CN106905968B - The preparation method of magnetic fluorescence material - Google Patents
The preparation method of magnetic fluorescence material Download PDFInfo
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- CN106905968B CN106905968B CN201710106721.4A CN201710106721A CN106905968B CN 106905968 B CN106905968 B CN 106905968B CN 201710106721 A CN201710106721 A CN 201710106721A CN 106905968 B CN106905968 B CN 106905968B
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 7
- 239000012188 paraffin wax Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000000295 emission spectrum Methods 0.000 claims description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000000696 magnetic material Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7729—Chalcogenides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0018—Diamagnetic or paramagnetic materials, i.e. materials with low susceptibility and no hysteresis
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Biophysics (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Luminescent Compositions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
A kind of preparation method of magnetic fluorescence material, ethylene glycol, Fe3+NaOH is added after mixing with europium ion, then adds paraffin, is sufficiently stirred and is placed in 250 DEG C of reaction kettles 10 hours or more to obtain the final product.A kind of preparation method of magnetic fluorescence material provided by the invention, series nanometer grade material, using hydro-thermal method one-step synthesis, method is simple, is easy to utilize.Material obtained has fluorescent characteristic, it may have superparamagnetic characteristic.
Description
Technical field
The present invention relates to a kind of preparation method of composite material more particularly to a kind of materials with magnetism and fluorescence property
Material, and preparation method thereof.
Background technique
Fluorescent material is a kind of material to shine after by the irradiation such as ultraviolet light, laser, after the irradiation outside material absorption,
The light consistent with its characteristic frequency can be absorbed, the first excited electronic state is risen to by original energy level or the second electronics swashs
Send out each different vibration levels and rotational energy level in state.Molecule in excitation state passes through the processes such as vibration relaxation, internal conversion
The lowest vibration energy level of the first excited state of molecule is transitted to, in this course they and congeneric elements or other molecular collisions
And energy is consumed, and no longer shine.
Chinese invention patent 201210112174.8 discloses a kind of fluorescence magnetic complex microsphere and graphene oxide is compound
Material and preparation method thereof, using graphene oxide composite material as carrier, and in its surface modification carboxylic group, then by fluorescence magnetic
Complex microsphere surface modification amino group, the carboxylic group and fluorescence magnetic for modifying surface of graphene oxide using Graft Method are multiple
It closes and forms amide between the amino group of microsphere surface modification, fluorescence magnetic complex microsphere is grafted on graphene oxide composite material table
Face obtains fluorescence magnetic complex microsphere and graphene oxide composite material.Fluorescence magnetic complex microsphere and graphene oxide composite wood
Material be in micro-spherical particle, partial size be 50nm~1,000nm, saturation magnetization be 10~50emu/g, emission peak be 500nm~
600nm。
Chinese invention patent 201310727257.2 discloses a kind of water soluble fluorescence magnetic corpusculum and preparation method thereof, uses
Biomineralization-modification is prepared for a kind of fluorescent magnetic corpusculum of cysteine modified, the fluorescent magnetic corpusculum be it is water-soluble,
And fluorescent stability is good, fluorescence intensity is high.Meanwhile preparation method of the invention is simple, easily operated, and joins without noxious material
With substantially increase application of the fluorescent magnetic corpusculum in terms of magnetic target and fluorescent tracing.
These technologies usually require that magnetic material can be assigned just now by being chemically modified with fluorescent characteristic.Also there is use
SiO2The mode of package obtains in the practice of the magnetic material with fluorescent characteristic, mixes according to by magnetic material with fluorescent material
Preparation method, it will usually encounter product and be magnetic, but do not have fluorescent characteristic, or there is fluorescent characteristic, but magnetic disappear.
Summary of the invention
It is an object of the present invention to provide a kind of preparation methods of magnetic fluorescence material, have fluorescent characteristic to obtain
Magnetic material.
It is another object of the present invention to provide a kind of magnetic-particles with fluorescent characteristic.
A kind of preparation method of magnetic fluorescence material provided by the invention, steps are as follows:
Ethylene glycol, Fe3+NaOH is added after mixing with europium ion, then adds paraffin, is sufficiently stirred and is placed on 250 DEG C of reaction kettles
In 10 hours or more to obtain the final product.
The preparation method of another kind magnetic fluorescence material provided by the invention, steps are as follows:
Solvent ethylene glycol and Fe3+With europium ion (Fe3+With europium ion molar ratio be 8: 1) mix after, be separately added into NaOH and
Paraffin, 10 hours or more in 250 DEG C of reaction kettles for stirring to obtain the final product.
The preparation method of various magnetic fluorescence materials provided by the invention, ethylene glycol dosage such as: 30ml.
The preparation method of various magnetic fluorescence materials provided by the invention, NaOH dosage such as: 0.5g.
The preparation method of various magnetic fluorescence materials provided by the invention, paraffin dosage such as: 5ml.
The preparation method of various magnetic fluorescence materials provided by the invention, Fe3+Such as: FeCl3And FeCl3·6H2O。
Through detecting, magnetic fluorescence material series nanometer grade material produced by the present invention, magnetic saturation intensity 76A/m, transmitting
Spectrum is 680nm~720nm, and excitation spectrum is 380nm~410nm.
Technical solution of the present invention realize the utility model has the advantages that
The preparation method of magnetic fluorescence material provided by the invention, using hydro-thermal method one-step synthesis, method is simple, is easy to benefit
With.Material obtained has fluorescent characteristic, it may have superparamagnetic characteristic.
