CN105600835B - A kind of magnanimity prepares Fe3O4The method of nanometer rods - Google Patents
A kind of magnanimity prepares Fe3O4The method of nanometer rods Download PDFInfo
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- CN105600835B CN105600835B CN201610207678.6A CN201610207678A CN105600835B CN 105600835 B CN105600835 B CN 105600835B CN 201610207678 A CN201610207678 A CN 201610207678A CN 105600835 B CN105600835 B CN 105600835B
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- 238000000034 method Methods 0.000 title claims abstract description 22
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910052925 anhydrite Inorganic materials 0.000 claims abstract description 22
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 19
- 238000006722 reduction reaction Methods 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 229910052603 melanterite Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 26
- 238000013019 agitation Methods 0.000 claims description 12
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 9
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000007790 solid phase Substances 0.000 claims description 8
- 229910001626 barium chloride Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 5
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000011858 nanopowder Substances 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 229910006540 α-FeOOH Inorganic materials 0.000 abstract description 2
- 229910002588 FeOOH Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005662 electromechanics Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 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
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- 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)
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- 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
Abstract
A kind of magnanimity prepares Fe3O4The method of nanometer rods, is related to technical field of nano material.By FeSO4·7H2O is dissolved in distilled water, adds CaSO4·2H2Quick Oxidation reaction is carried out after obtaining suspension, regulation pH value to 7~14 through ultrasonic disperse after O, then filters, dry acquisition α FeOOH/CaSO4·2H2O presomas；α‑FeOOH/CaSO4·2H2O presomas carry out reduction reaction under reducibility gas atmosphere, obtain Fe3O4@CaSO4Composite nano powder, then obtains Fe by post processing3O4Nanometer rods.Whole preparation system is easily built, easy to operate, condition is easily-controllable, with low cost, product constitutes easily-controllable, particle size and is evenly distributed, is difficult to reunite, is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to technical field of nano material, it is specifically related to a kind of magnanimity and prepares Fe3O4The method of nanometer rods.
Background technology
Ferroso-ferric oxide (Fe3O4) nanometer rods are a kind of functional materials of function admirable, be widely used in coating, plastics,
The fields such as rubber, ceramics, glass, cosmetics, auxiliary pharmaceutical adjuvant, are the second largest inorganic pigments for being only second to titanium dioxide.In addition, it
It is also act as preparing various ferritic raw materials, catalyst, polishing agent, magnetic fluid, magnetic recording material, gas sensor etc..With
Fe3O4Soft magnetic ferrite for Main Ingredients and Appearance and the magnetic element being made up of it are that a class applies extremely extensive function
Material and basic device, its application be related to electronics, information, electromechanics, automobile, metallurgy, space flight and aviation, traffic and transportation system,
The fields such as engineering, biology, medical science.
Both at home and abroad it has been reported that many on Fe3O4The preparation method of nanometer rods, mainly includes the hydro-thermal method precipitation method, molten
Glue-gel method, microemulsion method, hydro-thermal and solvent-thermal method, thermal decomposition method, method of electrostatic spinning and solid phase reduction method.Relative to solid phase
Reducing process, the product thermal stability that other method is prepared is good, and crystallinity is high, but is generally difficult to carry out actual scale
Production.And solid phase reduction method needs the aftertreatment technologys such as calcining, and obtained product purity is relatively low.
The content of the invention
In order to overcome drawbacks described above present in prior art, object of the present invention is to provide a kind of preparation of magnanimity
Fe3O4The method of nanometer rods, preparation technology is simple, cost is low, be adapted to industrialization continuously produces, and product purity is high.
To realize the purpose, present invention employs following technical scheme：
A kind of magnanimity prepares Fe3O4The method of nanometer rods, step is as follows：
Step 1, alpha-feooh/CaSO is prepared4·2H2O presomas
First by FeSO4·7H2O is dissolved in distilled water, adds CaSO4·2H2Suspension is obtained through ultrasonic disperse after O, is adjusted
PH value is saved to progress Quick Oxidation reaction after 7~14, then filters, dry acquisition alpha-feooh/CaSO4·2H2O presomas；
Step 2, solid phase reduction reaction prepares Fe3O4Nanometer rods
α-FeOOH/CaSO4·2H2O presomas carry out reduction reaction under reducibility gas atmosphere, obtain Fe3O4@CaSO4
Composite nano powder, then obtains Fe by post processing3O4Nanometer rods.
