CN104446420A - Preparation method of sulfur-doped ferric oxide magnetic particle magnetic material - Google Patents
Preparation method of sulfur-doped ferric oxide magnetic particle magnetic material Download PDFInfo
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- CN104446420A CN104446420A CN201410795123.9A CN201410795123A CN104446420A CN 104446420 A CN104446420 A CN 104446420A CN 201410795123 A CN201410795123 A CN 201410795123A CN 104446420 A CN104446420 A CN 104446420A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000000696 magnetic material Substances 0.000 title claims abstract description 13
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title abstract description 7
- 239000006249 magnetic particle Substances 0.000 title abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 29
- 229910001566 austenite Inorganic materials 0.000 claims description 25
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 17
- 238000013019 agitation Methods 0.000 claims description 16
- 238000009835 boiling Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000005864 Sulphur Substances 0.000 claims description 9
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000000460 chlorine Substances 0.000 claims description 8
- 229910052801 chlorine Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000002444 silanisation Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- -1 wherein Chemical compound 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Abstract
The invention relates to a preparation method of a sulfur-doped ferric oxide magnetic particle magnetic material. The method comprises the following steps: (1) preparing gama-Fe2O3 particles; (2) preparing gama- Fe2O3 particles with sulfur-doped surfaces; and (3) preparing a carbon-coated composite magnetic material. The prepared magnetic material is coated with ferric oxide, so that the magnetic property and dispersity can be improved, and by adopting an internal stable shell structure formed by a carbon coating technology, the corrosion-resistant property can be greatly improved, and the use loss of the magnetic material can be reduced.
Description
Technical field
The present invention relates to a kind of preparation method of iron oxide magnetic granular magnetic materials of sulfur doping.
Background technology
Magnetic Nano material has very important application in fields such as high density magnetic recording device, magnetic fluid, water purification, nuclear magnetic resonance, target medicine carrier, magnetic hyperthermy, catalyzer.Ferrous magnetic material is the ferric oxide of important a member, particularly ferrous magnetic material wherein.
Exposed ferric oxide particles is because high chemical reactivity is very easy to be corroded.Up to now, solution is: with physics, chemical process process nano grain surface, at the usual coated one deck of particle surface, inorganic or organism, promotes its stability, water dispersible and biocompatibility.From the application point of magnetic microsphere, for improving the colloidal stability of microballoon, regulating and controlling its surperficial hydrophilic, hydrophobic character and considering with the binding ability aspect of specific biological molecules, all needing to carry out surface-functionalized modification to magnetic microsphere.
In many researchs before, many inorganic and organic materialss are used to protect magnetic particle, such as: tensio-active agent/polymer shell and SiO
2shell, is all used to Coated magnetic particles.But tensio-active agent or polymer shell are not very stable in atmosphere, and are easily corroded by acid solution, cause the loss of saturation magnetization.Thin polymer shell can not stop the oxidation of high reaction activity magnetic nanoparticle completely; Polymer shell at high temperature has its inherent instability in addition, and this unstable even can be aggravated by the catalysis of magnetic particle institute.And SiO
2although shell has the features such as good unreactiveness, colloidal stability and biocompatibility, unstable in alkaline environment.
Summary of the invention
The invention provides a kind of preparation method of iron oxide magnetic granular magnetic materials of sulfur doping, magnetic material surface prepared by the method has the large carbon coating layer of specific surface area, kernel has the high and features such as the ferric oxide of the sulfur doping of magnetic property excellence of content, makes this material have good acid resistance and superior magnetic property.
