KR101350400B1 - The magnetic metal oxide nano particles, the magnetic intermetallic compound nano particles and methods of making them - Google Patents

Abstract

Metal oxide nano magnetic particles and intermetallic compound nano magnetic particles manufacturing method using ultrasonic irradiation according to the present invention using non-toxic metal salt as a raw material environmentally friendly nano magnetic particles capable of controlling the particle size of several hundred nanometers uniform size It can be manufactured in large quantities and can be applied in industries such as materials, medicine, electronics, optics and energy.
In addition, by manufacturing the nanoparticles by ultrasonic irradiation, compared with the case of preparing nanoparticles using a conventional surfactant, it is possible to prevent the phenomenon that the yield is lowered to produce nanoparticles in a yield close to about 100%.

Description

The magnetic metal oxide nano particles, the magnetic intermetallic compound nano particles and methods of making them}

The present invention relates to a metal oxide nano magnetic particles and intermetallic compound nano magnetic particles and a method for producing the same using ultrasonic irradiation.

In general, the method for producing nanoparticles can be largely divided into a solid phase method, a gas phase method and a liquid phase method.

The solid phase method has limitations in producing nanoparticles having a diameter of 100 nm or less. Therefore, the gas phase method and the liquid phase method are usefully used to produce functional nanoparticles having small particle diameters.

The gas phase method is classified into physical vapor deposition method (PVD) and chemical vapor deposition method (CVD) by cooling the high temperature steam, and the typical manufacturing methods include the gas evaporation method and the mixed gas method. . When the nanoparticles are prepared by using a gas phase method, there is an advantage in that the nanoparticles can be manufactured with less impurities, high purity, and small particle size. In particular, nickel nanoparticles for ceramic capacitor electrode materials used in mobile phones and the like have high purity manufactured by chemical vapor deposition. However, when manufacturing nanoparticles using a multi-component material, since the selection of raw materials is very difficult, it is difficult to manufacture nanoparticles whose composition is controlled.

On the other hand, in the liquid phase method of manufacturing nanoparticles in a solution, since the multi-component material can be prepared in a solution, there is an advantage that raw material mixing at the molecular level is possible. Unlike the gas phase method using a plasma or gas evaporation method, the liquid phase method does not require expensive equipment, is relatively simple in apparatus, and is easily used because it is possible to manufacture high-crystalline nanoparticles without aggregation in one step.

Typical preparation methods of the liquid phase method include coprecipitation method, alkoxide (sol-gel) method, reverse micelle method, spray pyrolysis method (droplet-particle conversion processor) and the like.

The method of preparing nanoparticles by the liquid phase method has been a method of producing metal nanoparticles in hydrogel form using a reducing agent or a surfactant after dissociating a metal compound in water. However, the above method has a disadvantage in that the yield is very low due to the concentration of the metal compound solution. Specifically, metal nanoparticles having a uniform particle size at a concentration of the metal compound of 0.05 M or less can be prepared. In addition, syntheses of cobalt (Ref. 1), iron (Ref. 2) and nickel (Ref. 3) by reverse micelle, sonochemical decomposition of metal carbonyl have been reported, but all of the above methods are multimolecular. It produces particles and is not suitable for mass synthesis because of their poor reproducibility at high concentrations.

In addition, the method for preparing the transition metal nanoparticles from the reaction of the metal precursor at a high temperature is not suitable for mass production because the size fractionation of the particles is essential to control the desired properties (Ref. 4).

In addition, methods of preparing metal nanoparticles through direct oxidation using pyrolysis in a solvent using CO ₂ (CO) ₈ and Fe (CO) ₅ together with a surfactant have been reported (Ref. 5). . However, these raw materials are very expensive and toxic and are not suitable for synthesis in large quantities.