Specific embodiment
Technical solution of the present invention described in detail below.The embodiment of the present invention be merely illustrative of the technical solution of the present invention and
It is unrestricted, although being described the invention in detail referring to preferred embodiment, those skilled in the art should understand that,
Can with modification or equivalent replacement of the invented technical scheme, without departing from the spirit and scope of the technical solution of the present invention,
It should all cover within the scope of the claims of the present invention.
Embodiment
Ethylene glycol 30ml, 1.08g FeCl3·6H2O, 0.1mol/L europium ion 5ml, are added 0.5g after mixing
NaOH and 5ml paraffin, stirring, 10 hours in 250 DEG C of reaction kettles, is cleaned three times later to obtain the final product.
Through detecting, the magnetic saturation intensity of magnetic fluorescence material is 76A/m, and emission spectrum is 680nm~720nm, exciting light
Spectrum is 380nm~410nm.
Claims (9)
1. a kind of preparation method of magnetic fluorescence material, it is characterised in that steps are as follows:
Ethylene glycol, Fe3+NaOH is added after mixing with europium ion, adds paraffin mixing is sufficiently stirred and be placed on 250 DEG C of reaction kettles
In 10 hours or more to obtain the final product.
2. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that the Fe3+With the europium
Molar ratio is 8: 1.
3. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that the ethylene glycol dosage is
30ml。
4. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that the NaOH dosage is
0.5g。
5. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that the paraffin dosage is
5ml。
6. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that the Fe3+It is selected from
FeCl3And FeCl3·6H2The one or more of O.
7. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that material magnetic saturation obtained is strong
Degree is 76A/m.
8. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that material Emission spectrum obtained
For 680nm~720nm.
9. the preparation method of magnetic fluorescence material according to claim 1, it is characterised in that material emitted light spectrum obtained
For 380nm~410nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710106721.4A CN106905968B (en) | 2017-02-24 | 2017-02-24 | The preparation method of magnetic fluorescence material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710106721.4A CN106905968B (en) | 2017-02-24 | 2017-02-24 | The preparation method of magnetic fluorescence material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106905968A CN106905968A (en) | 2017-06-30 |
| CN106905968B true CN106905968B (en) | 2019-05-24 |
Family
ID=59207919
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710106721.4A Active CN106905968B (en) | 2017-02-24 | 2017-02-24 | The preparation method of magnetic fluorescence material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106905968B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616593A (en) * | 2004-11-03 | 2005-05-18 | 东南大学 | Super fine fusiform fluorescent paramagnetic rare-earth granular material and its preparing method |
| CN1888007A (en) * | 2006-07-21 | 2007-01-03 | 上海师范大学 | Nanometer magnetic fluorescent microsphere and its prepn and application |
| CN101055782A (en) * | 2007-03-09 | 2007-10-17 | 上海师范大学 | A making method for novel biological compatible magnetic fluorescence nano particle |
| CN102115145A (en) * | 2010-11-23 | 2011-07-06 | 吉林大学 | Preparation method of rare earth europium nano crystal with fluorescence and magnetism |
| CN102660255A (en) * | 2012-04-20 | 2012-09-12 | 北京化工大学 | Magnetic fluorescent nanoparticle with biological activity and method for preparing magnetic fluorescent nanoparticle |
-
2017
- 2017-02-24 CN CN201710106721.4A patent/CN106905968B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616593A (en) * | 2004-11-03 | 2005-05-18 | 东南大学 | Super fine fusiform fluorescent paramagnetic rare-earth granular material and its preparing method |
| CN1888007A (en) * | 2006-07-21 | 2007-01-03 | 上海师范大学 | Nanometer magnetic fluorescent microsphere and its prepn and application |
| CN101055782A (en) * | 2007-03-09 | 2007-10-17 | 上海师范大学 | A making method for novel biological compatible magnetic fluorescence nano particle |
| CN102115145A (en) * | 2010-11-23 | 2011-07-06 | 吉林大学 | Preparation method of rare earth europium nano crystal with fluorescence and magnetism |
| CN102660255A (en) * | 2012-04-20 | 2012-09-12 | 北京化工大学 | Magnetic fluorescent nanoparticle with biological activity and method for preparing magnetic fluorescent nanoparticle |
Non-Patent Citations (2)
| Title |
|---|
| EuII-containing Cryptates as Contrast Agents for Ultra-high Field Strength;Joel Garcia等;《Chemical Communications》;20111102;12858-12860 |
| Magnetic Fe3O4 Nanoparticles Coupled with a Fluorescent Eu Conplex for Dual Imaging Applications;Pinxian Xi等;《Chem.Comuum.》;20120123;2952-2954 |
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| Publication number | Publication date |
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| CN106905968A (en) | 2017-06-30 |
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Effective date of registration: 20231023 Address after: Room 201, 2nd Floor, Building 1, No. 18 Huanyuan North Road, Zhongtai Street, Yuhang District, Hangzhou City, Zhejiang Province, 310000 Patentee after: Hangzhou Bochuang Biotechnology Co.,Ltd. Address before: 325035 Wenzhou City National University Science Park incubator, No. 38 Dongfang South Road, Ouhai District, Wenzhou, Zhejiang Patentee before: WENZHOU MEDICAL University |