To achieve these goals, the invention provides a kind of preparation method of iron oxide magnetic granular magnetic materials of sulfur doping, the method comprises the steps:
(1) γ-Fe is prepared
2o
3particle
The FeCl of preparation 1-2mol/L
3the aqueous solution, the MgCl of preparation 2-3mol/L
2the aqueous solution, according to often liter of MgCl
2the ratio that the aqueous solution adds 2-4mol HCl adds HCl and obtains mixed solution one, prepares the KOH aqueous solution of 1-2mol/L in addition, according to Fe
3+with Mg
2+mol ratio be 2-3:1, measure described FeCl
3the aqueous solution and described mixed solution one, be mixed with mixed solution two, according to FeCl
3, MgCl
2be 1-2:1:15-20 with the mol ratio of KOH, measure the described KOH aqueous solution, under agitation described mixed solution two is poured in the described KOH aqueous solution fast, be under agitation heated to boiling, keep boiling 10-15min, then heating is stopped, naturally cooling, hydroxide precursor Precipitation in process of cooling, centrifugation is carried out after end of processing to be precipitated, outwell clear liquid, obtain hydroxide precursor, sintering obtains γ-Fe under vacuo
2o
3particle;
(2) γ-Fe of surperficial sulfur doping is prepared
2o
3particle
By the γ-Fe of above-mentioned preparation
2o
3granular composite is to toluene and N, in the mixing solutions of N-METHYLFORMAMIDE, wherein, toluene and N, the volume ratio of dinethylformamide is 1:4-6, and ultrasonic disperse is even, then adds the dichloromethane solution of excessive 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, to make it fully react, described γ-Fe
2o
3be 1:5-10 with the mass ratio of the dichloromethane solution of 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, at 45-50 DEG C, Keep agitation obtains the γ-Fe of surface doping sulphur by Silanization reaction
2o
3particle;
(3) composite magnetic that carbon is coated is prepared
The acetone soln containing massfraction being 5-8 % oligoacrylonitrile is added the γ-Fe of above-mentioned surface doping sulphur
2o
3in particle, mass ratio is oligoacrylonitrile: martial ethiops is 0.02-0.05:1, mixes, evaporating solvent, drying at room temperature; At 220-240 DEG C of isothermal curing 3-5h, after ball milling, under inert atmosphere protection, at 750-800 DEG C of calcination temperature calcining 6-10h, obtain product.
Magneticsubstance prepared by the present invention, adopts sulphur to carry out coated to ferric oxide, the magnetic property improved and dispersiveness, and adopts containment structure stable in the formation of carbon cladding process, greatly improve corrosion resistance nature, and reduce magneticsubstance loss in use.
Embodiment
embodiment one
The FeCl of preparation 1mol/L
3the aqueous solution, the MgCl of preparation 2mol/L
2the aqueous solution, according to often liter of MgCl
2the ratio that the aqueous solution adds 2mol HCl adds HCl and obtains mixed solution one, prepares the KOH aqueous solution of 1mol/L in addition, according to Fe
3+with Mg
2+mol ratio be 2:1, measure described FeCl
3the aqueous solution and described mixed solution one, be mixed with mixed solution two, according to FeCl
3, MgCl
2be 1:1:15 with the mol ratio of KOH, measure the described KOH aqueous solution, under agitation described mixed solution two is poured in the described KOH aqueous solution fast, be under agitation heated to boiling, keep boiling 10min, then heating is stopped, naturally cooling, hydroxide precursor Precipitation in process of cooling, centrifugation is carried out after end of processing to be precipitated, outwell clear liquid, obtain hydroxide precursor, sintering obtains γ-Fe under vacuo
2o
3particle.
By the γ-Fe of above-mentioned preparation
2o
3granular composite is to toluene and N, in the mixing solutions of N-METHYLFORMAMIDE, wherein, toluene and N, the volume ratio of dinethylformamide is 1:4, and ultrasonic disperse is even, then adds the dichloromethane solution of excessive 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, to make it fully react, described γ-Fe
2o
3be 1:5 with the mass ratio of the dichloromethane solution of 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, at 45 DEG C, Keep agitation obtains the γ-Fe of surface doping sulphur by Silanization reaction
2o
3particle.
