KR20160088700A - Wustite particle and preparation method thereof - Google Patents
Wustite particle and preparation method thereof Download PDFInfo
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- KR20160088700A KR20160088700A KR1020150008115A KR20150008115A KR20160088700A KR 20160088700 A KR20160088700 A KR 20160088700A KR 1020150008115 A KR1020150008115 A KR 1020150008115A KR 20150008115 A KR20150008115 A KR 20150008115A KR 20160088700 A KR20160088700 A KR 20160088700A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/121—Coherent waves, e.g. laser beams
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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
- C01G49/04—Ferrous oxide (FeO)
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/60—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing iron, cobalt or nickel
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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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- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
Description
The present invention relates to a Vistite particle showing a luminescence property formed by phase change and a method for producing the same.
It is known that metal oxide nanoparticles vary in their magnetic, electrical and optical properties depending on their size and shape (Dai, ZR Adv. Func. Mater. 2003, vol.13, p.9). Based on these properties, metal oxide nanoparticles are expected to be applicable to various fields such as magnetic resonance imaging agents, various recording media, catalysts, energy storage, sensors and ferrofluids (Zarur, AJ Nature, 2000, vol.403, p.65; Majetich, SA Science, 1999, vol.284, p.470). Particularly, these nanomaterials have new characteristics as they are synthesized in the size of nanometer (10 -9 m) and they have unique properties for each material. They are used in materials industry, energy environment industry, electronics industry, Has been applied. As a result, it is anticipated that new convergence industries and nano technology markets will be created.
On the other hand, as the nanoparticle chemical synthesis of nanoparticles becomes possible along with the rapid development of nanotechnology, it is applied to a variety of fusion fields and is utilized in such fields as magnetic memories, magnetic sensors, and living cell separation. These nanoparticles have been prepared by a variety of synthetic methods including thermal decomposition of organic metal precursors, decomposition by sonic waves, reduction of metal ions at high temperatures, and reduction in reverse micelles. Among them, a method of heating a solution containing a surfactant to a high temperature and then applying a precursor to the solution for a short period of time, thereby lowering the temperature after the uniform nucleation and inducing the uniform nucleation of the particles And various technologies related thereto have been developed. In addition to these manufacturing methods, it is possible to control the magnetic, optical and electrical properties by controlling the size, crystallinity, and arrangement of the nanoparticles, and various characteristics control studies are progressing according to application fields.
Among these nanoparticles, especially iron oxide nanoparticles, vesstite (Fe 1 - x O), magnetite (Fe 3 O 4 ), maghemite (γ - Fe 2 O 3 ) and hematite (α - Fe 2 O 3 ) Etc., and have various applications such as magnetic resonance imaging contrast agent, magnetic memory device, contaminant trapping, magnetic separation and cell array, and drug delivery due to their unique characteristics. In order to apply these iron oxide nanoparticles to various fields, it is essential to understand the magnetic, electrical and optical properties of the material.
However, among the iron oxide nanoparticles, wustite is an unstable phase at high temperatures and pressures, so it is difficult to obtain through synthesis or phase change. Especially nano-sized vestite is not easy to synthesize. That is, although attempts have been made to synthesize vistite in various research groups by a method such as hydrothermal synthesis or pulsed laser deposition, there is a problem that it is not easy to synthesize nano-sized wovstite. In addition, even if the synthesis is difficult by such a method, there is a problem that it is difficult to obtain desired characteristics peculiar to the vestite because various kinds of iron oxides are mixed in the composition.
The prior art document related to the present invention is Korean Patent No. 10-0604975 (Patent Document 1). Specifically, in
Another prior art document related to the present invention is Korean Patent No. 10-0550194 (Patent Document 2). Specifically, in
SUMMARY OF THE INVENTION The present invention has been conceived to solve the problems described above, and it is an object of the present invention to provide a method for manufacturing a wastewater which is easy to produce and has a high purity, And a method for producing the same.
In order to solve the above problems, the vistite particles according to one embodiment of the present invention
Magnetite or maghemite particles are formed by phase change,
The phase change is achieved through laser irradiation,
And is phase-changed into a single crystal form due to the laser irradiation.
A method for producing vistite particles according to another embodiment of the present invention comprises
1) irradiating a laser to a magnetite or maghemite particle; And
2) phase change of the magnetite or maghemite into the single crystal form of vistite particles through the laser irradiation;
.
