CN106430327A - Porous sea-urchin-shaped Fe3O4@C composite material and preparation method thereof - Google Patents
Porous sea-urchin-shaped Fe3O4@C composite material and preparation method thereof Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 63
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000243 solution Substances 0.000 claims abstract description 46
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 45
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 45
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000011259 mixed solution Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 241000257465 Echinoidea Species 0.000 claims description 68
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 239000011258 core-shell material Substances 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000005253 cladding Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004886 process control 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 description 36
- 239000002244 precipitate Substances 0.000 description 36
- 239000007788 liquid Substances 0.000 description 32
- 238000005119 centrifugation Methods 0.000 description 18
- 238000004140 cleaning Methods 0.000 description 18
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 18
- 230000001681 protective effect Effects 0.000 description 17
- 239000000463 material Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000002114 nanocomposite Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229940056319 ferrosoferric oxide Drugs 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004176 ammonification Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 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)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
-
- 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
-
- 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
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention belongs to the technical field of semiconductor composite nano material preparation and relates to a porous sea-urchin-shaped Fe3O4@C composite material and a preparation method thereof. The preparation method includes the steps of a, dissolving ferric chloride into ethylene glycol, and stirring to form a ferric chloride solution; b, adding diethylenetriamine into the ferric chloride solution, and stirring to obtain a mixed solution; c, adding the mixed solution obtained in the step b into a reaction kettle, heating to a certain temperature, and performing reaction for a certain period of time to form a precursor; d, calcining the precursor obtained in the step c under an inert gas or vacuum environment to obtain the porous sea-urchin-shaped Fe3O4@C composite material. The preparation method has the advantages that the method is simple in process, low in equipment requirement and high in controllable degree; the porous sea-urchin-shaped Fe3O4@C composite material is prepared by reasonable process control, the prepared sea-urchin-shaped Fe3O4@C is even in size, good in dispersity and novel in morphology, a spherical structure comprises through holes, and the porous sea-urchin-shaped Fe3O4@C composite material is good in porosity, large in specific surface area, good in absorption performance, high in heavy metal ion absorption ability and widely applicable to energy and environment protection industry.
Description
Technical field
The invention belongs to semiconductor composite nano material preparation process technical field, it is related to a kind of porous sea urchin shape Fe3O4@C
The preparation method of composite.
Technical background
Ferroso-ferric oxide (Fe3O4) it is a kind of important spinel type ferrite, proceed by system from the forties in 20th century
Since research and production, Ferrite Material has obtained extremely rapidly developing.They are in magnetic fluid, electronic device, information storage
Deposit, the defeated biography of Magnetic Isolation, medicine, magnetic resonance imaging and protein absorption etc. field suffer from extensively applying.
However, simple ferroso-ferric oxide, because it is perishable, the unstable grade of property determines, limits its application.In recent years,
The nano composite material of core shell structure becomes current research in nanotechnology field due to the controlled physicochemical properties of itself
Study hotspot, and receive scientists and more and more pay attention to.Under normal circumstances, the highly stable carbon of utility is wrapping
Cover the Fe being easier oxidation deterioration3O4Produce composite, the combination property of material can be made to significantly improve.At present, with carbon bag
Cover Fe3O4The nano composite material of preparation mainly has：(1) carbon source and Fe are used glucose as3O4Mixing carbonization preparation magnetic core
Shell structure, but its shortcoming is mostly spheric granules packed structures (2) with mesoporous silicon oxide for templated synthesis Fe3O4Mesoporous carbon is multiple
Condensation material.(3) α-Fe of oleic acid-coated is synthesized with hydro-thermal method3O4Particle is presoma, then 500 DEG C of calcinings 1 are little under an argon atmosphere
When, obtain Fe3O4/ C nano composite, it is shaped as spindle.(4) activated carbon/Fe is prepared using homogeneous precipitation method3O4
Particle and CNT/Fe3O4The composites such as particle.But, the Fe of these carbon coatings3O4The common spy of nano composite material
Putting is：Specific surface area is low, and porosity is low, and material surface not increase its functional group through further functionalization, therefore makes
The Fe of carbon coating3O4The application of nano composite material is restricted.
