CN109052485A - A kind of preparation method of magnetic ferroferric oxide nanometer particle - Google Patents
A kind of preparation method of magnetic ferroferric oxide nanometer particle Download PDFInfo
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- CN109052485A CN109052485A CN201811081704.0A CN201811081704A CN109052485A CN 109052485 A CN109052485 A CN 109052485A CN 201811081704 A CN201811081704 A CN 201811081704A CN 109052485 A CN109052485 A CN 109052485A
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- ferroferric oxide
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- 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)
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- 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
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- 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
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Abstract
The present invention relates to a kind of preparation methods of magnetic ferroferric oxide nanometer particle, comprising the following steps: (1) weighs FeCl3·6H2O and FeCl2·4H2O solid is added distilled water dissolution, stirs to get clear solution；(2) under steady temperature, ammonium hydroxide is added dropwise into clear solution obtained in step (1), lower reaction is stirred by ultrasonic, sodium citrate solution is added dropwise after the reaction was completed；(3) after reaction, liquid is placed in right above magnet and is stood, taken supernatant liquid to wash drying, obtain magnetic ferroferric oxide nanometer particle.Compared with prior art, the magnetic ferroferric oxide nanometer grain diameter that the present invention is prepared is smaller, and performance is stablized, and has good dispersibility in an aqueous medium.
Description
Technical field
The present invention relates to a kind of preparation methods of nano material, more particularly, to a kind of magnetic ferroferric oxide nanometer particle
Preparation method.
Background technique
Magnetic nanoparticle is one of the research hotspot of world today's Material Field, is the one kind with wide application prospect
Functional material.Magnetic nanoparticle is the magnetic Nano material applied earliest, is widely used in magnetic recording material, magnetic fluid
Preparation and the fields such as powder core covering material.The feature of powder core is to coat a layer insulating on ferromagnetic particle surface to be situated between
Matter reduces eddy-current loss to increase resistivity, improves transformation efficiency.Common covering material has organic matter (such as resin), inorganic
Object (ceramics) etc., however, reducing the percentage composition of ferromagnetic material, therefore saturation induction due to the introducing of non-magnetic particle
Intensity and magnetic conductivity are accordingly reduced, therefore, as the nano ferriferrous oxide granule of excellent magnetic, because there is preparation simply, than
The features such as surface area is larger, magnetic anisotropy, and be attempted in the covering material applied to powder core.The system of nano magnetic particle
Preparation Method mainly has sol-gel method, pyrolysismethod, microemulsion method, solvent-thermal method, chemical coprecipitation etc..
If you need to be applied in powder core, then prepared ferroferric oxide nano granules is required to have granularity tiny
And uniform and conjunction favorable dispersibility, the particle that the above method prepares is in general easy to reunite, and granularity is big, also further
Carrying out dispersion could use, it is therefore desirable to improve to above method.
With the development of synthesis and detection technique, it is gradually improved to the size and shape control of magnetic nanoparticle.But it is right
It is still one in the synthesis of smaller size and the uniform particle of dispersibility to challenge.Existing coprecipitation prepares single-size
Magnetic-particle it is comparatively mature, but there are experimental implementation complexity, equipment such as need to heat at the devices, and particle dispersion is poor and energy
The deficiencies of big is consumed, to limit its further popularization and application.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of magnetic four oxidations three
The preparation method of iron nano-particle.
The whole preparation step of scientific design of the present invention and crucial process conditions, first using ultrasonic oscillation and co-precipitation
The lesser magnetic ferroferric oxide nanometer particle of mode synthesis particle partial size that method combines, then carries out surface with sodium citrate and repairs
Decorations, ferroferric oxide nano granules are dispersed, and four oxidations three of the favorable dispersibility that average grain diameter is 13nm or so are finally made
Iron nano-particle provides strong technical foundation in powder core preparation field for the magnetic nanoparticle of ferroso-ferric oxide.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of magnetic ferroferric oxide nanometer particle, which comprises the following steps:
(1) FeCl is weighed3·6H2O and FeCl2·4H2O solid is added distilled water dissolution, stirs to get clear solution；
(2) under steady temperature, ammonium hydroxide is added dropwise into clear solution obtained in step (1), lower reaction is stirred by ultrasonic,
After the reaction was completed, sodium citrate solution is added dropwise；
(3) after reaction, liquid is placed in right above magnet and is stood, taken supernatant liquid to wash drying, obtain magnetism
Ferroferric oxide nano granules.
As a preferred embodiment of the above solution, in step (1): FeCl3·6H2O and FeCl2·4H2The molar ratio of O solid is 2:
1。
As a preferred embodiment of the above solution, in step (1): the additive amount and FeCl of distilled water3·6H2The ratio of O solid is
(50mL):(0.002mol)。
As a preferred embodiment of the above solution, in step (2): the volume ratio of ammonium hydroxide and distilled water is 1:25.