The acetone soln containing massfraction being 5 % oligoacrylonitriles is added the γ-Fe of above-mentioned surface doping sulphur
2o
3in particle, mass ratio is oligoacrylonitrile: martial ethiops is 0.02:1, mixes, evaporating solvent, drying at room temperature; At 220 DEG C of isothermal curing 5h, after ball milling, under inert atmosphere protection, at 750 DEG C of calcination temperature calcining 10h, obtain product.
embodiment two
The FeCl of preparation 2mol/L
3the aqueous solution, the MgCl of preparation 3mol/L
2the aqueous solution, according to often liter of MgCl
2the ratio that the aqueous solution adds 4mol HCl adds HCl and obtains mixed solution one, prepares the KOH aqueous solution of 2mol/L in addition, according to Fe
3+with Mg
2+mol ratio be 3:1, measure described FeCl
3the aqueous solution and described mixed solution one, be mixed with mixed solution two, according to FeCl
3, MgCl
2be 2:1:20 with the mol ratio of KOH, measure the described KOH aqueous solution, under agitation described mixed solution two is poured in the described KOH aqueous solution fast, be under agitation heated to boiling, keep boiling 15min, then heating is stopped, naturally cooling, hydroxide precursor Precipitation in process of cooling, centrifugation is carried out after end of processing to be precipitated, outwell clear liquid, obtain hydroxide precursor, sintering obtains γ-Fe under vacuo
2o
3particle.
By the γ-Fe of above-mentioned preparation
2o
3granular composite is to toluene and N, in the mixing solutions of N-METHYLFORMAMIDE, wherein, toluene and N, the volume ratio of dinethylformamide is 1:6, and ultrasonic disperse is even, then adds the dichloromethane solution of excessive 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, to make it fully react, described γ-Fe
2o
3be 1:10 with the mass ratio of the dichloromethane solution of 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, at 50 DEG C, Keep agitation obtains the γ-Fe of surface doping sulphur by Silanization reaction
2o
3particle.
The acetone soln containing massfraction being 8 % oligoacrylonitriles is added the γ-Fe of above-mentioned surface doping sulphur
2o
3in particle, mass ratio is oligoacrylonitrile: martial ethiops is 0.05:1, mixes, evaporating solvent, drying at room temperature; At 240 DEG C of isothermal curing 3h, after ball milling, under inert atmosphere protection, at 800 DEG C of calcination temperature calcining 6h, obtain product.
comparative example
Preparation FeCl
3the aqueous solution (40ml, 1mol/L) ie in solution a; Preparation Mg (NO
3)
2the aqueous solution (10ml, 2mol/L), adds HCl(4.2mL, 12mol/L) obtain solution b; The preparation NaOH aqueous solution (500mL, 0.7mol/L) ie in solution c.Described solution a is mixed with described solution b, is mixed with FeCl3/Mg (NO3) 2 mixed solution, ie in solution d; Under agitation described solution d is poured in described solution c fast, be mixed with reaction solution e; Described reaction solution e is heated to boiling by electric furnace, keeps boiling 5 minutes, then stop heating; Take off described reaction solution e from electric furnace, naturally cool to room temperature, after about two hours, reddish-brown precipitation hydroxide precursor is separated out completely.Preparation FeCl
2the aqueous solution (400mL, 0.25mol/L) ie in solution f, ZnCl
2the aqueous solution (50mL, 0.5mol/L) ie in solution g; Described hydroxide precursor is distributed in described solution f, is mixed with mixed solution h, FeCl
2the mol ratio of NaOH when preparing with hydroxide precursor is 1:3.5; Under agitation described mixed solution h is heated to boiling, keeps boiling 20 minutes; Under agitation described solution g is added in the described mixed solution h of boiling, obtain mixed solution i; Under agitation continue to keep described mixed solution i to seethe with excitement 10 minutes, then stop heating; Make described mixed solution i naturally cool to room temperature, after 2 hours, nanoparticle is separated out completely with the form of throw out j.Outwelling the upper clear supernate after Precipitation, is that the acetone of 5 times amount of throw out j mixes with it with volume, and carry out centrifugation again after fully stirring, this step repeats 3 times.Throw out j after cleaning is moved in vacuum drier dry, after 24 hours, obtain γ-Fe
2o
3/ ZnFe
2o
4magnetic nano composite particles powder.
Magnetism testing is carried out to the magneticsubstance of embodiment 1-2 and comparative example.Test result show: the magneticsubstance that embodiment 1-2 obtains saturation magnetic field improve more than 10.5-14.2emu/g than comparative example, be that the work-ing life in the sour environment of 5 improves more than 40% at pH value.
