range is: 100-550Kgy;
F) solution behind the irradiation is used deionized water and absolute ethanol washing repeatedly, separate with magnetic separating device, repeated multiple times is to remove unreacted iron ion and hydrophilic surfactant active's polyvinyl alcohol in the solution;
G) in vacuum drying chamber, the gained sample was carried out air drying 10-15 hour then, can obtain the nano ferriferrous oxide powder of black, with the high-purity hydrogen reduction, obtain the nanometer iron powder end again.
Mainly utilize the radiation chemistry principle among the present invention, adopt the source of ferric sulfate as iron, as precipitating reagent, form ferric hydroxide colloid solution with ammoniacal liquor, utilize electron beam that the industrial electronic accelerator produces to be gone back ortho states hydrogen H, aqueous electron e what aqueous solution ionization produced - AqDeng having the reaction of reproducibility particle and ferric hydroxide colloid, obtain nano ferriferrous oxide, reduce tri-iron tetroxide with high-purity hydrogen again, get final product nanometer iron.Add the hydrophilic surfactant active and control the growth rate of nucleus, and control the size of particle, make particle reach nanoscale.The adding of isopropyl alcohol is the scavenger as oxidative free radical OH in addition.
The advantage of the inventive method is: at normal temperatures and pressures, need not to add any catalyst, prepare nanometer iron with the electron beam method of radiating.This method technical process is simple, with short production cycle, pollution-free, and the nano iron particles particle size of preparation gained is even, good dispersion.
The specific embodiment
Now specific embodiments of the invention are described in the back:
Embodiment one: the concrete processing step of present embodiment is as follows:
A. at first, take by weighing a certain amount of ferric sulfate, it is dissolved in the distilled water, make the concentration of solution iron ion reach 0.015mol/100ml with FA1004 ware formula electronic balance;
B. add hydrophilic surface active agent polyvinyl alcohol PVA then, concentration is 0.8g/100ml;
C. add the scavenger of isopropyl alcohol IPA as oxidative free radical OH again, concentration is 30ml/100ml, and adds ammoniacal liquor, forms ferric hydroxide colloid solution;
D. the above-mentioned solution for preparing is packed in the irradiation vessel, charge into nitrogen, then irradiation vessel is sealed to get rid of the oxygen in the solution;
E. adopting high-frequency and high-voltage industrial electronic accelerator, is that the irradiation dose with 400-500KGy carries out irradiation under 2.0MeV, 10mA ground that meter electron accelerator in working range;
F. the solution behind the irradiation is used deionized water and absolute ethanol washing three times, separated with magnetic separation technique again, three times repeatedly, to remove unreacted iron ion and the hydrophilic surface active agent polyvinyl alcohol PVA in the solution;
G. in vacuum drying chamber, carried out air drying 12 hours then, can obtain the nano ferriferrous oxide powder of black, and then, get the nanometer iron powder end with the high-purity hydrogen reduction.
Add hydrophilic surfactant active's polyvinyl alcohol among the present invention, can carry out surface modification to particle, cover one layer of polymeric at particle surface, so not only can stablize particle and controlled the growth of particle nucleation, and have the agglomeration that high surface energy, high chemical energy, particle very easily take place because of the metallic atom particle can effectively prevent solution evaporation the time.
The gained sample fits like a glove by the peak value of the characteristic peaks in the diffracting spectrum with JCPDS standard powder diffraction card (Fe-06-0696) mutually through X-ray diffractometer XRD test.The purity that this sample nanometer iron is described is very high.
From JEM-200CX type high resolution transmission electron microscopy tem observation, visible sample particle is spherical in shape, and granular size is comparatively even.And particle diameter is distributed between the 51-58.5nm.
The analysis of laser particle diameter distribution instrument shows the particle size distribution range of nanometer iron in water between 40-80nm, and its main peak appears at 53.0nm and goes out, and this and TEM experimental result are consistent.
Thermal analysis experiment result by differential scanning thermal analyzer DSC shows that the fusing point of obtained nanometer iron is 579.8 ℃, and the fusing point of common iron is 1534 ℃.This shows that when iron reaches nanoscale very big change takes place the performance of material.
By vibration magnetometer (EGEG Princeton Applied Research Model 155) experiment, find the hysteresis curve of prepared nanometer iron overlapping be a curve, this meets the feature of single domain soft magnetic materials, in addition, can get by data computation, the specific saturation magnetization and the coercivity of sample are respectively 110emu/g, 46Oe, far above specific saturation magnetization and the coercivity of normal commercial, it is reported that commercial specific saturation magnetization and coercivity with iron is 13emu/g and 1Oe with iron.Thereby the prepared nanometer iron of the inventive method can be used for the high density magnetic recording material.