As the further improvement of above-mentioned preparation method, FeSO in the suspension of step 14·7H2O、CaSO4·2H2O's
Mass concentration is followed successively by 1~27g/L, 1~20g/L.Drying temperature is 60~100 DEG C in step 1, and drying time is 2~6h.Step
The reaction temperature of reduction reaction is 400~600 DEG C in rapid 2, and the reaction time is 1~4h.Post processing is by Fe in step 23O4@
CaSO4It is slowly added into appropriate BaCl2In solution, stirring obtains Fe3O4And BaSO4Mixed solution, then through being cleaned by ultrasonic and magnetic point
From obtaining Fe3O4Nanometer rods.By Fe3O4@CaSO4It is added to BaCl2Whipping temp is 50~100 DEG C after solution, and mixing time is 1
~3h.
The present invention is shown in certain mass CaSO by a series of4The Fe obtained in template reaction system3O4Nanometer
Rod has narrower particle size distribution, higher draw ratio and the features such as stronger ferromagnetism.
Compared with prior art, beneficial effects of the present invention are shown：
1st, the present invention is realized by alpha-feooh/CaSO4·2H2O is presoma, then by Magneto separate at a certain temperature
Quickly obtain Fe3O4Nanometer rods.The Fe of preparation3O4Nanometer rods have preferably water-soluble, good biocompatibility, high absorption
Property, excellent catalysis and magnetic performance, can apply in magnetic resonance imaging, data storage, medicine and gene target, cell point
From and sewage disposal in terms of, have more wide application prospect.
2nd, present invention process is simple, and whole preparation system is easily built, easy to operate, condition is easily-controllable, with low cost, product
Easily-controllable, particle size is constituted to be evenly distributed, be difficult to reunite, be suitable for large-scale industrial production.Made using conventional soluble molysite
For reactant, the accessory substance produced in preparation process is few, and environmental pollution is smaller, is a kind of environment-friendly type synthesis technique.
Brief description of the drawings
Fig. 1 (a) is the XRD of the products therefrom of embodiment 1.
Fig. 1 (b) is the EDS spectrograms of the products therefrom of embodiment 1.
Fig. 2 (a) schemes for the TEM of the products therefrom of embodiment 1.
Fig. 2 (b) schemes for the HRTEM of the products therefrom of embodiment 1.
Fig. 2 (c) is the XRD spectra of product before and after post processing.
Fig. 3 is the room temperature hysteresis curve of product before and after post processing.
Fig. 4 collects spectrogram for the XRD that embodiment 1~4 prepares product.
Embodiment
With reference to embodiments and accompanying drawing is described in further detail to the present invention.
(the FeSO of embodiment 14·7H2O and CaSO4·2H2O weight ratio is 2：1)
Step 1, alpha-feooh/CaSO is prepared4·2H2O presomas
(1) by 2g FeSO4·7H2O is dissolved in 100mL distilled water, and magnetic agitation is allowed to abundant in 2 minutes at room temperature
Dissolving obtains solution a.
(2) again by 1g CaSO4·2H2O solution is slowly added into solution a, is continued magnetic agitation and is obtained within 3 minutes in palm fibre
Red suspension b.
(3) a small amount of ammoniacal liquor is added dropwise, regulation suspension b pH value is to 10, and it is in auburn solution c to obtain.
(4) solution c is filtered, then can obtains alpha-feooh/CaSO in 100 DEG C of dry 2h in an oven4·2H2Before O
Drive body.