The Vistide particles according to the present invention and the method for producing the Vistast particles according to the present invention are formed by phase change to form vistite particles, and it is possible to provide vistite particles formed in a nano size by a simpler method than those produced by the prior art Do. In addition, such vistite particles and a method for producing the same can remarkably increase the purity of vistite particles compared with those of the prior art, and can maintain excellent properties without losing specific properties of vistite.
Fig. 1 is a photograph of a magnetic nanoparticle collected by the following Example 1 under an optical microscope. Fig.
Fig. 2 is a photograph showing a phase change observed in the center portion of the trapped particles, which is a phase change caused by the following Example 2. Fig.
FIG. 3 is a photograph of a phase change observed by the following Example 2, wherein the phase change was observed in the entire region after the collection.
FIG. 4 is a graph showing an X-ray diffraction analysis before and after phase change according to Examples 1 and 2 below.
5 is a transmission electron microscope photograph before and after the phase change according to Example 1 and Example 2 below.
6 is a photograph showing the result of synthesizing the magnetite nanoparticles before the phase change by size.
Therefore, the inventors of the present invention have made intensive researches to develop vistite particles having high purity and specificity to vistite while forming nano-sized vestite particles by a simple method. As a result, Tight particles and a method for producing the same, and have completed the present invention.
Typically, the wustite is an ore of iron (II) oxide. These vestites are gray with a light green color and are named by Fritz Wust (1860-1938). Since such vestite is an unstable phase appearing under high temperature and pressure conditions, it is difficult to synthesize with conventional techniques and it is also difficult to obtain by phase change method. In particular, it is more difficult to synthesize the vestite in the nano-size by applying the conventional technique (for example, pulsed laser deposition, hydrothermal synthesis, etc.) because the vestite is unstable. In addition, even if a lot of efforts are made to synthesize the nano-size, there is a problem that it is very difficult to obtain high purity vistite according to the prior art because the impurities are inevitably mixed in the process when the conventional technology is applied . The present invention has been developed to solve such problems of the prior art.
Specifically, the vesstite (Fe 1 - x O) particles according to the present invention
A magnetite or a maghemite particle is formed by phase change,
The phase change is achieved through laser irradiation,
And is phase-changed into a single crystal form due to the laser irradiation.
The magnetite (Fe 3 O 4 ) or the maghemite (γ-Fe 2 O 3 ) particles may be iron oxide nanoparticles.
As described above, the Vistite particles formed by phase change according to the present invention have been invented in order to solve the problems of the prior art, and the magnetoite or the maghemite is phase-changed into a single crystal by irradiating a laser to the magnetite or the maghemite. To solve the problem. That is, the vestite particles according to the present invention are formed by phase-changing the magnetite or maghemite into a single crystal form by laser irradiation, and the vestite particles formed by the phase-change in this way are not formed by vapor deposition or hydrothermal synthesis The impurities such as other oxides are not mixed so that the purity is high and the vestite is formed only by the phase change. Therefore, it is possible to be formed of nano-sized fine vistite particles. Further, the vestite particles according to the present invention do not contain any other impurities and correspond to maintaining the characteristics unique to vistite. Further, it is a vistite particle made of a monocrystal type rather than a complicated structure as compared with conventional vistite particles or other iron oxide nanoparticles which are not subjected to conventional vapor deposition, hydrothermal synthesis, or the like, and therefore impurities must be contained. Since the conventional wustite particles according to the present invention are unstable phases formed at high temperatures and pressures, it is difficult to form vistite particles that overcome the above problems without mixing impurities in the prior art This is equivalent to a breakthrough improvement.
The vistite particles formed by the phase change show a single crystal form. More specifically, the cluster type of the spinel structure formed by the combination of the particles of several nanometers in size before the phase change is changed into a cubic crystal single crystal form . More specifically, the spinel structure before the phase change is a structure in which a plurality of granules (clusters) form clusters, and the cubic structure after the phase change is formed of one granule, thus forming a clean circle shape. That is, before the phase change, it can be compared to the shape of the bead after the phase change in the gangjeong shape.
This phase change is made possible by irradiating the magnetite or maghemite with a high-energy or high-power laser.
