CN108545782A - The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse - Google Patents
The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse Download PDFInfo
- Publication number
- CN108545782A CN108545782A CN201810469039.6A CN201810469039A CN108545782A CN 108545782 A CN108545782 A CN 108545782A CN 201810469039 A CN201810469039 A CN 201810469039A CN 108545782 A CN108545782 A CN 108545782A
- Authority
- CN
- China
- Prior art keywords
- coercivity
- monodisperse
- ultralow
- ferriferrous oxide
- nano flower
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002057 nanoflower Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 26
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229940056319 ferrosoferric oxide Drugs 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 150000002505 iron Chemical class 0.000 claims abstract description 7
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 6
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 5
- 239000001632 sodium acetate Substances 0.000 claims abstract description 5
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 claims abstract 4
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 230000005415 magnetization Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 17
- 238000000034 method Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 2
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- -1 medical diagnosis Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000011091 sodium acetates Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 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]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a kind of preparation methods of the ultralow coercivity ferriferrous oxide nano flower of monodisperse, include the following steps：Trivalent iron salt and sodium acetate are added in ethylene glycol, polyethylene glycol is added after stirring evenly, obtains mixed solution II；Sodium hydroxide solution is added dropwise to above-mentioned mixed solution II, after being added dropwise, 40 ± 5 DEG C is heated to and stirs 0.8~1.2 hour, obtain ferroso-ferric oxide colloidal sol；Ferroso-ferric oxide colloidal sol is placed in reaction kettle, 16~22h is reacted at a high temperature of 180~200 DEG C；By black product Magneto separate obtained by the reaction, wash, it is dry, obtain the ultralow coercivity ferriferrous oxide nano flower of monodisperse.The monodisperse ferriferrous oxide nano flower prepared using the present invention is with higher saturation magnetization, extremely low coercivity and good dispersibility and stability, the technical problem high compared with perfectly solving nano ferriferrous oxide bad dispersibility, coercivity.
Description
Technical field
The invention belongs to technical field of function materials, it is related to a kind of ultralow coercivity ferriferrous oxide nano flower of monodisperse
Preparation method.
Background technology
Ferroso-ferric oxide is a kind of common inverse spinel ferrite magnetic material, cheap since its is widely distributed,
And there is preferable magnetic property, become one of the magnetic material being most widely used.With the development of science and technology, especially
It is the research and development of nanotechnology, people are also gradually deep into a nanometer level to the research of ferroso-ferric oxide.With traditional four
Fe 3 O is compared, and nano ferriferrous oxide shows many excellent performances, is such as less than 10 in ferroso-ferric oxide crystallite dimension
When nanometer, extremely low coercivity is shown, hysteresis almost disappears and (is changed into soft magnetic materials by hard magnetic material)；Nano-scale
The magnetic susceptibility of ferroso-ferric oxide very strongly depends on the variation of temperature, shows superparamagnetism；Ferroferric oxide nano granules
The nanometer size effect and high specific surface area having make it have easy rhetorical function group of good absorption property etc..In addition
Due to the characteristics such as high saturation and magnetic intensity and good biocompatibility possessed by ferroso-ferric oxide itself, nanometer four is made to aoxidize
Three-iron is in many biomedical and Industrial Engineering fields such as biological medicine, medical diagnosis, medicament slow release, sewage disposal, catalyst
It has a wide range of applications.
Although the preparation method of current nano ferriferrous oxide have very much, due to nano ferriferrous oxide particle very
Small, itself with magnetism, makes it easily reunite, seriously limits its scope of application again；Meanwhile ferroso-ferric oxide is only in grain size
Can just have extremely low coercivity when less than 10 nanometers, otherwise excessively high coercivity will seriously affect subsequent modification and material
Recycling.Thus how under conditions of ensureing nano ferriferrous oxide good characteristic, acquisition monodisperse, low-coercivity are received
Rice ferroso-ferric oxide becomes an urgent demand of its research and development.