Claims (1)
1. a preparation method for the iron oxide magnetic granular magnetic materials of sulfur doping, the method comprises the steps:
(1) γ-Fe is prepared
2o
3particle
The FeCl of preparation 1-2mol/L
3the aqueous solution, the MgCl of preparation 2-3mol/L
2the aqueous solution, according to often liter of MgCl
2the ratio that the aqueous solution adds 2-4mol HCl adds HCl and obtains mixed solution one, prepares the KOH aqueous solution of 1-2mol/L in addition, according to Fe
3+with Mg
2+mol ratio be 2-3:1, measure described FeCl
3the aqueous solution and described mixed solution one, be mixed with mixed solution two, according to FeCl
3, MgCl
2be 1-2:1:15-20 with the mol ratio of KOH, measure the described KOH aqueous solution, under agitation described mixed solution two is poured in the described KOH aqueous solution fast, be under agitation heated to boiling, keep boiling 10-15min, then heating is stopped, naturally cooling, hydroxide precursor Precipitation in process of cooling, centrifugation is carried out after end of processing to be precipitated, outwell clear liquid, obtain hydroxide precursor, sintering obtains γ-Fe under vacuo
2o
3particle;
(2) γ-Fe of surperficial sulfur doping is prepared
2o
3particle
By the γ-Fe of above-mentioned preparation
2o
3granular composite is to toluene and N, in the mixing solutions of N-METHYLFORMAMIDE, wherein, toluene and N, the volume ratio of dinethylformamide is 1:4-6, and ultrasonic disperse is even, then adds the dichloromethane solution of excessive 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, to make it fully react, described γ-Fe
2o
3be 1:5-10 with the mass ratio of the dichloromethane solution of 2-(4-chlorine sulfonyl-phenyl)-ethyl trimethoxy silane, at 45-50 DEG C, Keep agitation obtains the γ-Fe of surface doping sulphur by Silanization reaction
2o
3particle;
(3) composite magnetic that carbon is coated is prepared
The acetone soln containing massfraction being 5-8 % oligoacrylonitrile is added the γ-Fe of above-mentioned surface doping sulphur
2o
3in particle, mass ratio is oligoacrylonitrile: martial ethiops is 0.02-0.05:1, mixes, evaporating solvent, drying at room temperature; At 220-240 DEG C of isothermal curing 3-5h, after ball milling, under inert atmosphere protection, at 750-800 DEG C of calcination temperature calcining 6-10h, obtain product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410795123.9A CN104446420A (en) | 2014-12-20 | 2014-12-20 | Preparation method of sulfur-doped ferric oxide magnetic particle magnetic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410795123.9A CN104446420A (en) | 2014-12-20 | 2014-12-20 | Preparation method of sulfur-doped ferric oxide magnetic particle magnetic material |
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| Publication Number | Publication Date |
|---|---|
| CN104446420A true CN104446420A (en) | 2015-03-25 |
Family
ID=52893269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410795123.9A Pending CN104446420A (en) | 2014-12-20 | 2014-12-20 | Preparation method of sulfur-doped ferric oxide magnetic particle magnetic material |
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| Country | Link |
|---|---|
| CN (1) | CN104446420A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986804A (en) * | 2015-08-12 | 2015-10-21 | 兰州大学 | Method for preparing gamma-Fe2O3 magnetic nano-particles |
| US20200116713A1 (en) * | 2017-06-30 | 2020-04-16 | Tdk Corporation | Analysis kit and analysis method |
| CN111048753A (en) * | 2019-11-29 | 2020-04-21 | 上海应用技术大学 | Iron oxide doped phosphorus atom composite material and preparation method and application thereof |
-
2014
- 2014-12-20 CN CN201410795123.9A patent/CN104446420A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986804A (en) * | 2015-08-12 | 2015-10-21 | 兰州大学 | Method for preparing gamma-Fe2O3 magnetic nano-particles |
| US20200116713A1 (en) * | 2017-06-30 | 2020-04-16 | Tdk Corporation | Analysis kit and analysis method |
| CN111048753A (en) * | 2019-11-29 | 2020-04-21 | 上海应用技术大学 | Iron oxide doped phosphorus atom composite material and preparation method and application thereof |
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