CN108417331A - A kind of preparation method of the single gold-coating magnetic nano particle of small scale - Google Patents
A kind of preparation method of the single gold-coating magnetic nano particle of small scale Download PDFInfo
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- CN108417331A CN108417331A CN201810461255.6A CN201810461255A CN108417331A CN 108417331 A CN108417331 A CN 108417331A CN 201810461255 A CN201810461255 A CN 201810461255A CN 108417331 A CN108417331 A CN 108417331A
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- nano particle
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- magnetic
- gold
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Classifications
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- 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
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
-
- 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
-
- 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)
-
- 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
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
-
- 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
Abstract
A kind of preparation method of the single gold-coating magnetic nano particle of small scale, which is characterized in that include the following steps：Step 1, Iron dichloride tetrahydrate and ferric chloride hexahydrate are dissolved in distilled water, are passed through nitrogen, be stirred continuously and heated, while ammonium hydroxide is added, obtain the reactant containing precipitation；Step 2, precipitation is detached with centrifuge, drying in vacuum drying oven is put into after precipitation is cleaned, obtains Fe3O4Nano particle；Step 3, by Fe3O4Nano particle is placed in vacuum tube furnace and handles, and obtains Fe3O4Magnetic nanoparticle；Step 4, by Fe3O4Magnetic nanoparticle is put into the beaker equipped with deionized water, then by one piece of SiO2Substrate is put into beaker, beaker is placed in SiO in microwave oscillation water-bath after vibrating2Substrate takes out, and is put into drying in vacuum drying oven, obtains to surface and be evenly distributed with Fe3O4The SiO of magnetic nanoparticle2Substrate；Step 5, using plated film instrument in SiO2One layer of gold particle is sputtered on substrate, i.e., in SiO2A kind of single gold-coating magnetic nano particle of small scale is obtained on substrate.
Description
Technical field
The present invention relates to a kind of preparation methods of magnetic nanoparticle, and in particular to a kind of small single gold-coating magnetic of scale
The preparation method of nano particle.
Background technology
So far, there is quite a lot of Fe for applied to biomedical sector304Magnetic nanoparticle is ground
Study carefully, to Fe304There has also been more ripe theories for the analysis of the magnetic property of magnetic nanoparticle, but much both in reunion shape
The magnetic property of magnetic nanoparticle is analyzed.Compared to reunion shape magnetic nanoparticle, the small single magnetic nanoparticle energy of scale
It is enough more accurately to analyze microcosmic nanometer magnetic structure and magnetic property (performances such as magnetic domain, magnetic conductivity and magnetic loss), magnetism is received
Application of the rice grain in biomedicine provides crucial technological guidance, therefore to the magnetism of the single magnetic nanoparticle of small scale
Energy research is of great significance and scientific value.Research to magnetic nanoparticle, magnetic force microscopy are one and divide well
Analysis means.But it is sizable tired to go the magnetic property for measuring the single magnetic nanoparticle of small scale to have using magnetic force microscopy
Difficulty, because magnetic nanoparticle will produce the magnetic probe of reunion and magnetic force microscopy due to itself mutual magnetic force
Magnetic force can be generated to nano particle and enable its drift unstable.So needing a kind of small scale that can be solved the above problems single
Gold-coating magnetic nano particle.
Invention content
The present invention is to carry out to solve the above-mentioned problems, and it is an object of the present invention to provide a kind of single gold-coating magnetic of small scale
The preparation method of nano particle.