The process conditions reacted in step (2) as a preferred embodiment of the above solution, are as follows: 25 DEG C of steady temperature, reaction time 1-
2h。
As a preferred embodiment of the above solution, in step (2): the sodium citrate solution concentration is 0.02mol/L, sodium citrate
The additive amount and FeCl of solution2·4H2The ratio of O is 0.1-0.2mL:0.001mol, and addition sodium citrate is to four oxidation three of magnetism
Iron nano-particle is surface modified, and prevents from reuniting.
As a preferred embodiment of the above solution, in step (2): reacting, can accelerate anti-under ultrasound and the collective effect of stirring
Answer rate, shatter product, micronized particles
As a preferred embodiment of the above solution, in step (3): time of repose 30min.
The operation washed in step (3) as a preferred embodiment of the above solution, are as follows: cleaned 4 times using acetone, be then added first
Straight alcohol cleaning is analyzed, deionized water cleaning is added.
Process conditions dry in step (3) as a preferred embodiment of the above solution, are as follows: using vacuum drying, temperature is 60 DEG C,
Time is 48h, low temperature, long time drying processing, can obtain that particle is smaller, the ferriferrous oxide nano of favorable dispersibility
Grain.
Compared with prior art, the present invention is based on co-precipitation principle, dexterously used ultrasonic oscillation dispersion and it is coprecipitated
Shallow lake method is prepared for the lesser magnetic ferroferric oxide nanometer particle of grain diameter, and makes magnetic by the surface modification of sodium citrate
Property ferroferric oxide nano granules dispersibility it is more preferable.Experimental facilities of the present invention is simple, easy to operate, at low cost, and low energy consumption, made
Standby nanometer Fe3O4The favorable dispersibility of magnetic-particle, performance are stablized, can be answered extensively very well as the covering material of powder core
For fields such as machinery, electronics, optics, magnetics, chemical industry and biology.
Detailed description of the invention
The magnetic response of Fig. 1 magnetic ferroferric oxide nanometer particle prepared by the present invention detects figure；
The XRD diagram of Fig. 2 magnetic ferroferric oxide nanometer particle prepared by the present invention.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The FeCl of 0.002mol is weighed respectively3·6H2The FeCl of O solid particle and 0.001mol2·4H2O solid, is placed in
In beaker, the distilled water of 50mL is added, stirs into clear solution with glass bar；At 25 DEG C of steady temperature, dropwise into solution
The NH of 2mL is added3·H2O reacts 1h under ultrasound and stirring collective effect, the citric acid of 0.02mol/L is added dropwise after reaction
Sodium solution 0.1mL is surface modified；Sufficiently after reaction, liquid is placed in right above magnet, stands 30min, takes out upper liquid
Body then after washed processing, obtains finely dispersed magnetic ferroferric oxide nanometer particle, is then transferred to vacuum baking
In case, 60 DEG C of low temperature drying 48h obtain that particle is smaller, the magnetic ferroferric oxide nanometer particle of favorable dispersibility.
The magnetic Fe that will be prepared3O4Nanoparticle sample is taken pictures, and Fig. 1 show magnetic Fe of the invention3O4Nanometer
Grain carries out magnetic response detection figure, finds out from figure and has synthesized the good ferroferric oxide nano granules of magnetic response.Fig. 2 is to be prepared into
The XRD diagram of the magnetic ferroferric oxide nanometer particle arrived, the diffraction of particle almost consistent with standard diagram from gained diffraction spectrogram
Peak is also relatively more sharp, this shows that preparing particle is Fe3O4Particle and crystallinity is preferable, purity is higher, and according to Scherrer formula meter
It is about 13nm that prepared magnetic ferroferric oxide nanometer mean particle size can be obtained by, which calculating, and grain diameter is smaller.Present invention preparation
The ferroferric oxide nano granules performance of obtained favorable dispersibility is stablized, soilless sticking phenomenon, has in an aqueous medium good
Dispersibility.
Embodiment 2
The FeCl of 0.004mol is weighed respectively3·6H2The FeCl of O solid particle and 0.002mol2·4H2O solid, is placed in
In beaker, the distilled water of 100mL is added, stirs into clear solution with glass bar；At 25 DEG C of steady temperature, dropwise into solution
The NH of 4mL is added3·H2O reacts 2h under ultrasound and stirring collective effect, the citric acid of 0.02mol/L is added dropwise after reaction
Sodium solution 0.4mL is surface modified；Sufficiently after reaction, liquid is placed in right above magnet, stands 30min, takes out upper liquid
Body then after washed processing, obtains finely dispersed magnetic ferroferric oxide nanometer particle, is then transferred to vacuum baking
In case, 60 DEG C of low temperature drying 48h obtain that particle is smaller, the magnetic ferroferric oxide nanometer particle of favorable dispersibility.