The preparation method of current most common nano ferriferrous oxide mainly has chemical coprecipitation, sol-gal process and molten
Three kinds of the hot method of agent.The crystallite dimension for the nano-particle that chemical coprecipitation is prepared is not easy to control and is unevenly distributed, due to receiving
The coercivity (or remanent magnetism) of rice corpuscles is usually very high, so that it is easily reunited, is unfavorable for subsequent modification and recycling, together
When, need same protective atmosphere, technique relatively complicated in preparation process；Although sol-gal process crystallite dimension is easy to control and distribution is equal
It is even, but there is very scabrous hard aggregation in the ferriferrous oxide nano-particle that its preparation process can make；Common solvent heat
Ferriferrous oxide nano-particle that method is prepared dispersibility is usually preferable, but there are still nano-particle coercivity is excessive, and crystal grain
The non-uniform problem of size.Therefore, it is necessary to be improved to the above-mentioned prior art.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparations of the ultralow coercivity nano ferriferrous oxide of monodisperse
Method, the monodisperse ferriferrous oxide nano flower prepared using the present invention with higher saturation magnetization, extremely low rectify
Stupid power and good dispersibility and stability, perfectly solve the high skill of nano ferriferrous oxide bad dispersibility, coercivity
Art problem.
In order to solve the problems, such as that above-mentioned skill, the present invention provide a kind of system of the ultralow coercivity ferriferrous oxide nano flower of monodisperse
Preparation Method includes the following steps：
1), 0.0406 mole of trivalent iron salt and sodium acetate are added in ethylene glycol, obtain mixing after stirring evenly molten
Liquid I；
Trivalent iron salt, sodium acetate molar ratio be 1：4~5,
In general, the ethylene glycol of 500~700 milliliters of every 0.0406 mole of trivalent iron salt adapted；
2) simultaneously uniform stirring, is added into above-mentioned mixed solution I in 2~3 grams of polyethylene glycol (PEG), obtains mixing molten
Liquid II；
3) 2~2.2g (preferably 2.1g) sodium hydroxide, is configured to sodium hydroxide solution, under stirring condition, by this
(time for adding is 0.8~1.2 hour) is added dropwise to above-mentioned mixed solution II in sodium hydroxide solution, after being added dropwise, is heated to 40
± 5 DEG C are stirred 0.8~1.2 hour, and ferroso-ferric oxide colloidal sol is obtained；
4), ferroso-ferric oxide colloidal sol is placed in reaction kettle (it includes that stainless steel casing and polytetrafluoroethyllining lining form to be
Pyroreaction kettle) in, 16~22h is reacted at a high temperature of 180~200 DEG C；
By black product Magneto separate obtained by the reaction, wash, it is dry, obtain the ultralow coercivity ferriferrous oxide nano of monodisperse
Flower (superparamagnetism monodisperse ferriferrous oxide nano flower).
The improvement of the preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse as the present invention：The trivalent
Molysite is ferric nitrate (nine water ferric nitrates) or iron chloride (Iron trichloride hexahydrate).
The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse as the present invention is further improved：It is poly-
The molecular weight of ethylene glycol (PEG) is 4000~20000.
The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse as the present invention is further improved：Institute
It states in step 3), the volume ratio of sodium hydroxide solution and mixed solution II is 1：15~25 (preferably 1：20).
The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse as the present invention is further improved：Institute
It states in step 4), washs to be cleaned successively with second alcohol and water；Dry is freeze-drying.The freeze-drying is specially：Clearly
Retain 20 ± 5 milliliters of water after washing, it is 24 ± 2 hours dry in -86 ± 5 DEG C.
The present invention uses solvent-thermal method, introduces PEG as surfactant, monodispersed ultralow coercivity four is prepared
Fe 3 O nanometer flower structure.