The present invention provides a kind of preparation methods of the small single gold-coating magnetic nano particle of scale, have such spy
Sign, includes the following steps：
Step 1, divalent iron salt and trivalent iron salt are dissolved in the distilled water of 100-250ml, obtain containing ferrous iron from
The mixed solution of son and ferric ion is stirred continuously the mixed solution and is heated to 55-60 DEG C, simultaneously under nitrogen protection
Ammonium hydroxide is slowly added to until the ph values of mixed solution are 8.5-9.5, obtaining the reaction comprising sediment after reaction 1.5-2.5h is situated between
Matter；
Step 2, sediment is separated from reaction medium using centrifuge, the sediment isolated will sink
It is put into 40-60 DEG C of vacuum drying oven and is dried after starch cleaning, obtain the Fe of grain size 5-15nm3O4Nano particle；
Step 3, first by Fe3O4Nano particle is placed in the vacuum tube furnace that temperature is 450-550 DEG C and keeps the temperature 1.5-2.5h,
Then by Fe3O4Nano particle is cooled to room temperature jointly with vacuum tube furnace, obtains Fe3O4Magnetic nanoparticle；
Step 4, the Fe of 0.2-0.5g is weighed3O4Magnetic nanoparticle is put into the beaker of the deionized water equipped with 40-60ml
In, then by one piece of SiO2Substrate is put into beaker, beaker is placed in SiO in microwave oscillation water-bath after vibrating 50-60min2Base
Piece takes out from beaker, by the SiO of taking-up2After substrate is put into 40-50 DEG C of vacuum drying chamber dry 0.5-1h, surface is obtained
It is evenly distributed with Fe3O4The SiO of magnetic nanoparticle2Substrate；
Step 5, by plated film instrument in such a way that metal spraying sputters Fe is evenly distributed on surface3O4Magnetic nanoparticle
SiO2The gold particle that a layer thickness is 2-5nm is sputtered on substrate, i.e., in SiO2A kind of single gold-coating magnetic of small scale is obtained on substrate
Property nano particle.
In a kind of preparation method of the small single gold-coating magnetic nano particle of scale provided by the invention, can also have
Such feature：Wherein, in step 1, divalent iron salt is Iron dichloride tetrahydrate, and trivalent iron salt is ferric chloride hexahydrate.
In a kind of preparation method of the small single gold-coating magnetic nano particle of scale provided by the invention, can also have
Such feature：Wherein, in step 1, the ratio of ferrous ion and ferric ion is 1:1.5-2.0.
In a kind of preparation method of the small single gold-coating magnetic nano particle of scale provided by the invention, can also have
Such feature：Wherein, in step 2, when sediment undergoes washing, is first cleaned 3-5 times with deionized water, then is cleaned 2-4 times with ethyl alcohol.
In a kind of preparation method of the small single gold-coating magnetic nano particle of scale provided by the invention, can also have
Such feature：Wherein, in step 5, use electric current of the plated film instrument when carrying out metal spraying sputtering is 15-20mA, time 5-8s.
The effect of invention
According to a kind of preparation method of the small single gold-coating magnetic nano particle of scale according to the present invention, because using
The method that magnetic nanoparticle is coated and fixed in gold, so that small scale magnetic nanoparticle can individually disperse simultaneously well
And it is not easy to drift about below magnetic force microscopy.Therefore the single gold-coating magnetic nano particle of the small scale of kind of the present invention is effective
Single stability of the small scale magnetic nanoparticle in performance testing process is improved, is more conducive to and explores magnetic Nano
The magnetic mechanism and essence of grain.
Description of the drawings
Fig. 1 is the small scale magnetic Fe of reunion shape in the embodiment of the present invention one304Nano particle under magnetic microscope
Surface topography map；
Fig. 2 is the small scale magnetic Fe of reunion shape in the embodiment of the present invention one304Nano particle under magnetic microscope
Magnetogram；
Fig. 3 is the single gold-coating magnetic nano particle of small scale in the embodiment of the present invention two under magnetic microscope
Surface topography map；
Fig. 4 is the single gold-coating magnetic nano particle of small scale in the embodiment of the present invention two in magnetic microscope
Under magnetogram.
Specific implementation mode
In order to which the technological means for making the present invention realize is easy to understand with effect, with reference to embodiments and attached drawing is to this
Invention is specifically addressed.
<Embodiment one>
Fig. 1 is the small scale magnetic Fe of reunion shape in the embodiment of the present invention one304Nano particle under magnetic microscope
Surface topography map.
Step 1, ferric chloride hexahydrate and Iron dichloride tetrahydrate are dissolved in the distilled water of 150ml, are obtained containing two
The mixed solution of valence iron ion and ferric ion so that the ratio of ferrous ion and ferric ion is 1 in mixed solution:
1.6, then mixed solution is transferred in 500ml three-necked flasks, leads to nitrogen protection, mechanical agitation is uniform, and three-necked flask is set
It is heated to 55 DEG C in water-bath, is slowly added to ammonium hydroxide until the ph values of mixed solution are 8.5, is obtained comprising heavy after reacting 1.8h
The reaction medium of starch.
