CN106986391A - A kind of magnetic colloid core shell structure α Fe2O3Preparation method - Google Patents
A kind of magnetic colloid core shell structure α Fe2O3Preparation method Download PDFInfo
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- CN106986391A CN106986391A CN201710249533.7A CN201710249533A CN106986391A CN 106986391 A CN106986391 A CN 106986391A CN 201710249533 A CN201710249533 A CN 201710249533A CN 106986391 A CN106986391 A CN 106986391A
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- 239000000084 colloidal system Substances 0.000 title claims abstract description 33
- 239000011258 core-shell material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000004471 Glycine Substances 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 11
- 229910000859 α-Fe Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000012046 mixed solvent Substances 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 230000035484 reaction time Effects 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
- 239000002245 particle Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- -1 environment Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000036285 pathological change Effects 0.000 description 1
- 231100000915 pathological change Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000036301 sexual development Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- 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
- C01P2004/03—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
- C01P2004/50—Agglomerated particles
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
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)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a kind of magnetic colloid core shell structure α Fe2O3Preparation method, belong to the synthesis technical field of core-shell structured nanomaterials.Technical scheme main points are：Using glycine as structure directing agent, using water, the hot method of alcohol mixed solvent, using method from bottom to top by controlling reaction time, reaction condition to prepare magnetic colloid core shell structure α Fe2O3.The inventive method is simple and feasible, and magnetic colloid core shell structure α Fe are realized first2O3Synthesis, the α Fe of core shell structure2O3With magnetic, nontoxic, wide material sources and it is with low cost the features such as, therefore with important potential practical value.
Description
Technical field
The invention belongs to the synthesis technical field of core-shell structured nanomaterials, and in particular to a kind of magnetic colloid core shell structure
α-Fe2O3Preparation method.
Background technology
Compared with single nano-particle, the three-dimensional super-structure being made up of nano particle shows excellent physics and chemistry
Performance, this complicated superstructure that basic construction unit is assembled into function causes chemistry, physics and material supply section educational circles and ground
Study carefully the broad interest of scholar.Colloform texture（Colloidosome）It is one of this three-dimensional super-structure, is used as one in superstructure
The colloform texture of important kind is planted, is microcapsules or microballoon with hollow structure and shell, shell is usually the glue by accumulating
Shape particle or the colloidal particle of solidification composition.Since researcher uses micron-sized polystyrene spheres（PS balls）And water-in-oil type
Suspension synthesize first after colloid, its excellent mechanical stability, the magnetic of controllable particle diameter distribution and precursor particle,
Optics, photoluminescent property cause the interest of numerous scientific research personnel, current numerous studies its released in drug delivery, spices and dyestuff
Put, the potential application in terms of energy stores and photonic device.
However, complicated building-up process is the principal element for restricting colloform texture nano material practical application.Conventional synthesis
The method of colloid is first to synthesize colloidal spheres, then realizes the self assembly of colloidal particle in water-oil interface.The process is comparatively laborious, consumption
When, limit the practical application of colloid.Scientific workers are directed to developing method simple and easy to apply improving the reality of colloid
Border application, Pang etc. is using tert-butylamine as structure directing agent, polyvinylpyrrolidone（PVP）As surfactant, pass through
Simple and effective one-step method synthesizes the Fe-soc-MOF superstructures of three-dimensional hollow structure using emulsion template（That is colloid）.Yu classes
Topic group describes a kind of chemical method of novel one-step synthesis colloid, and high yield synthesizes formaldehyde resin（PFR）, Ag@PFR
It is produced with Au@PFR.However, the method for easy controllable synthesis colloid is still huge challenge, although the synthesis of colloid is
Through achieving part achievement, but the colloid of core shell structure is not synthesized so far.
With the development in the fields such as chemical, environment, biomaterial and biomedicine, nanometer technology and other subject
Intersect sexual development to be taken seriously.Application major embodiment of the nano material in medical science solves the targeting of medicine using nanometer technology
Property, nano material loads onto sensor or idiosyncratic carrier, the special mechanical property using nano material and utilizes nano material
Skin effect etc..Nanometer technology has been applied to the research of pharmaceutical carrier, and magnetic nanoparticle is sent with medicine formation compound
Enter in vivo, can be accurate to up to site of pathological change to cure disease by the guide effect of external magnetic field.Magnetic colloid nucleocapsid knot
α-the Fe of structure2O3, because its magnetic, nontoxic, wide material sources and it is with low cost the features such as, study simple possible synthetic method will have
There are important significance of scientific research and practical value.
The content of the invention
Present invention solves the technical problem that there is provided a kind of magnetic colloid core shell structure α-Fe2O3Preparation method, the party
Method is using glycine as structure directing agent, using water, the hot method of alcohol mixed solvent, using method from bottom to top control the reaction time,
Reaction condition prepares the α-Fe of magnetic colloid core shell structure2O3。
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, a kind of magnetic colloid core shell structure α-Fe2O3's
Preparation method, it is characterised in that concretely comprise the following steps：0.8mmol iron chloride and 0.3g structure directing agent glycine are dissolved in 2mL and gone
Ionized water with the mixed solution of 18mL ethanol, persistently stirring 5min, mixture then being transferred into reaction under nitrogen protection
In 160 DEG C of heating response 12h in kettle, reaction end is naturally cooled to after room temperature, and precipitation is collected by centrifugation, is repeatedly washed with ethanol,
Magnetic colloid core shell structure α-Fe are dried to obtain then at 60 DEG C2O3。
The invention has the advantages that：The present invention realizes magnetic colloid core shell structure α-Fe first2O3Synthesis,
Using glycine as structure directing agent, prepared using water, the hot step of method one of alcohol mixed solvent, method is simple and feasible, rubber polymer
Body size can pass through reaction condition control；α-the Fe of core shell structure2O3With magnetic, nontoxic, wide material sources and the spy such as with low cost
Point, therefore with important potential practical value.