The present invention has the advantages that：Preparation process is simple, raw material easily obtains；Ferriferrous oxide nano flower obtained
With higher saturation magnetization, extremely low coercivity and good dispersibility and stability；Each nano flower is by several
The ferroso-ferric oxide little crystal grain that a grain size is 5 to 10 nanometers forms, and overall dimensions are ideally solved and received between 40 to 60 nanometers
The high technical problem of rice ferroso-ferric oxide bad dispersibility, coercivity.
Ferriferrous oxide nano that the method for the present invention is prepared flower, can directly as catalyst and medical development agent etc.,
The magnetic core that can be used for preparing the nuclear-shell structured nano-composite material of various polar group modifications, in biomedical and Industrial Engineering neck
There is huge application potential in domain.
Description of the drawings
The specific implementation mode of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the transmission electron microscope photo of the ultralow coercivity ferriferrous oxide nano flower of monodisperse prepared by embodiment 1.
Fig. 2 is the transmission electron microscope photo of the ultralow coercivity ferriferrous oxide nano flower of monodisperse prepared by embodiment 2.
Fig. 3 is the transmission electron microscope photo of the ultralow coercivity ferriferrous oxide nano flower of monodisperse prepared by embodiment 3.
Fig. 4 is the transmission electron microscope photo of the ultralow coercivity ferriferrous oxide nano flower of monodisperse prepared by embodiment 4.
Fig. 5 is the transmission electron microscope photo of the ultralow coercivity ferriferrous oxide nano flower of monodisperse prepared by embodiment 5.
Fig. 6 is the XRD spectra of the ultralow coercivity ferriferrous oxide nano flower of monodisperse prepared by embodiment 1.
Fig. 7 is the hysteresis loop figure of the ultralow coercivity ferriferrous oxide nano flower of monodisperse prepared by embodiment 1.
Specific implementation mode
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
A kind of preparation method of the ultralow coercivity ferriferrous oxide nano flower of embodiment 1, monodisperse, carries out following step successively
Suddenly：
1), 0.0406 mole of (16.4 grams) nine water ferric nitrate is added in 600 milliliters of ethylene glycol and stirs 30 minutes, then
26.9 grams of (0.1977 mole) sodium acetates are added, mixed solution I is obtained after stirring and dissolving；
2) simultaneously uniform stirring, is added in above-mentioned mixed solution I in the polyethylene glycol (PEG) that 3 gram-molecular weights are 10000, is obtained
To mixed solution II；
3), under stirring condition, by 30 milliliters of a concentration of 0.07 gram every milliliter of sodium hydrate aqueous solution (hydrogen-oxygens containing 2.1g
Change sodium), (that is, time for adding is 1 hour) is added drop-wise in mixed solution II with 30 milliliters/speed hourly, after being added dropwise,
It is heated to 40 DEG C and continues heating stirring 1 hour, obtain ferroso-ferric oxide colloidal sol；
4), ferroso-ferric oxide colloidal sol is placed in reaction kettle (it includes that stainless steel casing and polytetrafluoroethyllining lining form to be
Pyroreaction kettle) in, react 16h at a high temperature of 190 DEG C；
By black product Magneto separate obtained by the reaction, wash (being washed successively with the deionized water of 50ml ethyl alcohol and 50ml),
Retain 20 milliliters of water, it is 24 hours dry in -86 DEG C；Up to the ultralow coercitive ferriferrous oxide nano flower of monodisperse.
A kind of preparation method of the ultralow coercivity ferriferrous oxide nano flower of embodiment 2, monodisperse：
Make the dosage of polyethylene glycol in step 2) (PEG) into 2 grams；Remaining is equal to embodiment 1.
A kind of preparation method of the ultralow coercivity ferriferrous oxide nano flower of embodiment 3, monodisperse：
In step 2), it is 20000 polyethylene glycol (PEG) to select molecular weight, and the dosage of polyethylene glycol (PEG) is 3
Gram；Remaining is equal to embodiment 1.