Step 2, gained is precipitated using centrifuge and is separated from reaction medium, the precipitation of gained first uses deionized water
Cleaning 3 times, then after clean 2 times with ethyl alcohol, it is put into freeze-day with constant temperature in 40 DEG C of vacuum drying oven, the Fe of obtained grain size 15nm or so304
Particle.
Step 3, by Fe obtained304Nano particle, which is positioned over to be warming up in 450 DEG C of vacuum tube furnace, keeps the temperature 1.5h, so
Afterwards by Fe304Nano particle is cooled to room temperature jointly with vacuum tube furnace, and the reunion of grain size 15nm as shown in Figure 1 or so is made
The Fe of the small scale of shape304Magnetic nanoparticle.
Fig. 2 is the small scale magnetic Fe of reunion shape in the embodiment of the present invention one304Nano particle under magnetic microscope
Magnetogram.
As shown in Fig. 2, the Fe of the present embodiment304Apparent brilliant black region is presented in nano particle magnetogram, and brilliant black corresponds to respectively
The magnetic anode and magnetic cathode of nano particle illustrate that reunion shape nano particle magnetogram is detected.
<Embodiment two>
Step 1, ferric chloride hexahydrate and Iron dichloride tetrahydrate are dissolved in the distilled water of 250ml, are obtained containing two
The mixed solution of valence iron ion and ferric ion so that the ratio of ferrous ion and ferric ion is 1 in mixed solution:
2, then mixed solution is transferred in 500ml three-necked flasks, leads to nitrogen protection, mechanical agitation is uniform, and three-necked flask is placed in
60 DEG C are heated in water-bath, be slowly added to ammonium hydroxide until mixed solution ph values be 9, react 2.5h after obtain include sediment
Reaction medium.
Step 2, gained is precipitated using centrifuge and is separated from reaction medium, the precipitation of gained first uses deionized water
Cleaning 5 times, then after clean 4 times with ethyl alcohol, it is put into freeze-day with constant temperature in 60 DEG C of vacuum drying oven, the Fe of obtained grain size 10nm or so304
Particle.
Step 3, by Fe obtained304Nano particle, which is positioned over to be warming up in 500 DEG C of vacuum tube furnace, keeps the temperature 2.5h, so
Afterwards by Fe304Nano particle is cooled to room temperature jointly with vacuum tube furnace, and the Fe of grain size 10nm is made304Magnetic nanoparticle.
Step 4, the Fe of the grain size 10nm of 0.2g steps 3 preparation is weighed304Magnetic nanoparticle is put into equipped with 60ml deionizations
In the beaker of water, and by one piece of SiO2Substrate is put into beaker, which is placed in microwave oscillation water-bath and vibrates 1h, then
By SiO2Substrate is put into freeze-day with constant temperature 1h in 50 DEG C of vacuum drying chamber after being taken out in beaker, obtains that surface is evenly dispersed to be had
Fe3O4The SiO of magnetic nanoparticle2Substrate.
Step 5, using plated film instrument in SiO2The gold of a layer thickness 5nm is sputtered on substrate by the method that metal spraying sputters
Grain, the operating current 20mA of plated film instrument, metal spraying sputtering time is 8s, i.e., in SiO2Substrate must arrive surface and be coated with gold nano grain
The single Fe of small scale304Nano particle.
Fig. 3 is the single gold-coating magnetic nano particle of small scale in the embodiment of the present invention two under magnetic microscope
Surface topography map.
As shown in figure 3, the small single Fe of scale304Nano grain surface almost all is covered by gold nano grain, therefore can be with
Learn that the surface topography map that detected is the single Fe of small scale304The gold nano grain of nano grain surface.
Fig. 4 is the single gold-coating magnetic nano particle of small scale in the embodiment of the present invention two in magnetic microscope
Under magnetogram.
As shown in figure 4, the single small scale Fe of the present embodiment two304Have in magnetic nanoparticle magnetogram and to be apparent from
Comparison of light and shade region illustrates clearly to detect the magnetogram of single small scale magnetic nanoparticle using our method
Out.