However, in some special application fields, such as absorption, the defeated biography of medicine etc., need the characteristics such as big specific surface area, in order
Mesoporous carbon be a kind of there is the controlled nano material of high-specific surface area, big pore volume, homogeneous adjustable aperture, mesoscopic structure, its
Have a wide range of applications in catalysis, absorption, optics and electrochemical field.By mesoporous carbon and Fe3O4The magnetic being combined and preparing
Microballoon can be used for the fields such as wastewater treatment, catalyst carrier, bio-separation.Although current someone adopts multiple methods to prepare porous
Magnetic composite.In Patent No. CN103585955A, C/Fe is prepared using conventional hydrothermal method3O4Nano-particle, and utilize
Small particle Fe3O4As pore creating material, by low-temperature carbonization, acid etching forms surface band hole coralliform composite C/
Fe3O4.In CN103417974A, it is raw material using reduced iron powder, with nitric acid dissolving magnetic field co-precipitation, obtain the flower-shaped Fe of porous3O4
Nanostructured, then with polyvinyl alcohol as crosslinking agent, p-methyl benzenesulfonic acid is surfactant, makes the flower-shaped Fe of porous3O4With galactolipin
Make to mix and through high temperature cabonization, obtain the cellular Fe of carbon coating3O4Nanostructured.Huang et al., in " Rapid removal
of heavy metal cations and anions from aqueous solutions by an amino-
Functionalized magnetic nano-adsorbent ", using Fe2+and Fe3+Coprecipitation Fe3O4, then coat
PAA, last DETA ammonification, obtain Fe3O4Composite construction.However, existing method is complicated, time-consuming, power consumption big, adsorptivity, separation
Property not high, bad control, and uncomfortable a large amount of produce, limit its practical application to a certain extent.And preparation fine dispersion
Property, uniform particle diameter porous sea urchin shape Fe3O4@C composite remains extremely difficult.In consideration of it, the present invention attempts by letter
Single, cost effective method prepares a kind of porous sea urchin shape Fe3O4@C composite, and this material has higher heavy metal ion suction
Attached performance.
Content of the invention
Primary technical problem to be solved by this invention is to provide a kind of process is simple, low cost, reaction time short, uniform
, porous sea urchin shape Fe3O4The preparation method of@C composite.
A kind of porous sea urchin shape Fe3O4The preparation method of@C composite, comprises the following steps：
A. iron chloride is dissolved in ethylene glycol, stirring, forms ferric chloride solution；
B. diethylenetriamine is added in described ferric chloride solution, stirring, form mixed solution；
C. mixed solution described in step b is added in reactor, is heated to uniform temperature, react certain time, shape
Become presoma；
D. the presoma that step c obtains is calcined under inert gas or vacuum environment, obtain final product product.
Further, the diethylenetriamine of described step b and the mol ratio of iron chloride are (1-9)：1.
Further, the ferric chloride solution concentration of described step a is 1 × 10-5-8×10-5mol/mL.
Further, the mixing time of described step b is 10-50 minute.
Further, the uniform temperature of described step c is 120-200 DEG C, and reaction certain time is 4-12h.
Further, the inert gas of described step d is nitrogen or argon gas.
Further, in described step d, calcining heat is 300～800 DEG C, and the time of calcining is 90～300min.
Further, in described step d, the programming rate of calcining is 5～30 DEG C/min.
Present invention additionally comprises, a kind of porous sea urchin shape Fe3O4@C composite is it is characterised in that use above-mentioned preparation method
The porous sea urchin shape Fe of preparation3O4@C.
Further, the Fe of described porous sea urchin shape3O4@C composite is core shell structure, and kernel is Fe3O4, around interior
Core cladding for C；Described Fe3O4@C is constituted by spherical structure with around the bayonet fittings of spherical structure, and described spherical structure contains
Through hole, a diameter of 0.6 μm -2.32 μm of described spherical structure, the length of described bayonet fittings is 1.07 μm -1.63 μm.
Compared with prior art, its prominent effect is the present invention：The porous sea urchin shape Fe of the present invention3O4The preparation method of@C,
Preparation process is simple, low for equipment requirements, controllable degree is high.By rational technology controlling and process, realize porous sea urchin shape Fe3O4@C
Preparation, this sea urchin shape Fe3O4@C is uniform in size, good dispersion, novel in shape, and described spherical structure contains through hole, has preferably
Porous, specific surface area is big, and absorption property is good, has higher heavy metal ion adsorbed ability, has in the energy, environmental protection industry (epi)
It is widely applied.
Brief description
Fig. 1 is the porous sea urchin shape Fe prepared by example 23O4SEM (SEM) photo of@C.