A kind of preparation method of the ultralow coercivity ferriferrous oxide nano flower of embodiment 4, monodisperse：
In step 2), it is 4000 polyethylene glycol (PEG) to select molecular weight, and the dosage of polyethylene glycol (PEG) is 3
Gram；Remaining is equal to embodiment 1.
A kind of preparation method of the ultralow coercivity ferriferrous oxide nano flower of embodiment 5, monodisperse：
In step 2), it is 10000 polyethylene glycol (PEG) to select molecular weight, and the dosage of polyethylene glycol (PEG) is
2.5 gram；Remaining is equal to embodiment 1.
A kind of preparation method of the ultralow coercivity ferriferrous oxide nano flower of embodiment 6, monodisperse：
Make nine water ferric nitrates in step 1) into Iron trichloride hexahydrate；Mole is constant；Remaining is equal to embodiment 1.
Test one, every magnetic property by vibrating magnetometer (VSM) and transmission electron microscope (TEM) to above-mentioned case
And its pattern is characterized, acquired results are as shown in the table.
Table 1
Comparative example 1, cancellation step 3) in sodium hydroxide solution addition；Remaining is equal to embodiment 1.
Comparative example 2-1, cancellation step 2) in polyethylene glycol addition；That is, sodium hydroxide solution is added dropwise to mixed solution I
In；Remaining is equal to embodiment 1.
Comparative example 2-2, the usage amount of polyethylene glycol in step 2) (10000) is changed to 4 grams；Remaining is equal to embodiment 1.
Comparative example 2-3, the molecular weight of the polyethylene glycol in step 2) is changed to 40000, usage amount is still 3 grams；Remaining etc.
It is same as
Embodiment 1.
In comparative example 3, step 3), cancel the step of heating for 40 DEG C after dripping sodium hydroxide solution；That is, sodium hydroxide
After aqueous solution is added dropwise, continue heating stirring at room temperature 1 hour；Remaining is equal to embodiment 1.
Comparative example 4-1, the reaction temperature in step 4) is risen to 220 DEG C by 190 DEG C；Remaining is equal to embodiment 1.
Comparative example 4-2, the reaction time in step 4) was changed to 8 hours by 16 hours；Remaining is equal to embodiment 1.
" retaining 20 milliliters of water, 24 hours dry in -86 DEG C " in step 4), is made into " vacuum is dry at 60 DEG C by comparative example 5
Dry 24 hours "；Remaining is equal to embodiment 1.
Above-mentioned all comparative examples are carried out to the detection of properties according to one mode of above-mentioned experiment, acquired results are such as
Described in the following table 2.
Table 2
| Saturation magnetization emu/g | Coercivity Oe | Pattern | |
| Comparative example 1 | 46.53 | 11.02 | Nano flower-like structure, particle bad dispersibility are not formed |
| Comparative example 2-1 | 44.76 | 8.910 | Nano flower-like structure is not formed, and particle has irregular reunion |
| Comparative example 2-2 | 50.53 | 9.221 | Nano flower-like structure is not formed, and particle has irregular reunion |
| Comparative example 2-3 | 45.66 | 7.198 | There are nano flower-like structure, particle bad dispersibility |
| Comparative example 3 | 48.13 | 7.025 | There is part nano flower-like structure, but is distributed very uneven |
| Comparative example 4-1 | 65.19 | 98.47 | Nano flower-like structure is not formed, and crystal grain is larger, reunites |
| Comparative example 4-2 | 33.45 | 17.26 | Nano flower-like structure is not formed, and particle has irregular reunion |
| Comparative example 5 | 48.49 | 8.521 | There are nano flower-like structure, particle bad dispersibility |
Finally, it should also be noted that it is listed above be only the present invention several specific embodiments.Obviously, this hair
Bright to be not limited to above example, acceptable there are many deformations.Those skilled in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
Claims (5)
1. the preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse, it is characterized in that including the following steps：
1), 0.0406 mole of trivalent iron salt and sodium acetate are added in ethylene glycol, mixed solution I is obtained after stirring evenly；
Trivalent iron salt, sodium acetate molar ratio be 1：4~5,
2) simultaneously uniform stirring, is added into above-mentioned mixed solution I in 2~3 grams of polyethylene glycol, obtains mixed solution II；
3) 2~2.2g sodium hydroxides, are configured to sodium hydroxide solution, under stirring condition, this sodium hydroxide solution is added dropwise
To above-mentioned mixed solution II, after being added dropwise, it is heated to 40 ± 5 DEG C and stirs 0.8~1.2 hour, obtain ferroso-ferric oxide colloidal sol；
4), ferroso-ferric oxide colloidal sol is placed in reaction kettle, 16~22h is reacted at a high temperature of 180~200 DEG C；
By black product Magneto separate obtained by the reaction, wash, it is dry, obtain the ultralow coercivity ferriferrous oxide nano flower of monodisperse.