Step 2, solid phase reduction reaction prepares Fe3O4@CaSO4, post-process and obtain Fe3O4Nanometer rods
(1) by a certain amount of alpha-feooh/CaSO4·2H2O presomas are put into burning boat, then are placed in boat is burnt in tube furnace,
Reduction reaction is carried out in a hydrogen atmosphere, and reaction temperature is 550 DEG C, and the reaction time is 1h.Then under reducing atmosphere, it is naturally cold
But the Fe in black solid state powder is obtained afterwards3O4@CaSO4Composite granule.
(2) by Fe3O4@CaSO4It is slowly added into BaCl2In solution, magnetic agitation 1h obtains being in grey black at 100 DEG C
Fe3O4And BaSO4Mixed solution.
(3) again by Fe3O4And BaSO4Mixed solution is cleaned by ultrasonic and Magneto separate, so as to obtain Fe3O4Nanometer rods.
Fig. 1 (a), Fig. 1 (b) are followed successively by XRD, EDS spectrogram of the products therefrom of embodiment 1, the Fe with standard3O4Spectrogram
(JCPDS：76-1849) compared to that can obtain, products therefrom is high-purity Fe3O4.The product prepared from EDS power spectrums it can be seen from the figure that
In only contain Fe elements and O elements, do not contain other elements, further demonstrate that the product be high-purity Fe3O4Nanometer rods.In addition,
Granularity is carried out with Nano measurer analysis softwares to understand products therefrom Fe after statistical analysis3O4The size of nanometer rods is
200nm or so.
Fig. 2 (a) and Fig. 2 (b) are followed successively by TEM and the HRTEM figure of the products therefrom of embodiment 1, by Tu Ke get：The form of product
To be spherical, and crystallization degree is high, good dispersion, the diameter about 200nm of particle；Each particle is monocrystalline, by (311) and
(222) interplanar distance further confirms that obtained product is Fe3O4.Fig. 2 (c) is the XRD spectra of product before and after post processing, by scheming
As can be seen that products therefrom is pure Fe after post processing3O4Nanometer rods, then before processing be mainly Fe3O4@CaSO4。
Fig. 3 is the room temperature hysteresis curve of product before and after post processing, as seen from the figure, product Fe before post processing3O4@CaSO4
Saturation magnetization 41emu/g, product Fe3O4 saturation magnetization is about 71emu/g after post processing, is shown excellent
Magnetic property.
(the FeSO of embodiment 24·7H2O and CaSO4·2H2O weight ratio is 1：1)
Step 1, alpha-feooh/CaSO is prepared4·2H2O presomas
(1) by 2g FeSO4·7H2O is dissolved in 100mL distilled water, and magnetic agitation is allowed to abundant in 3 minutes at room temperature
Dissolving obtains solution a.
(2) again by 2g CaSO4·2H2O solution is slowly added into solution a, is continued magnetic agitation and is obtained within 2 minutes in palm fibre
Red suspension b.
(3) a small amount of ammoniacal liquor is added dropwise, regulation suspension b pH value is to 7, and it is in auburn solution c to obtain.
(4) solution c is filtered, then can obtains alpha-feooh/CaSO in 60 DEG C of dry 6h in an oven4·2H2O forerunner
Body.
Step 2, solid phase reduction reaction prepares Fe3O4@CaSO4, post-process and obtain Fe3O4Nanometer rods
(1) by a certain amount of alpha-feooh/CaSO4·2H2O presomas are put into burning boat, then are placed in boat is burnt in tube furnace,
Reduction reaction is carried out in a hydrogen atmosphere, and reaction temperature is 400 DEG C, and the reaction time is 4h.Then under reducing atmosphere, it is naturally cold
But the Fe in black solid state powder is obtained afterwards3O4@CaSO4Composite granule.
(2) by Fe3O4@CaSO4It is slowly added into BaCl2In solution, magnetic agitation 2h is obtained in grey black at 80 DEG C
Fe3O4And BaSO4Mixed solution.
(3) again by Fe3O4And BaSO4Mixed solution is cleaned by ultrasonic and Magneto separate, so as to obtain Fe3O4Nanometer rods.