Fig. 2 is the porous sea urchin shape Fe prepared by example 23O4Transmission electron microscope (TEM) photo of@C.
Fig. 3 is the porous sea urchin shape Fe prepared by example 23O4Transmission electron microscope (TEM) photo of@C.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but does not limit the present invention, chlorination in the present embodiment
Iron adopts Iron trichloride hexahydrate.
Embodiment 1
A kind of porous sea urchin shape Fe3O4The preparation method of@C composite, comprises the following steps that：
A. 0.8g Iron trichloride hexahydrate is dissolved in 50ml ethylene glycol, stirs 40 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 5.93 × 10-5mol/mL；
B. 1g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 40min, form mixed solution；
Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 180 DEG C
After reaction 8 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 200cm3/
Min, rises to 350 DEG C with the programming rate of 20 DEG C/min by room temperature, constant temperature 120min, and subsequently this system is naturally cooled room
Temperature, that is, obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 2
A kind of Fe3O4The preparation method of@C porous sea urchin shape core shell structure, comprises the following steps that：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
The porous sea urchin shape Fe that accompanying drawing 1-3 is prepared for the method3O4SEM the and TEM figure of@C, is understood successfully to prepare by accompanying drawing
Go out Fe3O4@C composite, Fe3O4@C composite is core shell structure, and kernel is Fe3O4, it is C around kernel cladding；Institute
State Fe3O4@C is constituted by spherical structure with around the bayonet fittings of spherical structure, and described spherical structure contains through hole, described spherical
A diameter of 0.6 μm -2.32 μm of structure, the length of described bayonet fittings is 1.07 μm -1.63 μm.Size uniform, is porous knot
Structure, can be used for Adsorption of Heavy Metal Ions, is widely used in the energy, in environmental protection industry (epi).
Embodiment 3
With the difference of embodiment 2, this embodiment is that the amount of iron chloride changes into 0.8g, other are same as Example 2, tool
Body is as follows：
A. 0.8g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 7.41 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 1.51 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 4
With the difference of embodiment 2, this embodiment is that the amount of iron chloride changes into 0.2g, other are same as Example 2, tool
Body is as follows：
A. 0.2g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 1.85 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 6.04 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 5
With the difference of embodiment 2, this embodiment is that mixing time changes into 60min, other are same as Example 2, specifically
As follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 60min, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 60min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 6
The difference of this embodiment and embodiment 2 is that the amount of diethylenetriamine (DETA) changes into 1g, other and embodiment 2
Identical, specific as follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 1g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixed solution；
Described diethylenetriamine is 6.04 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 7
With the difference of embodiment 2, this embodiment is that reaction temperature changes into 180 DEG C, other are same as Example 2, specifically
As follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 180 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 8
With the difference of embodiment 2, this embodiment is that the reaction time is changed into 8 hours, other are same as Example 2, specifically
As follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 8 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin Fe of porous3O4@C.
Embodiment 9
With the difference of embodiment 2, this embodiment is that programming rate changes into 20 DEG C/min, other are same as Example 2,
Specific as follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 20 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room
Temperature, that is, obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 10
With the difference of embodiment 2, this embodiment is that programming rate changes into 30 DEG C/min, other are same as Example 2,
Specific as follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 30 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room
Temperature, that is, obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 11
With the difference of embodiment 2, this embodiment is that annealing speed changes into 300 DEG C, other are same as Example 2, specifically
As follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 300 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 12
With the difference of embodiment 2, this embodiment is that annealing speed changes into 600 DEG C, other are same as Example 2, specifically
As follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 600 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 13
With the difference of embodiment 2, this embodiment is that annealing time changes into 90min, other are same as Example 2, specifically
As follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 90min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 14
With the difference of embodiment 2, this embodiment is that annealing time changes into 300min, other are same as Example 2, tool
Body is as follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 300min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 15
With the difference of embodiment 2, this embodiment is that gas flow rate changes into 150cm3/ min, other and embodiment 2 phase
With specific as follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 150cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 16
With the difference of embodiment 2, this embodiment is that gas flow rate changes into 400cm3/ min, other and embodiment 2 phase
With specific as follows：
A. 0.4g Iron trichloride hexahydrate is dissolved in 40ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride is molten
The concentration of liquid is 3.70 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 3.02 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through nitrogen as protective gas, flow velocity is 400cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 17
This embodiment and the three of embodiment 2, other are same as Example 2, specific as follows：
A kind of Fe3O4The preparation method of@C porous sea urchin shape core shell structure, comprises the following steps that：
A. 1.3g Iron trichloride hexahydrate is dissolved in 60.5ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, iron chloride
The concentration of solution is 8 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 1 with the mol ratio of iron chloride：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, is passed through argon gas as protective gas, flow velocity is 300cm3/
Min, rises to 450 DEG C with the programming rate of 5 DEG C/min by room temperature, constant temperature 180min, and subsequently this system is naturally cooled room temperature,
Obtain the sea urchin shape Fe of porous3O4@C.