Embodiment 3
The FeCl of 0.002mol is weighed respectively3·6H2The FeCl of O solid particle and 0.001mol2·4H2O solid, is placed in
In beaker, the distilled water of 50mL is added, stirs into clear solution with glass bar；At 25 DEG C of steady temperature, dropwise into solution
The NH of 2mL is added3·H2O reacts 1.5h under ultrasound and stirring collective effect, the lemon of 0.02mol/L is added dropwise after reaction
Acid sodium solution 0.15mL is surface modified；Sufficiently after reaction, liquid is placed in right above magnet, stands 30min, takes out upper layer
Liquid then after washed processing, obtains finely dispersed magnetic ferroferric oxide nanometer particle, is then transferred to vacuum
In baking oven, 60 DEG C of low temperature drying 48h obtain that particle is smaller, the magnetic ferroferric oxide nanometer particle of favorable dispersibility.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (9)
1. a kind of preparation method of magnetic ferroferric oxide nanometer particle, which comprises the following steps:
(1) FeCl is weighed3·6H2O and FeCl2·4H2O solid is added distilled water dissolution, stirs to get clear solution；
(2) under steady temperature, ammonium hydroxide is added dropwise into clear solution obtained in step (1), lower reaction, reaction is stirred by ultrasonic
After the completion, sodium citrate solution is added dropwise；
(3) after reaction, liquid is placed in right above magnet and is stood, supernatant liquid is taken to wash drying, obtain magnetic four oxygen
Change three iron nano-particles.
2. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(1) in: FeCl3·6H2O and FeCl2·4H2The molar ratio of O solid is 2:1.
3. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(1) in: the additive amount and FeCl of distilled water3·6H2The ratio of O solid is (50mL): (0.002mol).
4. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(2) in: the volume ratio of ammonium hydroxide and distilled water is 1:25.
5. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(2) process conditions reacted in are as follows: 25 DEG C of steady temperature, reaction time 1-2h.
6. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(2) in: the sodium citrate solution concentration is 0.02mol/L, the additive amount and FeCl of sodium citrate solution2·4H2The ratio of O
For (0.1-0.2mL): (0.001mol).
7. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(3) in: time of repose 30min.
8. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(3) operation washed in are as follows: cleaned 4 times using acetone first, analysis straight alcohol cleaning is then added, it is clear to add deionized water
It washes.
9. a kind of preparation method of magnetic ferroferric oxide nanometer particle according to claim 1, which is characterized in that step
(3) dry process conditions in are as follows: using vacuum drying, temperature is 60 DEG C, time 48h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650974A (en) * | 2019-01-14 | 2019-04-19 | 湖南大学 | Nitrogen loss and the method for improving composting production fertilizer efficiency in composting process are reduced using ferriferous oxide nano material |
| CN111330552A (en) * | 2019-12-07 | 2020-06-26 | 江苏省农业科学院 | Method for purifying plant anthocyanin by using magnetic nano material |
| CN112047385A (en) * | 2020-08-19 | 2020-12-08 | 安徽景成新材料有限公司 | Method for preparing superfine nano ferroferric oxide by ultrasonic spraying method |
| CN114209845A (en) * | 2021-12-18 | 2022-03-22 | 苏州健雄职业技术学院 | Preparation method of magnetic nanoparticles |
| CN116259459A (en) * | 2023-02-22 | 2023-06-13 | 上海蓝载信息科技有限公司 | Super-magnetic citric acid coated iron oxide nanoparticle, and synthesis method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294908A (en) * | 2015-11-20 | 2016-02-03 | 云南健牛生物科技有限公司 | Synthesis method and applications of magnetic nano high-molecular polymer |
-
2018
- 2018-09-17 CN CN201811081704.0A patent/CN109052485A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294908A (en) * | 2015-11-20 | 2016-02-03 | 云南健牛生物科技有限公司 | Synthesis method and applications of magnetic nano high-molecular polymer |
Non-Patent Citations (1)
| Title |
|---|
| 张赛等: ""环境友好型水基四氧化三铁磁流体的制备与表征"", 《精细化工》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650974A (en) * | 2019-01-14 | 2019-04-19 | 湖南大学 | Nitrogen loss and the method for improving composting production fertilizer efficiency in composting process are reduced using ferriferous oxide nano material |
| CN109650974B (en) * | 2019-01-14 | 2021-07-09 | 湖南大学 | Method for reducing nitrogen loss in composting process and improving fertilizer efficiency of compost product by using iron oxide nano material |
| CN111330552A (en) * | 2019-12-07 | 2020-06-26 | 江苏省农业科学院 | Method for purifying plant anthocyanin by using magnetic nano material |
| CN112047385A (en) * | 2020-08-19 | 2020-12-08 | 安徽景成新材料有限公司 | Method for preparing superfine nano ferroferric oxide by ultrasonic spraying method |
| CN114209845A (en) * | 2021-12-18 | 2022-03-22 | 苏州健雄职业技术学院 | Preparation method of magnetic nanoparticles |
| CN114209845B (en) * | 2021-12-18 | 2023-11-07 | 苏州健雄职业技术学院 | Preparation method of magnetic nano particles |
| CN116259459A (en) * | 2023-02-22 | 2023-06-13 | 上海蓝载信息科技有限公司 | Super-magnetic citric acid coated iron oxide nanoparticle, and synthesis method and application thereof |
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Application publication date: 20181221 |