(the FeSO of embodiment 34·7H2O and CaSO4·2H2O weight ratio is 1：2)
Step 1, alpha-feooh/CaSO is prepared4·2H2O presomas
(1) by 1g FeSO4·7H2O is dissolved in 100mL distilled water, and magnetic agitation is allowed to abundant in 1 minute at room temperature
Dissolving obtains solution a.
(2) again by 2g CaSO4·2H2O solution is slowly added into solution a, is continued magnetic agitation and is obtained within 3 minutes in palm fibre
Red suspension b.
(3) a small amount of ammoniacal liquor is added dropwise, regulation suspension b pH value is to 12, and it is in auburn solution c to obtain.
(4) solution c is filtered, then can obtains alpha-feooh/CaSO in 80 DEG C of dry 6h in an oven4·2H2O forerunner
Body.
Step 2, solid phase reduction reaction prepares Fe3O4@CaSO4, post-process and obtain Fe3O4Nanometer rods
(1) by a certain amount of alpha-feooh/CaSO4·2H2O presomas are put into burning boat, then are placed in boat is burnt in tube furnace,
Reduction reaction is carried out in a hydrogen atmosphere, and reaction temperature is 600 DEG C, and the reaction time is 1.5h.Then under reducing atmosphere, it is natural
The Fe in black solid state powder is obtained after cooling3O4@CaSO4Composite granule.
(2) by Fe3O4@CaSO4It is slowly added into BaCl2In solution, magnetic agitation 3h is obtained in grey black at 50 DEG C
Fe3O4And BaSO4Mixed solution.
(3) again by Fe3O4And BaSO4Mixed solution is cleaned by ultrasonic and Magneto separate, so as to obtain Fe3O4Nanometer rods.
Embodiment 4 is (without CaSO4·2H2O)
Without CaSO4·2H2O, other step be the same as Examples 1.
The XRD for preparing product by embodiment 1~4 collects spectrogram (as shown in Figure 4), FeSO4·7HO/CaSO4·
2H2O mass ratioes are to Fe3O4Form has a major impact, and both weight ratios are 2：When 1, pure Fe can be obtained3O4Nanometer rods；And do not having
There is addition CaSO4·2H2During O, the product of acquisition is random Fe3O4Nano particle.When both part by weight such as 1：1、1：2
When, the purity of the product of acquisition is relatively low.
Claims (1)
1. a kind of magnanimity prepares Fe3O4The method of nanometer rods, it is characterised in that step is as follows：
Step 1, alpha-feooh/CaSO is prepared4·2H2O presomas
(1) by 2g FeSO4·7H2O is dissolved in 100mL distilled water, and magnetic agitation is allowed to abundant dissolving for 2 minutes at room temperature
Obtain solution a；
(2) again by 1g CaSO4·2H2O solution is slowly added into solution a, is continued magnetic agitation and is obtained within 3 minutes being in brownish red
Suspension b；
(3) a small amount of ammoniacal liquor is added dropwise, regulation suspension b pH value is to 10, and it is in auburn solution c to obtain；
(4) solution c is filtered, then can obtains alpha-feooh/CaSO in 100 DEG C of dry 2h in an oven4·2H2O presomas；
Step 2, solid phase reduction reaction prepares Fe3O4@CaSO4, post-process and obtain Fe3O4Nanometer rods
(1) by a certain amount of alpha-feooh/CaSO4·2H2O presomas are put into burning boat, then are placed in boat is burnt in tube furnace, in hydrogen
Reduction reaction is carried out under gas atmosphere, reaction temperature is 550 DEG C, and the reaction time is 1h；Then under reducing atmosphere, after natural cooling
Obtain the Fe in black solid state powder3O4@CaSO4Composite granule；
(2) by Fe3O4@CaSO4It is slowly added into BaCl2In solution, magnetic agitation 1h is obtained in grey black at 100 DEG C
Fe3O4And BaSO4Mixed solution；
(3) again by Fe3O4And BaSO4Mixed solution is cleaned by ultrasonic and Magneto separate, so as to obtain Fe3O4Nanometer rods.
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