The effect of embodiment
According to embodiment one and embodiment two it is found that when magnetic nanoparticle is coated and fixed using gold, magnetic Nano
The good dispersion of grain, magnetic nanoparticle can individually scatter and single magnetic nanoparticle enabled to fix,
When solving the magnetic behavior for observing magnetic nanoparticle under magnetic force microscopy, because of the magnetism of magnetic probe and nano particle
The problem of interacting and magnetic nanoparticle caused to drift about.Therefore it is prepared using the method that magnetic nanoparticle is coated and fixed in gold
The obtained single gold-coating magnetic nano particle of small scale effectively raises single small scale magnetic nanoparticle and is examined in performance
Stability during survey is more conducive to the magnetic mechanism and essence for exploring magnetic nanoparticle.
The above embodiment is the preferred case of the present invention, is not intended to limit protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the single gold-coating magnetic nano particle of small scale, which is characterized in that include the following steps：
Step 1, divalent iron salt and trivalent iron salt are dissolved in the distilled water of 100-250ml, obtain containing ferrous ion and
The mixed solution of ferric ion is stirred continuously the mixed solution and is heated to 55-60 DEG C, while slowly under nitrogen protection
Ammonium hydroxide is added until the ph values of the mixed solution are 8.5-9.5, obtaining the reaction comprising sediment after reaction 1.5-2.5h is situated between
Matter；
Step 2, the sediment is separated from the reaction medium using centrifuge, the sediment isolated,
It is dried being put into 40-60 DEG C of vacuum drying oven after the sediment undergoes washing, obtains the Fe of grain size 5-15nm3O4Nanometer
Grain；
Step 3, first by the Fe3O4Nano particle is placed in the vacuum tube furnace that temperature is 450-550 DEG C and keeps the temperature 1.5-2.5h,
Then by the Fe3O4Nano particle is cooled to room temperature jointly with the vacuum tube furnace, obtains Fe3O4Magnetic nanoparticle；
Step 4, the Fe of 0.2-0.5g is weighed3O4Magnetic nanoparticle is put into the beaker of the deionized water equipped with 40-60ml
In, then by one piece of SiO2Substrate is put into the beaker, and the beaker is placed in microwave oscillation water-bath and vibrates 50-60min
Afterwards by the SiO2Substrate takes out from the beaker, by the SiO of taking-up2Substrate is put into 40-50 DEG C of vacuum drying chamber
After dry 0.5-1h, obtains to surface and be evenly distributed with the Fe3O4The SiO of magnetic nanoparticle2Substrate；
Step 5, by plated film instrument in such a way that metal spraying sputters the Fe is evenly distributed on surface3O4Magnetic nanoparticle
The SiO2The gold particle that a layer thickness is 2-5nm is sputtered on substrate, i.e., in the SiO2It is single that a kind of small scale is obtained on substrate
Gold-coating magnetic nano particle.
2. a kind of preparation method of small single gold-coating magnetic nano particle of scale according to claim 1, feature exist
In：
Wherein, in the step 1, the divalent iron salt is Iron dichloride tetrahydrate, and the trivalent iron salt is ferric chloride hexahydrate.
3. a kind of preparation method of small single gold-coating magnetic nano particle of scale according to claim 1, feature exist
In：
Wherein, in the step 1, the ratio of the ferrous ion and the ferric ion is 1:1.5-2.0.
4. a kind of preparation method of small single gold-coating magnetic nano particle of scale according to claim 1, feature exist
In：
Wherein, in the step 2, when sediment undergoes washing, is first cleaned 3-5 times with deionized water, then is cleaned 2-4 times with ethyl alcohol.
5. a kind of preparation method of small single gold-coating magnetic nano particle of scale according to claim 1, feature exist
In：
Wherein, in the step 5, use electric current of the plated film instrument when carrying out metal spraying sputtering is 15-20mA, time 5-
8s。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390453A (en) * | 2020-11-25 | 2021-02-23 | 上海交通大学 | Modified magnetic Fe3O4Powder, method for the production thereof and use thereof |
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| EP1532274A2 (en) * | 2002-06-28 | 2005-05-25 | Purdue Research Foundation | Magnetic nanomaterials and methods for detection of biological materials |
| CN101108423A (en) * | 2007-08-17 | 2008-01-23 | 湖南工业大学 | Novel method of manufacturing Fe3O4/Au magnetic complex nano particle |
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| CN112390453A (en) * | 2020-11-25 | 2021-02-23 | 上海交通大学 | Modified magnetic Fe3O4Powder, method for the production thereof and use thereof |
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