Claims (1)

1. the manufacture method of a nanometer iron adopts the radiation chemistry method to prepare nano material, it is characterized in that the processing step of this method is as follows:
A) adopting ferric sulfate is raw material, and it is dissolved in the distilled water, and the concentration of iron ion is 0.005-0.02mol/100ml in the solution;
B) add hydrophilic surfactant active's polyvinyl alcohol then, its concentration is 0.4-1.0g/100ml;
C) add the scavenger of isopropyl alcohol again as oxidative free radical OH; Its concentration is 15-30ml/100ml, and adds ammoniacal liquor again, forms ferric hydroxide colloid solution;
D) the above-mentioned mixed solution for preparing is packed in the irradiation vessel, and charge into nitrogen, seal irradiation vessel then to get rid of the oxygen in the solution;
E) adopting high-frequency and high-voltage industrial electronic accelerator, is to carry out irradiation with different irradiation doses under ground that meter electron accelerator of 2.0MeV, 10mA in working range, and the irradiation dose scope is: 100-550KGy;
F) solution behind the irradiation is used deionized water and absolute ethanol washing repeatedly, separate with magnetic separating device, repeated multiple times is to remove unreacted iron ion and hydrophilic surfactant active's polyvinyl alcohol in the solution;
G) in vacuum drying chamber, the gained sample was carried out air drying 10-15 hour then, can obtain the nano ferriferrous oxide powder of black, with the high-purity hydrogen reduction, obtain the nanometer iron powder end again.
CN 200410084285 2004-11-18 2004-11-18 Method for manufacturing nanometer iron Pending CN1631587A (en)

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CN 200410084285 CN1631587A (en) 2004-11-18 2004-11-18 Method for manufacturing nanometer iron

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100464908C (en) * 2006-07-03 2009-03-04 南京大学 Method for preparing nanometer zero-valent iron grain using improved liquid phase reduction method
CN103792117A (en) * 2014-01-20 2014-05-14 湘潭大学 Method for preparing speckles suitable for high-temperature environment
CN109576332A (en) * 2018-11-02 2019-04-05 内蒙古科技大学 A kind of method of biological reducing preparation magnetic nano ferroferric oxide
CN110368941A (en) * 2019-07-29 2019-10-25 东华理工大学 The sintering activity carbon rod and preparation method and application of deposition reduction iron nano-particle in a kind of hole
CN111392780A (en) * 2020-03-26 2020-07-10 陈宛莎 Composite oxide nano-particles capable of emitting THz frequency and preparation method thereof
CN113173604A (en) * 2020-08-05 2021-07-27 河南济源钢铁(集团)有限公司 Method for preparing nano iron and oxide thereof by taking sintering ash as raw material
CN114988356A (en) * 2022-05-31 2022-09-02 西安交通大学 Device and method for preparing hydrogen and oxygen by irradiating liquid water with electrons
CN115532263A (en) * 2022-11-03 2022-12-30 清华大学 Iron-carbon composite material and irradiation preparation method and application method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100464908C (en) * 2006-07-03 2009-03-04 南京大学 Method for preparing nanometer zero-valent iron grain using improved liquid phase reduction method
CN103792117A (en) * 2014-01-20 2014-05-14 湘潭大学 Method for preparing speckles suitable for high-temperature environment
CN103792117B (en) * 2014-01-20 2016-01-20 湘潭大学 Preparation is applicable to the method for hot environment speckle
CN109576332A (en) * 2018-11-02 2019-04-05 内蒙古科技大学 A kind of method of biological reducing preparation magnetic nano ferroferric oxide
CN109576332B (en) * 2018-11-02 2021-09-28 内蒙古科技大学 Method for preparing magnetic nano ferroferric oxide by biological reduction
CN110368941A (en) * 2019-07-29 2019-10-25 东华理工大学 The sintering activity carbon rod and preparation method and application of deposition reduction iron nano-particle in a kind of hole
CN111392780B (en) * 2020-03-26 2023-04-25 陈宛莎 Composite oxide nano particle capable of emitting THz frequency and preparation method thereof
CN111392780A (en) * 2020-03-26 2020-07-10 陈宛莎 Composite oxide nano-particles capable of emitting THz frequency and preparation method thereof
CN113173604A (en) * 2020-08-05 2021-07-27 河南济源钢铁(集团)有限公司 Method for preparing nano iron and oxide thereof by taking sintering ash as raw material
CN114988356A (en) * 2022-05-31 2022-09-02 西安交通大学 Device and method for preparing hydrogen and oxygen by irradiating liquid water with electrons
CN114988356B (en) * 2022-05-31 2023-09-19 西安交通大学 Device and method for preparing hydrogen and oxygen by electron irradiation of liquid water
CN115532263A (en) * 2022-11-03 2022-12-30 清华大学 Iron-carbon composite material and irradiation preparation method and application method thereof
CN115532263B (en) * 2022-11-03 2024-05-07 清华大学 Iron-carbon composite material and irradiation preparation method and application method thereof

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