2. the preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse according to claim 1, it is characterized in that：
The trivalent iron salt is ferric nitrate or iron chloride.
3. the preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse according to claim 2, it is characterized in that：
The molecular weight of polyethylene glycol is 4000~20000.
4. the preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse according to claim 2 or 3, feature
It is：
In the step 3), the volume ratio of sodium hydroxide solution and mixed solution II is 1：15~25.
5. the preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse according to claim 2 or 3, feature
It is：
In the step 4), wash to be cleaned successively with second alcohol and water；Dry is freeze-drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810469039.6A CN108545782B (en) | 2018-05-16 | 2018-05-16 | The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810469039.6A CN108545782B (en) | 2018-05-16 | 2018-05-16 | The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108545782A true CN108545782A (en) | 2018-09-18 |
| CN108545782B CN108545782B (en) | 2019-11-15 |
Family
ID=63495036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810469039.6A Active CN108545782B (en) | 2018-05-16 | 2018-05-16 | The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108545782B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110550666A (en) * | 2019-09-27 | 2019-12-10 | 陕西科技大学 | Monodisperse and superparamagnetic ferroferric oxide nanoflower and preparation method thereof |
| CN112125344A (en) * | 2019-06-25 | 2020-12-25 | 北京化工大学 | Preparation method of monodisperse nano iron oxide dispersoid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010707A (en) * | 2010-10-21 | 2011-04-13 | 中山大学 | Method for preparing magneto-chromism ferroferric oxide sol |
| CN105932237A (en) * | 2016-05-10 | 2016-09-07 | 江苏楚汉新能源科技有限公司 | Method for preparing spindle-shaped Fe<3>O<4>/C composite negative electrode material |
| CN106799246A (en) * | 2017-02-26 | 2017-06-06 | 河南师范大学 | A kind of magnetic MoS2@Fe3O4Composite visible light catalyst and its preparation method and application |
| CN106890627A (en) * | 2017-01-20 | 2017-06-27 | 贵州理工学院 | A kind of preparation method of the magnetic mesoporous imprinted material of sandwich structure of energy separating Ge |
-
2018
- 2018-05-16 CN CN201810469039.6A patent/CN108545782B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010707A (en) * | 2010-10-21 | 2011-04-13 | 中山大学 | Method for preparing magneto-chromism ferroferric oxide sol |
| CN105932237A (en) * | 2016-05-10 | 2016-09-07 | 江苏楚汉新能源科技有限公司 | Method for preparing spindle-shaped Fe<3>O<4>/C composite negative electrode material |
| CN106890627A (en) * | 2017-01-20 | 2017-06-27 | 贵州理工学院 | A kind of preparation method of the magnetic mesoporous imprinted material of sandwich structure of energy separating Ge |
| CN106799246A (en) * | 2017-02-26 | 2017-06-06 | 河南师范大学 | A kind of magnetic MoS2@Fe3O4Composite visible light catalyst and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| QIANWEN WANG ET AL.: "Magnetically recyclable visible-light-responsive MoS2@Fe3O4 photocatalysts targeting efficient wastewater treatment", 《CHEMICAL ROUTES TO MATERIALS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125344A (en) * | 2019-06-25 | 2020-12-25 | 北京化工大学 | Preparation method of monodisperse nano iron oxide dispersoid |