Brief description of the drawings
Fig. 1 is magnetic colloid core shell structure α-Fe made from the embodiment of the present invention2O3XRD；
Fig. 2 is magnetic colloid core shell structure α-Fe prepared by the embodiment of the present invention2O3SEM figures and TEM figures, a-e is magnetic in figure
Property colloid core shell structure α-Fe2O3SEM photograph, f-g be magnetic colloid core shell structure α-Fe2O3TEM photos, in g in accompanying drawing
For magnetic colloid core shell structure α-Fe2O3HRTEM photos.
Embodiment
With reference to specific embodiment, the invention will be further described, but simultaneously the invention is not limited in any way
Content.
Embodiment
Weigh 0.8mmol iron chloride（FeCl3·6H2O, analyzes pure, Chemical Reagent Co., Ltd., Sinopharm Group）And
0.3g glycine（Analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group）It is dissolved in the mixing of 2mL deionized waters and 18mL ethanol
In solution, in persistently stirring 5min on magnetic stirring apparatus in nitrogen environmental protection, mixture is then transferred to 50mL poly- four
In the reactor of PVF inner bag, in 160 DEG C of heating response 12h, reaction end is naturally cooled to after room temperature, and it is heavy to be collected by centrifugation
Form sediment, repeatedly washed with ethanol, magnetic colloid core shell structure α-Fe are dried to obtain then at 60 DEG C2O3。
X-ray powder diffraction is measured to gained sample（XRD）Collection of illustrative plates is as shown in figure 1, all diffraction maximums can
Index turns to the α-Fe of hexagonal phase2O3（Standard card is JCPDS No. 33-0664）, impurity peaks appearance, does not show product
It is pure hexagonal phase α-Fe2O3, sharp peak type imply that sample has good crystallinity.
Fig. 2 is that magnetic colloid core shell structure α-Fe are made in the present embodiment2O3SEM figures and TEM figures, a-e shows institute in figure
Obtain α-Fe2O3The SEM photograph of sample, from the SEM photograph of low power（A and b）It can be seen that sample is the spherical colloid of about 3 μm of diameter
Structure, α-Fe2O3The shell of colloid is assembled by about 500nm nanometer plate, and c illustrates a complete core shell structure, accordingly
The SEM photograph of high magnification nucleocapsid is shown in d and e, from d as can be seen that internal core be also be about 100nm by less diameter nanometer
Disk is constituted, and can be apparent from observing these nanometer plates from d and e and is assembled by less nano particle, core-shell glue structure
Further it can be verified by TEM photos, as shown in f in Fig. 2 and g.HRTEM pictures（It is built in g）Show nanometer
Particle clearly lattice fringe, spacing of lattice is 0.368nm and 0.267nm, corresponds respectively to α-Fe2O3's（012）Crystal face and
（014）Crystal face, HRTEM results show that colloid has good crystallinity, with the XRD spectrum analysis result phase one in Fig. 1
Cause.
Embodiment above describes general principle, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (1)
1. a kind of magnetic colloid core shell structure α-Fe2O3Preparation method, it is characterised in that concretely comprise the following steps：By 0.8mmol chlorinations
Iron and 0.3g structure directing agent glycine are dissolved in 2mL deionized waters with the mixed solution of 18mL ethanol, holding under nitrogen protection
Mixture, is then transferred in reactor in 160 DEG C of heating response 12h, reaction end naturally cools to room by continuous stirring 5min
Wen Hou, is collected by centrifugation precipitation, is repeatedly washed with ethanol, and magnetic colloid core shell structure α-Fe are dried to obtain then at 60 DEG C2O3。
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| CN201710249533.7A CN106986391A (en) | 2017-04-17 | 2017-04-17 | A kind of magnetic colloid core shell structure α Fe2O3Preparation method |
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| CN201710249533.7A CN106986391A (en) | 2017-04-17 | 2017-04-17 | A kind of magnetic colloid core shell structure α Fe2O3Preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439482A (en) * | 2018-05-24 | 2018-08-24 | 合肥学院 | A kind of grain size and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder |
| CN113670991A (en) * | 2021-09-08 | 2021-11-19 | 大连理工大学 | Hematite-based single crystal room temperature gas-sensitive material exposing high-energy crystal face, and preparation method and application thereof |
-
2017
- 2017-04-17 CN CN201710249533.7A patent/CN106986391A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439482A (en) * | 2018-05-24 | 2018-08-24 | 合肥学院 | A kind of grain size and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder |
| CN113670991A (en) * | 2021-09-08 | 2021-11-19 | 大连理工大学 | Hematite-based single crystal room temperature gas-sensitive material exposing high-energy crystal face, and preparation method and application thereof |
| CN113670991B (en) * | 2021-09-08 | 2024-01-30 | 大连理工大学 | Hematite-based monocrystal room temperature gas-sensitive material exposing high-energy crystal face, and preparation method and application thereof |
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Application publication date: 20170728 |