Embodiment 18
A kind of Fe3O4The preparation method of@C porous sea urchin shape core shell structure, comprises the following steps that：
A. 0.15g Iron trichloride hexahydrate is dissolved in 53.8ml ethylene glycol, stirs 30 minutes, form ferric chloride solution, chlorination
The concentration of ferrous solution is 1 × 10-5mol/mL；
B. 0.5g diethylenetriamine (DETA) will be added in ferric chloride solution in step a, stir 30min, form mixing molten
Liquid；Described diethylenetriamine is 9 with the mol ratio of Iron trichloride hexahydrate：1.
C. described mixed solution is added in tetrafluoroethene reactor, and reactor is put in insulating box, at 160 DEG C
After reaction 6 hours, that is, obtain black precipitate.
D. the black precipitate of step c is processed, that is, take out, centrifugation, cleaning, dried process, obtain the sea urchin shape of porous
Fe3O4@C presoma.
E. the presoma that step d obtains is placed in tube furnace, under vacuum condition, with the programming rate of 5 DEG C/min by room
Temperature rise to 450 DEG C, constant temperature 180min, subsequently this system be naturally cooled room temperature, that is, obtain the sea urchin shape Fe of porous3O4@C.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.Right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (10)
1. a kind of porous sea urchin shape Fe3O4The preparation method of@C composite is it is characterised in that comprise the following steps：
A. iron chloride is dissolved in ethylene glycol, stirring, forms ferric chloride solution；
B. diethylenetriamine is added in described ferric chloride solution, stirring, form mixed solution；
C. mixed solution described in step b is added in reactor, is heated to uniform temperature, react certain time, before formation
Drive body；
D. the presoma that step c obtains is calcined under inert gas or vacuum environment, obtain final product product.
2. a kind of porous sea urchin shape Fe as claimed in claim 13O4The preparation method of@C composite is it is characterised in that described
The diethylenetriamine of step b and the mol ratio of iron chloride are (1-9)：1.
3. a kind of porous sea urchin shape Fe as claimed in claim 1 or 23O4The preparation method of@C composite it is characterised in that
The ferric chloride solution concentration of described step a is 1 × 10-5-8×10-5mol/mL.
4. a kind of porous sea urchin shape Fe as claimed in claim 1 or 23O4The preparation method of@C composite it is characterised in that
The mixing time of described step b is 10-50 minute.
5. a kind of porous sea urchin shape Fe as claimed in claim 1 or 23O4The preparation method of@C composite it is characterised in that
The uniform temperature of described step c is 120-200 DEG C, and reaction certain time is 4-12h.
6. a kind of porous sea urchin shape Fe as claimed in claim 13O4The preparation method of@C composite is it is characterised in that described
The inert gas of step d is nitrogen or argon gas.
7. a kind of porous sea urchin shape Fe as claimed in claim 13O4The preparation method of@C composite is it is characterised in that described
In step d, the temperature of calcining is 300～800 DEG C, and the time of calcining is 90～300min.
8. a kind of porous sea urchin shape Fe as described in claim 1 or 6 or 73O4The preparation method of@C composite, its feature exists
In in described step d, the programming rate of calcining is 5～30 DEG C/min.
9. a kind of porous sea urchin shape Fe3O4@C composite is it is characterised in that use the preparation of any one of the claims 1-8
The porous sea urchin shape Fe of method preparation3O4@C.
10. a kind of porous sea urchin shape Fe as claimed in claim 93O4@C composite is it is characterised in that described porous sea urchin
The Fe of shape3O4@C composite is core shell structure, and kernel is Fe3O4, it is C around kernel cladding；Described Fe3O4@C is by spherical junctions
Structure and the bayonet fittings around spherical structure are constituted, and described spherical structure contains through hole, a diameter of 0.6 μ of described spherical structure
M-2.32 μm, the length of described bayonet fittings is 1.07 μm -1.63 μm.
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