Currently, the synthesis and basic research of ultra-fine metal nanoparticles of less than 100 nm are actively conducted in Korea and abroad, but research on nanoparticles of more than 100 nm and less than 1000 nm is limited. In the United States, titanium is produced by Micron Metal and Atlantic Equipment Engineers, zinc by Big River Zinc, iron by Atlantic Equipment Engineers, and cobalt by OMG. Doing. In Japan, Kawatetsu Mining has commercialized and produced 200 nm nickel powder production technology from nickel chloride by vapor phase chemical reaction. In Korea, few companies produce nano metal powders of 100 nm or more and 1000 nm or less.Titanium is manufactured by Changsung and dry grinding, which produce cobalt from metal powders with particle size of 1000 nm or more by liquid phase method. There are only a few in addition to Sejong Materials.

As a conventional technique, the Republic of Korea Patent Publication No. 10-2005-0079151 provides a method for mass production of nanocrystalline metal oxide powder using the ultrasonic spray combustion method. Specifically, (1) mixing the metal salt solution and the fuel (first step), (2) ultrasonic spraying the solution mixed in the first step together with a carrier gas (second step), (3) reacting the sprayed solution in a high temperature reaction zone for a period of time (third step), and (4) collecting the powder produced as a result of the reaction in the reaction zone (fourth step).

When the nanocrystalline metal oxide is prepared by the above method, there is an advantage that the nanocrystalline metal oxide can be manufactured in a large amount, but the nanocrystalline metal oxide having a particle size of 20 to 30 nm is prepared, thereby preparing in the present invention. There is a difference that particles of 100 nm or more and 1000 nm or less are not produced.

In addition, the Republic of Korea Patent Publication 10-2006-0043925 provides a method for producing magnetic or metal oxide nanoparticles. Specifically, (1) adding a magnetic or metal precursor to a surfactant or a solvent containing a surfactant to prepare a mixed solution, (2) heating the mixed solution to 50 ~ 600 ℃ to pyrolyze the precursor To form magnetic or metal oxide nanoparticles, and (3) separating the nanoparticles.

When the magnetic or metal oxide nanoparticles are manufactured by the above method, the magnetic or metal oxide nanoparticles may be prepared in large quantities, but the yield is very low due to the concentration of the mixed solution.

Accordingly, the present inventors have been researching a method for producing nanoparticles of 100 nm or more and 1000 nm or less while solving the conventional problems, and when the nanoparticles are manufactured using ultrasonic waves, the particle size is 100 nm or more and 1000 nm. It was found that the following nanoparticles can be produced uniformly in large quantities, and completed the present invention.

Reference 1 C. Petit et al., J. Phys. Chem. B. 1999, 103, 1805

Reference 2 J. P. Wilcoson et al., J. Phys. Chem. B. 1999, 103, 9809

Reference 3 D. H. Chen, 2002, J. Mater. Chem. 12, 2412

Reference 4 Murray et al., US patent 6,262,129

Reference 5 VF Puntes et al., Science 2001, 291, 2115, T. Hyoen et al., J. Am. Chem. Soc., 2001, 123, 12798

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for preparing metal oxide nanomagnetic particles and intermetallic compound nanomagnetic particles using ultrasonic irradiation.

It is another object of the present invention to provide a metal oxide nanomagnetic particles and intermetallic compound nanomagnetic particles prepared according to the above method.

According to an aspect of the present invention,

Preparing a metal precursor solution by dissolving a metal salt containing one metal in an organic solvent (step 1);

Preparing nanoparticles by irradiating ultrasonic waves to the metal precursor solution of step 1 (step 2);

Precipitating nanoparticles by adding ethanol to the metal precursor solution of step 2 (step 3); And

Drying and heat-treating the nanoparticles of step 3 (step 4);

It provides a method for producing a metal oxide nanomagnetic particles comprising a.

Further, according to the present invention,

Preparing a metal precursor solution by dissolving a metal salt including two or more metals in an organic solvent (step 1);

Preparing nanoparticles by irradiating ultrasonic waves to the metal precursor solution of step 1 (step 2);

Precipitating nanoparticles by adding ethanol to the metal precursor solution of step 2 (step 3); And

Drying and heat-treating the nanoparticles of step 3 (step 4);

It provides a method for producing an intermetallic compound nano-magnetic particles comprising a.

Furthermore, the present invention provides a metal oxide nanomagnetic particles produced according to the above production method.

Furthermore, the present invention provides an intermetallic compound nanomagnetic particles prepared according to the above production method.

Metal oxide nano magnetic particles and intermetallic compound nano magnetic particles manufacturing method using ultrasonic irradiation according to the present invention using non-toxic metal salt as a raw material environmentally friendly nano magnetic particles capable of controlling the particle size of several hundred nanometers uniform size It can be manufactured in large quantities and can be applied in industries such as materials, medicine, electronics, optics and energy.

In addition, by manufacturing the nanoparticles by ultrasonic irradiation, compared with the case of preparing nanoparticles using a conventional surfactant, it is possible to prevent the phenomenon that the yield is lowered to produce nanoparticles in a yield close to about 100%.

1 is a photograph taken with a scanning electron microscope (left) and transmission electron microscope (right) of the iron oxide (Fe ₂ O ₃ ) nanoparticles prepared in Example 1.
FIG. 2 is a photograph of hematite (α-Fe ₂ O ₃ ) nanomagnetic particles prepared according to Example 2 using a scanning electron microscope (left) and a transmission electron microscope (right).
FIG. 3 is a photograph of the maghemite (γ-Fe ₂ O ₃ ) nanomagnetic particles prepared according to Example 3 using a scanning electron microscope (left) and a transmission electron microscope (right).
4 is a photograph of the magnetite (γ-Fe ₃ O ₄ ) nanomagnetic particles prepared according to Example 4 with a scanning electron microscope (left) and a transmission electron microscope (right).
FIG. 5 shows hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ), and magnetite (γ-Fe ₃ O ₄ ) nanomagnetic particles prepared according to Examples 2, 3, and ₄ X-ray diffraction analysis graph.
FIG. 6 shows hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ), and magnetite (γ-Fe ₃ O ₄ ) nanomagnetic particles prepared according to Examples 2, 3, and ₄ The magnetic hysteresis curve of.
7 is a photograph taken with a scanning electron microscope of hematite (α-Fe ₂ O ₃ ) nanomagnetic particles prepared in 300 nm, 500 nm, 700 nm and 1000 nm size by Example 5.
8 is a photograph taken with a scanning electron microscope (left) and a transmission electron microscope (right) of the iron cobalt (FeCo) nanomagnetic particles prepared in Example 6.
9 is an X-ray diffraction graph of the iron cobalt (FeCo) nanomagnetic particles prepared in Example 6.
10 is a photograph taken with a scanning electron microscope (left) and a transmission electron microscope (right) of the iron platinum (FePt) nanomagnetic particles prepared in Example 7.
11 is an X-ray diffraction graph of the iron platinum (FePt) nanomagnetic particles prepared by Example 7.
12 is a photograph taken with a scanning electron microscope (left) of hematite (α-Fe ₂ O ₃ ) nano-magnetic particles prepared in large quantities according to Example 8 and hematite (α-Fe ₂ O ₃ ) nano-magnetic particles It is the photograph which weighed on the scale after making 20 g and drying.

The present invention provides a method for producing metal oxide nanomagnetic particles using ultrasonic irradiation.

Hereinafter, the present invention will be described in detail.

The present invention comprises the steps of dissolving a metal salt containing one metal in an organic solvent to prepare a metal precursor solution (step 1);

Preparing nanoparticles by irradiating ultrasonic waves to the metal precursor solution of step 1 (step 2);

Precipitating nanoparticles by adding ethanol to the metal precursor solution of step 2 (step 3); And

Drying and heat-treating the nanoparticles of step 3 (step 4);

It provides a method for producing a metal oxide nanomagnetic particles comprising a.

Hereinafter, a method of manufacturing the metal oxide nanomagnetic particles according to the present invention will be described in more detail step by step.

First, in the present invention, step 1 is a step of preparing a metal precursor solution, to prepare a metal precursor solution by dissolving a metal salt containing one metal in an organic solvent.

At this time, it is preferable to use a metal salt of step 1 which is inexpensive and non-toxic. By using the non-toxic as the metal salt there is an advantage that can be synthesized in large quantities.

Specifically, the metal is preferably selected from Group IIA metals, Group IIIA metals, Group IVA metals, transition metals, and lanthanide metals, specifically magnesium, calcium, strontium, barium, titanium, vanadium, chromium, manganese, iron, and cobalt. Nickel, Copper, Zinc, Gallium, Germanium, Yttrium, Zirconium, Molybdenum, Ruthenium, Silver, Cadmium, Indium, Tin, Platinum, Gold, Lead, Lanthanum, Cerium, Proseodymium, Nedium, Samarium, Euro It is more preferable to use pium, gadolium, terbium, dysprosium, ytterbium, ruthenium and the like.

In addition, the salt of the metal salt of step 1 is nitrate, carbonate, chloride, phosphate, borate, oxide, sulfonate, sulfate, stearic acid salt, myristinate, acetate, acetylacetonate, hydrates thereof and mixtures thereof It is preferable to use.

The solvent used in the preparation of the metal precursor solution in step 1 may be selected from the group comprising ether, hydrocarbon, and alcohol as an organic solvent. Preferably, butyl ether, hexyl ether, octyl ether, decyl ether, benzyl ether, phenyl ether and the like can be used as the ether organic solvent, and hexane, benzene, tetradecine, hexadecine, octadecine, toluene, xylene as the hydrocarbon-based solvent. And chlorobenzoic acid, and the like, and may be used as alcohols. Hexatecanol, 1,2-hexadecanediol, octyl alcohol, 1,2-octanediol, decanol, 1,2-dodecanediol and ethylene glycol Etc. can be used.

Next, step 2 is a step of preparing nanoparticles by irradiating ultrasonic waves to the metal precursor solution prepared in step 1.

In the step 2, the ultrasonic wave may be irradiated for 1 to 12 hours at an intensity of 2 to 200 kHz, preferably from 5 minutes to 1 hour at an intensity of 20 kHz, and more preferably, the ultrasonic irradiation time is 10 minutes to 30 minutes. Investigate to minutes. If the ultrasonic wave is irradiated at an intensity of less than 2 kHz, there is a problem that the nano-particles are not produced because the ultrasonic irradiation is not made sufficiently, and when irradiated at an intensity of more than 200 kHz, the nanoparticles aggregate to form an aggregate This can happen.

When the nanoparticles are manufactured by ultrasonic irradiation in the step 2, compared with the case of preparing nanoparticles using a conventional surfactant, the yield is reduced to prevent the phenomenon that the nanoparticles in a yield close to about 100% It can manufacture.

Next, step 3 is to add ethanol to the metal precursor solution to precipitate the nanoparticles.

When the excess ethanol is added to the metal precursor solution to precipitate the nanoparticles formed in the metal precursor solution of step 2, the metal oxide nanoparticles are precipitated. The metal oxide nanoparticles precipitated in the metal precursor solution may be separated by centrifugation, and centrifugation may be performed three or more times to recover the nanoparticles.

Next, the step 4 is a step of drying and heat-treating the nanoparticles separated in the step 3, the nanoparticles are given a magnetization while undergoing a heat treatment step.

The drying of step 4 is preferably performed for 3 to 12 hours at a temperature of 50 to 80 ℃.

In addition, the heat treatment of step 4 is preferably performed for 3 to 12 hours at a temperature of 200 to 1200 ℃, more preferably may be performed for 3 to 12 hours at a temperature of 250 to 1000 ℃. If the heat treatment is performed at a temperature of less than 200 ℃ in step 4, there may be a problem that the magnetism is not sufficiently given to the nanoparticles, and if the heat treatment is performed at a temperature exceeding 1200 ℃ by the high temperature of the nanoparticles Problems may occur in the production of monodisperse nanoparticles by changing the physical properties and forming an aggregate.

In addition, the heat treatment of step 4 may be prepared by forming an atmosphere using nitrogen, argon, oxygen, and hydrogen gas according to the nanoparticles to be prepared, thereby producing the desired nanoparticles.

Nanomagnetic particles produced according to the above production method has a size of 100 nm to 1000 nm. This can be applied in industrial fields such as materials, medicine, electronics, optics, energy, etc. by broadening the scope of research and commercialization for the production of 100 nm to 1000 nm nanoparticles, which have been conventionally limited.

In another aspect, the present invention comprises the steps of dissolving a metal salt containing two or more metals in an organic solvent to prepare a metal precursor solution (step 1);

Preparing nanoparticles by irradiating ultrasonic waves to the metal precursor solution of step 1 (step 2);

Precipitating nanoparticles by adding ethanol to the metal precursor solution of step 2 (step 3); And

Drying and heat-treating the nanoparticles of step 3 (step 4);

It provides a method for producing an intermetallic compound nano-magnetic particles comprising a.

In the present invention, step 1 is a step of preparing a metal precursor solution, to dissolve a metal salt containing two or more metals in an organic solvent to prepare a metal precursor solution. At this time, two or more kinds of metals of step 1 may be used by mixing two or more kinds as the same metals mentioned in the method for preparing the metal oxide nanomagnetic particles.

Hereinafter, the manufacturing method of the intermetallic compound nanomagnetic particles is omitted because it is the same as the manufacturing method of the metal oxide nanomagnetic particles.

Furthermore, the present invention provides a metal oxide nanomagnetic particles prepared according to the above production method.

Furthermore, the present invention provides an intermetallic compound nanomagnetic particles prepared according to the above production method.

The metal oxide nanomagnetic particles and the intermetallic compound nanomagnetic particles prepared according to the present invention can obtain a large amount of nanomagnetic particles capable of controlling particle sizes of several hundred nanometers by using nontoxic metal salts as raw materials. It is available in industries such as materials, medicine, electronics, optics and energy. In addition, by manufacturing the nanoparticles by the ultrasonic irradiation, compared with the case of preparing nanoparticles using a conventional surfactant, the yield can be prevented from lowering the phenomenon can be produced nanoparticles in a yield close to about 100%. .

Hereinafter, the present invention will be described in detail by way of examples. However, the following examples are illustrative of the present invention, and the present invention is not limited by the following examples.

Example 1 Preparation of 300 nm Iron Oxide (Fe ₂ O ₃ ) Nanoparticles

0.5 mmol of iron acetylacetonate hydrate was added to a Erlenmeyer flask containing 10 mL of octyl ether to prepare a metal precursor solution while stirring, and then ultrasonic waves of 20 kHz (50%) intensity were irradiated for 10 minutes using an ultrasonic irradiator.

As the ultrasonic wave was examined, it was observed that the solution, which was initially orange, turned blackish brown over time, indicating that the iron oxide nanoparticles were successfully synthesized. Excess ethanol was added to the mixed solution in which the iron oxide nanoparticles were prepared to allow the produced nanoparticles to precipitate, followed by centrifugation to separate the nanoparticles and the supernatant, thereby removing the supernatant. The washing process was repeated at least three times, and the precipitate was dried at 80 ° C. for 12 hours to obtain iron oxide nanoparticles having a size of 300 nm.

Example 2 Preparation of 300 nm Hematite (α-Fe ₂ O ₃ ) Nanomagnetic Particles

The nanoparticles prepared and dried in Example 1 were heat-treated at 300 ° C. for 3 hours in an argon atmosphere to obtain hematite (α-Fe ₂ O ₃ ) nanomagnetic particles.

Example 3 Preparation of 300 nm Maghite (γ-Fe ₂ O ₃ ) Nano Magnetic Particles

The nanoparticles prepared and dried in Example 1 were heat-treated at 500 ° C. for 3 hours in an argon atmosphere to obtain maghemite (γ-Fe ₂ O ₃ ) nanomagnetic particles.

Example 4 Preparation of 300 nm Magnetite (γ-Fe ₃ O ₄ ) Nano Magnetic Particles

The nanoparticles prepared and dried in Example 1 were heat-treated at 700 ° C. for 3 hours in an argon atmosphere to obtain magnetite (γ-Fe ₃ O ₄ ) nanomagnetic particles.

Example 5 Preparation of 300 nm, 500 nm, 700 nm and 1000 nm Magnetite (γ-Fe ₃ O ₄ ) Nano Magnetic Particles

By varying the mixing ratio of the metal salt and the organic solvent and the ultrasonic irradiation time, magnetite (γ-Fe ₃ O ₄ ) nanomagnetic particles having different sizes of 300 nm, 500 nm, 700 nm and 1000 nm were prepared in four flasks, respectively.

Magnite (γ-Fe ₂ O ₃ ) having a size of 300 nm was prepared according to Example 1, but was irradiated with ultrasonic waves for 10 minutes, and magnetite (γ-Fe ₂ O ₃ ) having a size of 500 nm was used for Example 1 It was prepared according to the ultrasonic irradiation for 30 minutes. In addition, the 700 nm size maghemite (γ-Fe ₂ O ₃ ) was prepared according to Example 1, but the solvent used was mixed with octyl ether and benzyl ether in a ratio of 7 to 3, the ultrasonic wave 10 minutes Investigate. Finally, 1000 nm size maghemite (γ-Fe ₂ O ₃ ) was prepared according to Example 1, but the solvent used was mixed with octyl ether and benzyl ether in a ratio of 5 to 5, and ultrasonic waves were 10 minutes. Investigate.

In the four flasks, all of the initially orange solution turned to blackish brown color upon irradiation with ultrasound, indicating that the iron oxide nanoparticles were successfully synthesized.

Thereafter, an excess of ethanol was added to the four flasks in which the nanoparticles were produced to allow the nanoparticles to precipitate. The centrifugation was repeated three or more times to separate the precipitate and the supernatant, and the residue was then heated at 80 ° C. for 12 hours. Dried. The dried nanoparticles were heat-treated at 500 ° C. for 3 hours in an argon atmosphere to complete the preparation of maghemite (γ-Fe ₂ O ₃ ) having sizes of 300 nm, 500 nm, 700 nm and 1000 nm.

Example 6 Preparation of 500 nm Iron Cobalt (FeCo) Nanomagnetic Particles

0.6 mmol of iron acetylacetonate hydrate and 0.4 mmol of cobalt acetylacetonate hydrate were added to an Erlenmeyer flask containing 10 mL of octyl ether to prepare a metal precursor solution while stirring, followed by 20 kHz (50%) intensity for 30 minutes using an ultrasonic irradiator. Ultrasound was irradiated.

Upon irradiation of the ultrasound, it was observed that the solution, which was initially orange, turned black over time, indicating that iron cobalt (FeCo) nanoparticles were successfully prepared. Excess ethanol was added to the mixed solution in which the iron cobalt nanoparticles were prepared to allow the nanoparticles to precipitate, followed by centrifugation to separate the nanoparticles and the supernatant, and the supernatant was removed. The washing process was repeated at least three times, and the precipitate was dried at 80 ° C. for 12 hours. Thereafter, the dried nanoparticles were heat-treated at 500 ° C. for 3 hours in an argon atmosphere to complete preparation of iron cobalt (FeCo) nanomagnetic particles having a size of 500 nm.

Example 7 Preparation of 500 nm Iron Platinum (FePt) Nano Magnetic Particles

Iron platinum (FePt) nanomagnetic particles were prepared in the same manner as in Example 6, except that 0.5 mmol of iron acetylacetonate hydrate and 0.5 mmol of platinum acetylacetonate were dissolved in 10 mL of octyl ether.

Example 8 Mass Production of 300 nm Hematite (α-Fe ₂ O ₃ ) Nanomagnetic Particles

A 300 nm hematite (α-Fe ₂ O ₃ ) nanomagnetic particles were prepared in the same manner as in Example 2 except that 100 mmol of iron acetylacetonate hydrate was dissolved in 80 mL of octyl ether as a metal salt.

Experimental Example 1 Shape Analysis of the Metal Oxide Nanomagnetic Particles Prepared in Examples 2, 3, and 4

Hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ) and magnetite (γ-Fe ₃ O ₄ ) nano-manufactured differently according to the heat treatment time set in Examples 2, 3 and 4 Magnetic particles were analyzed by scanning electron microscopy and transmission electron microscopy.

First, Figure 2 is a photograph of the hematite (α-Fe ₂ O ₃ ) nanomagnetic particles prepared in Example 2 with a scanning electron microscope (left) and a transmission electron microscope (right), Figure 3 is an embodiment Maghite (γ-Fe ₂ O ₃ ) nanomagnetic particles prepared by 3 is a photograph taken with a scanning electron microscope (left) and a transmission electron microscope (right), Figure 4 is a magnetite prepared by Example 4 (γ-Fe ₃ O ₄ ) Nanomagnetic particles were taken with a scanning electron microscope (left) and a transmission electron microscope (right). As can be seen from the photographs of FIGS. 2 to 4, spherical hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ), and magnetite (γ-Fe ₃ O ₄ ) having a size of 300 nm ) It was confirmed that the nanomagnetic particles were prepared in a uniform size, respectively.

When manufacturing the magnetic nanoparticles using the present invention from the photo of Figures 2 to 4, it was proved that the manufacturing process is simplified because the size of the nanoparticles is not required, unlike the prior art.

Experimental Example 2 Magnetic Analysis of Metal Oxide Nanomagnetic Particles Prepared in Examples 2, 3, and 4

Hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ) by performing the magnetic hysteresis curve experiment and X-ray diffraction analysis of the nano-magnetic particles prepared in Examples 2, 3, 4 And magnetite (γ-Fe ₃ O ₄ ) was confirmed. FIG. 5 shows hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ), and magnetite (γ-Fe ₃ O ₄ ) nanomagnetic particles prepared according to Examples 2, 3, and ₄ X-ray diffraction analysis graph. From the graph of FIG. 5, hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ), and magnetite (γ-Fe ₃ ) were changed by heat treatment from iron oxide (Fe ₂ O ₃ ) nanoparticles. It was confirmed that O ₄ ) was prepared as originally intended.

6 is hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ), and magnetite (γ-Fe ₃ O ₄ ) nanomagnetics prepared in Examples 2, 3, and ₄ Shows the hysteresis curve of the particle. It can be seen that the nanomagnetic particles of Examples 2, 3, and 4 show a change in magnetic strength according to the external magnetic field applied to FIG. 6, and the magnetic properties are also enhanced as the heat treatment temperature is increased. Could know.

Therefore, the nanomagnetic particles prepared in Examples 2, 3, and 4 through FIGS. 5 and 6 are hematite (α-Fe ₂ O ₃ ), maghemite (γ-Fe ₂ O ₃ ), and magnetite (γ-Fe). ₃ O ₄ ), it was confirmed that the materials are magnetic and specifically, the higher the heat treatment temperature, the larger the magnetism.

Experimental Example 3 Shape Analysis of Hematite (α-Fe ₂ O ₃ ) Nanomagnetic Particles Prepared in Various Sizes

In Example 5, the magnetite (α-Fe ₃ O ₄ ) nano magnetic particles prepared in 300 nm, 500 nm, 700 nm and 1000 nm sizes were analyzed by scanning electron microscope.

FIG. 7 is a photograph of hematite (α-Fe ₂ O ₃ ) nanomagnetic particles prepared in various sizes according to Example 5 with a scanning electron microscope. From the photograph of FIG. 7, it was confirmed that hematite (α-Fe ₂ O ₃ ) nanomagnetic particles having a desired size can be prepared by changing the ultrasonic irradiation time and the type of organic solvent.

Therefore, it can be seen from FIG. 7 that the size of the nanomagnetic particles can be adjusted according to the irradiation time of the ultrasound, the type and amount of the solvent.

Experimental Example 4 Shape Analysis of Intermetallic Compound Nanomagnetic Particles Prepared in Examples 6 and 7

X-ray diffraction analysis, scanning electron microscopy and transmission electron microscopy of iron cobalt (FeCo) nanomagnetic particles and iron platinum (FePt) nanomagnetic particles prepared using metal salts including two or more metals in Examples 6 and 7 As shown in FIGS. 8, 9, 10, and 11.

8 is a photograph taken with a scanning electron microscope (left) and a transmission electron microscope (right) of the iron cobalt (FeCo) nanomagnetic particles prepared according to Example 6, Figure 9 is iron cobalt prepared by Example 6 X-ray diffraction analysis graph of (FeCo) nanomagnetic particles. As shown in FIG. 8, it was confirmed that the iron cobalt (FeCo) nanomagnetic particles were prepared through the X-ray diffraction pattern, and as shown in FIG. 9, the sizes of the iron cobalt (FeCo) nanomagnetic particles also had a uniform distribution. I could confirm that.

10 is a photograph taken with a scanning electron microscope (left) and a transmission electron microscope (right) of the iron platinum (FePt) nanomagnetic particles prepared in Example 7, Figure 11 is an iron prepared by Example 7 X-ray diffraction graph of platinum (FePt) nanomagnetic particles. 10 and 11 it was confirmed that the iron platinum (FePt) nanomagnetic particles having a particle size of 500 nm was also produced in a uniform size.

Experimental Example 5 Analysis of 300 nm Hematite (α-Fe ₂ O ₃ ) Nanomagnetic Particles Prepared in Mass Production

The shape and yield of the 300 nm hematite (α-Fe ₂ O ₃ ) nanomagnetic particles prepared in large quantities according to Example 8 were analyzed, and the possibility of mass production was shown in FIG. 12. 12 is a photograph taken with a scanning electron microscope (left) of hematite (α-Fe ₂ O ₃ ) nanomagnetic particles prepared in large quantities according to Example 8 and hematite (α-Fe ₂ O ₃ ) nanomagnetic particles It is the photograph which weighed on the scale after making 20 g and drying.

To the results based on the raw material iron acetylacetonate hydrate and octyl ether in bulk hematite (α-Fe ₂ O ₃₎ in the case of producing a nano-magnetic particles, hematite produced in lab scale tight (α-Fe ₂ O ₃ ) It was confirmed that uniform nanoparticles were prepared in the same manner as nanomagnetic particles. In addition, the yield of the hematite (a-Fe ₂ O ₃ ) nanomagnetic particles was 95%, yielding a yield close to about 100% it was confirmed that the loss of the raw material also hardly occurred.

Claims (10)

Preparing a metal precursor solution by dissolving a metal salt containing one metal in an organic solvent (step 1);
Preparing nanoparticles by irradiating ultrasonic waves to the metal precursor solution of step 1 (step 2);
Precipitating nanoparticles by adding ethanol to the metal precursor solution of step 2 (step 3); And
Drying and heat-treating the nanoparticles of step 3 (step 4);
Method for producing a metal oxide nanomagnetic particles comprising a.
Preparing a metal precursor solution by dissolving a metal salt including two or more metals in an organic solvent (step 1);
Preparing nanoparticles by irradiating ultrasonic waves to the metal precursor solution of step 1 (step 2);
Precipitating nanoparticles by adding ethanol to the metal precursor solution of step 2 (step 3); And
Drying and heat-treating the nanoparticles of step 3 (step 4);
Method for producing an intermetallic compound nano-magnetic particles comprising a.
The method of claim 1 or claim 2, wherein the metal of step 1 is a nano-magnetic particles, characterized in that selected from the group consisting of Group IIA metal, Group IIIA metal, Group IVA metal, transition metal and lanthanide metal Way.
The method of claim 1 or 2, wherein the salt of the metal salt of step 1 is nitrate, carbonate, chloride, phosphate, borate, oxide, sulfonate, sulfate, stearic acid salt, myristinate, acetate, acetylacetonate, Method for producing a nano-magnetic particles, characterized in that selected from the group comprising these hydrates and mixtures thereof.
The method of claim 1, wherein the organic solvent of step 1 is selected from the group comprising ether, hydrocarbon, and alcohol.
The method of claim 1 or 2, wherein the ultrasonic wave of step 2 is irradiated for 1 to 12 hours at an intensity of 2 to 200 kHz.
The method of claim 1, wherein the heat treatment of Step 4 is performed for 3 to 12 hours at a temperature of 200 to 1200 ° C. 4.
The method of claim 1 or 2, wherein the nanoparticles have a size of 100 nm to 1000 nm.
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