On the other hand, the wavelength of the laser irradiation enabling the phase change is not limited to a specific range as long as it is a numerical range of high energy enabling a phase change. Preferably, the wavelength is 500-1,000 nm, . Also, it is preferable that the irradiation of the laser is performed through a multiphoton laser. In general argon and helium neon monophoton lasers, the coherence of the wavelengths is excellent, but the energy of the phase change is not sufficient. It is difficult to change and is not desirable.
Further, the output of the laser irradiation enabling the phase change is not limited to a specific range as long as it is a high output range enabling phase change, but it is preferable that the output is 60-300 mW. When the output of the laser irradiation is less than 60 mW, it is not preferable to make a phase change because it does not reach the high output required by the present invention to phase-change into vistite particles, and when the output of the laser irradiation exceeds 300 mW It is not preferable because laser irradiation is unnecessarily outputted even though high-power laser irradiation required for phase change is performed, which is uneconomical.
On the other hand, the vistite particles are formed in a nano-size by phase change unlike vistite particles synthesized by a conventional technique. The average particle size of the vistite particles is not particularly limited, but the magnetite or mag- It is preferable that the size of the hematite nanoparticles is not greatly different from that of the hematite nanoparticles. Thus, the average particle diameter of the vistite particles is preferably in the range of 5-500 nm.
On the other hand, the average particle size of the magnetite or maghemite particles is not particularly limited, but is preferably 5-500 nm. When the average particle size of the magnetite or maghemite particles is less than 5 nm, Or when the average particle size of the magnetite or maghemite particles exceeds 500 nm, the size of the vistite particles is excessively large Which is undesirable.
On the other hand, as another effect of the present invention, the vistite particles according to the present invention exhibit luminescent characteristics after the phase change. Particularly, the vistite particles exhibit luminescence characteristics at a wavelength of 500 nm to 650 nm.
A method for producing vistitate particles according to another aspect of the present invention comprises the steps of
1) irradiating a laser to a magnetite or maghemite particle; And
2) phase change of the magnetite or maghemite into the single crystal form of vistite particles through the laser irradiation;
.
The method of producing vistite particles according to the present invention is characterized in that impurities are present in a mixture of impurities when producing vistitate particles in the prior art, and it is difficult to express specific characteristics of vistite as desired, And a manufacturing method which solves the problems of the prior art. That is, when the vistite particles are prepared by the production method according to the present invention, the purity is high, the characteristic specific to vistite can be expressed as desired, and it is possible to form the vistite particles into nano-sized fine particles. This effect is achieved by the above-described production method, specifically, by phase-changing the magnetite or maghemite particle into a single crystal form by laser irradiation with high energy or high output.
Meanwhile, although there is no particular limitation before carrying out the steps of the production method according to the present invention, it is preferable to perform the production method after providing a reducing atmosphere. Such a reducing atmosphere can be applied to the present invention without any particular limitation as long as it is a known method as a condition for forming the minimum atmosphere to be reduced.
On the other hand, although there is no particular limitation on the laser irradiation, it is preferable that the laser irradiation is performed in a high energy range, preferably at a wavelength of 500-1,000 nm.
Although there is no particular limitation on the laser irradiation, it is preferable that the laser irradiation is performed at a power of 60-300 mW as a high power range.
On the other hand, the average particle diameter of the vestite particles formed by the phase change by the above-mentioned production method is not particularly limited, but is preferably 5-500 nm.
The average particle diameter of the magnetite or maghemite particles is not particularly limited, but is preferably 5-500 nm.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Example
< Example 1: Synthesis of magnetic nanoparticles >
Synthesis of magnetite (Fe 3 O 4 ) nanoparticles was carried out via the polyol method. In this reaction, iron chloride hexahydrate (FeCl 3 .6H 2 O) is a precursor. Ethylene glycol is a reducing agent and a solvent. Sodium acetate, distilled water (H 2 O) Were used as adjuvants to aid in hydrolysis. After the above chemical materials were mixed, the mixed solution was heated to a temperature of 200 ° C while maintaining the stirrings. After the reaction solution was cooled to room temperature, ethanol was added thereto, followed by washing with a centrifugal separator to obtain final magnetite magnetic nanoparticles. The thus-synthesized magnetic nanoparticles were collected on a thin organic substrate using a magnet, and then the particles were measured with an optical microscope. The results are shown in FIG. The size of the measurement area in FIG. 1 was 5.5 nm, and the average particle diameter of the collected magnetite magnetic nanoparticles was 100 nm. Then, to replace the solvent with Dulbecco's Phosphate-Buffered Saline (DPBS), the same procedure as that of the above centrifugal separation was performed. And it was natural drying. After completely drying, the organic particles were coated on the surface of the collected particles and dried again.
< Example 2: magnetite particles Vestite Particle Phase change >
The magnetite magnetic nanoparticles collected in Example 1 were irradiated with a multiphoton laser beam at a wavelength of 780 nm and a power of 150 mW. When the laser beam of high energy and high power was irradiated in this way, the magnetite magnetic nanoparticles were phase-changed into a vestite single crystal particle. FIG. 2 is a photograph showing the phase change partially induced in the central part of the captured particles after complete drying, and FIG. 3 is a photograph showing the phase change induced in the whole area.
FIG. 4 is a graph of the X-ray diffraction analysis after the phase change. FIG. 4 shows that the initial Fe 3 O 4 nanoparticles were changed to FeO by laser irradiation. 5 (a) to 5 (d) are photographs showing Fe 3 O 4 before the phase change and FIGS. 5 (e) to 5 (h) is a photograph showing FeO after the phase change. In particular, it can be seen from FIG. 5 that if a plurality of small peaks that were seen before the phase change were combined and had a crystal structure of a cluster type of spinel structure before the phase change, then after the phase change, the single crystal of cubic structure It was confirmed that the
Meanwhile, FIG. 6 is a photograph showing the result of synthesizing the magnetite nanoparticles before the phase change by size.
Comparative Example
The magnetite particles of the above-mentioned example were tried to be produced as vistite particles by applying the conventional hydrothermal synthesis method, but the metal oxide containing iron oxide impurities was regarded as the present comparative example.
Experimental Example
The optical characteristics of the vistite particles causing the phase change according to Example 2 and the comparative example of the magnetite particles were compared by fluorescence microscope. The measurement was performed by a fluorescence microscope after the laser irradiation, partial irradiation, and irradiation of the entire area. FIG. 2 and FIG. 3 show that a phase change occurs in a portion irradiated with a laser and a luminescence characteristic appears in a phase-changed nanoparticle. Thus, it can be seen that fine particles showing luminescence characteristics can be obtained through phase change.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. It is natural.
Claims (12)
The phase change is achieved through laser irradiation,
Wherein the laser beam is phase-changed into a single crystal form due to the laser irradiation.
Wherein the vistite particles exhibit a luminescence characteristic after the phase change.
Wherein the laser irradiation has a wavelength of 500-1,000 nm.
Wherein the laser irradiation has an output of 60-300 mW.
Wherein the vestite particles have an average particle diameter of 5-500 nm.
Wherein the magnetite or maghemite particles have an average particle diameter of 5-500 nm.
Wherein the vistite particles exhibit luminescence characteristics at a wavelength of 500 nm to 650 nm.
2) phase change of the magnetite or maghemite into the single crystal form of vistite particles through the laser irradiation;
≪ / RTI >
Wherein the laser irradiation is performed at a wavelength of 500-1,000 nm.
Wherein the laser irradiation is performed at an output of 60-300 mW.
Wherein the average particle size of the vestite particles produced by the method is in the range of 5 to 500 nm.
Wherein the average particle size of the magnetite or maghemite particles is 5-500 nm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100550194B1 (en) | 2002-04-17 | 2006-02-08 | 인터내셔널 비지네스 머신즈 코포레이션 | Synthesis of Magnetite Nanoparticles and the Process of Forming Fe-Based Nanomaterials |
| KR100604975B1 (en) | 2004-11-10 | 2006-07-28 | 학교법인연세대학교 | Preparation Method of Magnetic and Metal Oxide Nanoparticles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100550194B1 (en) | 2002-04-17 | 2006-02-08 | 인터내셔널 비지네스 머신즈 코포레이션 | Synthesis of Magnetite Nanoparticles and the Process of Forming Fe-Based Nanomaterials |
| KR100604975B1 (en) | 2004-11-10 | 2006-07-28 | 학교법인연세대학교 | Preparation Method of Magnetic and Metal Oxide Nanoparticles |
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