| CN112125344B (en) * | 2019-06-25 | 2022-12-09 | 北京化工大学 | Preparation method of monodisperse nano iron oxide dispersoid |
| CN110550666A (en) * | 2019-09-27 | 2019-12-10 | 陕西科技大学 | Monodisperse and superparamagnetic ferroferric oxide nanoflower and preparation method thereof |
| CN110550666B (en) * | 2019-09-27 | 2022-01-28 | 陕西科技大学 | Monodisperse and superparamagnetic ferroferric oxide nanoflower and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108545782B (en) | 2019-11-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Trpkov et al. | Hydrothermal synthesis, morphology, magnetic properties and self-assembly of hierarchical α-Fe2O3 (hematite) mushroom-, cube-and sphere-like superstructures | |
| Moreno et al. | Preparation of narrow size distribution superparamagnetic γ-Fe2O3 nanoparticles in a sol− gel transparent SiO2 matrix | |
| Liu et al. | Magnetic behavior of Zn-doped Fe3O4 nanoparticles estimated in terms of crystal domain size | |
| Lu et al. | Green synthesis and characterization of superparamagnetic Fe3O4 nanoparticles | |
| Moumen et al. | Control of the size of cobalt ferrite magnetic fluid | |
| Egizbek et al. | Stability and cytotoxicity study of NiFe2O4 nanocomposites synthesized by co-precipitation and subsequent thermal annealing | |
| CN101289314B (en) | Method for preparing nano hollow microballoons of spinelle type ferrite | |
| US7892520B2 (en) | Solid-state synthesis of iron oxide nanoparticles | |
| Zhao et al. | Effect of surfactant amount on the morphology and magnetic properties of monodisperse ZnFe2O4 nanoparticles | |
| CN106315684B (en) | The preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size | |
| Oh et al. | Synthesis of Fe3O4 nanoparticles of various size via the polyol method | |
| CN108545782B (en) | The preparation method of the ultralow coercivity ferriferrous oxide nano flower of monodisperse | |
| CN104045336B (en) | The preparation method of nickel ferrite magnetic nano-fiber material | |
| CN111072070B (en) | Preparation method of high-saturation magnetization superparamagnetic porous ferrite microspheres | |
| CN109665565B (en) | Nano Fe3O4Preparation method of composite graphene and nano Fe3O4Composite graphene | |
| Elayakumar et al. | Structural and magnetic characterization of rare earth element Cerium-doped nickel ferrite nanoparticles (NiCe x Fe2-x O4) by sol-gel method with antibacterial activity | |
| CN101728046A (en) | Method for preparing mono-disperse magnetic controllable Fe3O4-SiO2 nuclear shell ball cluster | |
| CN102923785A (en) | Preparation method of CoFe2O4 magnetic nano material | |
| CN101913852A (en) | Method for synthesizing spherical superparamagnetic ferrite nano druse | |
| CN111517372A (en) | Fullerene coated Fe3O4Composite nano material and preparation method thereof | |
| CN101125684A (en) | Preparation method for gamma-Fe2O3 magnetic nano particles | |
| JPH03126626A (en) | Maghemite particulate plate and its production | |
| Jing et al. | Hydrothermal fabrication of various morphological α-Fe2O3 nanoparticles modified by surfactants | |
| Rafizadeh-Sourki et al. | Facile synthesis of Zn0. 5Ni0. 5Fe2O4/carbon nanocomposite for hyperthermia and drug delivery applications | |
| CN106395914A (en) | Superparamagnetic Fe3O4 coated by oleic acid and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |