KR101480169B1 - The Method for Preparation of Monodisperse Iron Oxide Nanoparticles Using High Pressure Homogenizer and Monodisperse Iron Oxide Nanoparticels Thereof - Google Patents
The Method for Preparation of Monodisperse Iron Oxide Nanoparticles Using High Pressure Homogenizer and Monodisperse Iron Oxide Nanoparticels Thereof Download PDFInfo
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- KR101480169B1 KR101480169B1 KR1020140065847A KR20140065847A KR101480169B1 KR 101480169 B1 KR101480169 B1 KR 101480169B1 KR 1020140065847 A KR1020140065847 A KR 1020140065847A KR 20140065847 A KR20140065847 A KR 20140065847A KR 101480169 B1 KR101480169 B1 KR 101480169B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
Abstract
Description
The present invention relates to a method for producing monodispersed iron oxide nanoparticles using an ultra-high pressure homogenizer and monodisperse iron oxide nanoparticles produced thereby. More particularly, the present invention relates to a method for producing monodisperse iron oxide nanoparticles having a particle size of 10 to 30 nm using an ultra-high pressure homogenizer and monodisperse iron oxide nanoparticles produced thereby. , Magnetic optical elements, magnetic ink, heavy metal wastewater treatment, MRI contrast agent, drug delivery system, and thermal therapy.
As the particles decrease in nanometer size, they exhibit new electrical, optical, or magnetic properties that did not appear at bulk size. In nanoparticles, unlike lumps, the ratio of the surface is large. Since the surface ratio depends on the size of the particles, the size of the nanoparticles is the most important factor in determining the physical and chemical properties.
In the case of iron oxide nanoparticles, when the particle size is below a certain critical size, a single magnetic domain is formed. In this case, the iron oxide particles are superparamagnetized and the kinetic energy And dispersed in an appropriate solvent to give a stable colloidal state. However, conventional methods for preparing nanoparticles such as sol-gel method, coprecipitation method, pyrolysis of an organic metal precursor, high-temperature oxidation and reduction of metal ions, and precipitation, oxidation and reduction in reverse micelle are not easy to control the size of iron oxide nanoparticles , The particle size distribution is too wide from several nanometers to several hundred nanometers, and the study of magnetic properties and structures according to the size of iron oxide has not been accurate until recently.
In addition, pyrolysis of the organometallic precursor, high temperature oxidation and reduction of the metal ions, etc., require a more efficient and uniform synthesis method of iron oxide nanoparticles because the reaction takes place at a high temperature and the process is complicated.
First, J. AM. Chem. Soc. 2001, 123, 12798 discloses a method for the synthesis of uniform magnetic iron oxide nanoparticles from pyrolysis of iron-oleic acid complexes made from the reaction of pentacarbonyl iron with oleic acid without size selection. However, there is a problem that the production temperature is high and the production time is long, for example, the production temperature of iron oxide is 100 ° C or more and the reaction takes two hours in total for 3 hours or more. Also, since Fe (CO) 5 used as a raw material for producing iron oxide is very toxic, expensive, and difficult to store, the method is not suitable for manufacturing iron oxide nanoparticles.
Secondly, Korean Patent Laid-Open Publication No. 10-2006-0012346 (Mar. 2, 2006) discloses a method for synthesizing nano-sized magnetic particles of uniform size from pyrolysis of a ferroallate complex formed from the reaction of ferric chloride and sodium oleate Lt; / RTI > However, there is a problem that the production temperature is high and the process is complicated, for example, the iron oxide production temperature is 300 ° C or higher and the pressure is reduced to 0.3 Torr.
Third, in Journal of Alloys and Compouns, 2009, 475, and 898, the method of synthesizing magnetite nanoparticles from hydrothermal synthesis by adding hydrogen peroxide as an oxidizing agent to ferrous hydroxide (Fe (OH) 2 ) produced by adding ammonia water to a ferrous sulfate solution . However, since a ferric hydroxide solution is prepared by adding a polyethylene glycol polymer as a dispersant and hydrogen peroxide is added as an oxidizing agent, a hydrothermal synthesis process is carried out at 160 ° C. for 5 to 8 hours, and a long manufacturing time is required. It was not effective in production.
Accordingly, the present inventors have conducted studies to solve problems such as complicated processes at high temperatures, long production time, wide particle size distribution of particles, toxic surfactants and oxidizing agents, which are disadvantages of conventional iron oxide nanoparticle production methods, The present invention has been accomplished based on the synthesis of monodisperse iron oxide nanoparticles which can economically produce iron oxide nanoparticles having excellent crystallinity and uniform size by a simple process at room temperature by a synthesis method using a homogenizer.
The object of the present invention is to solve the above-mentioned problems, and it is an object of the present invention to provide a method for producing a ferrofluidic iron oxide nanoparticle by passing a ferrohydroxide solution through an ultra-high pressure homogenizer, To provide a method for producing monodispersed iron oxide nanoparticles and monodisperse iron oxide nanoparticles produced thereby.
Another object of the present invention is to provide a method for producing monodispersed iron oxide nanoparticles using an ultra-high pressure homogenizer capable of economically manufacturing iron oxide nanoparticles having excellent crystallinity and uniform size and to provide monodispersed iron oxide nanoparticles prepared thereby .
Another object of the present invention is to provide a method for preparing monodispersed iron oxide nanoparticles using a radical reaction of an ultra-high pressure homogenizer without adding any additional oxidizing agent, surfactant and radical scavenger, and to provide monodisperse iron oxide nanoparticles prepared thereby.
The present invention relates to a process for producing monodisperse iron oxide nanoparticles and monodisperse iron oxide nanoparticles produced thereby.
In the present invention, FIG. 1 can be referred to as an example of the ultra-high pressure homogenizer.
The ultra-high pressure homogenizer of FIG. 1 may be composed of a sample inlet, a pressure pump for applying pressure to the fluid, a fine orifice nozzle chamber, a heat exchanger and an outlet.
The pressure pump may apply pressure to the fluid to move the fluid to the fine orifice nozzle chamber.
Figure 2 illustrates a portion of the interior of the fine orifice nozzle chamber. In the present invention, when water is passed through the chamber, H 2 O 2 , which is an oxidant, is generated by the OH radicals formed by dissociation of water molecules and their combination, and monodisperse iron oxide nanoparticles Can be produced. In addition, the heat exchanger may serve to cool some of the heat generated when the fluid passes through the chamber.
Hereinafter, a method for producing monodispersed iron oxide nanoparticles using the ultra-high pressure homogenizer of the present invention will be described in detail.
The method for producing monodisperse iron oxide nanoparticles using the ultra-high pressure homogenizer of the present invention comprises:
(a) preparing a solution of iron hydroxide,
(b) injecting the prepared iron hydroxide solution into an injection port of a sample and applying ultrahigh pressure to the sample through a pressure pump,
(c) passing the ultrahigh pressure iron hydroxide solution through a fine orifice nozzle chamber to obtain a precipitate, and
(d) washing and drying the precipitate of step (c)
.
The monodisperse iron oxide nanoparticles of the present invention can be produced by the above-described production method, so that the separation process of the monodisperse iron oxide nanoparticles is not necessary, thereby simplifying the process and shortening the process time. In addition, the uniformly sized iron oxide nanoparticles Is produced.
Further, the present invention is characterized in that monodisperse iron oxide nanoparticles are produced in an eco-friendly manner by simplifying the process, shortening the processing time, and utilizing the radical reaction by the ultra-high pressure homogenizer without adding any oxidizer and hydrothermal synthesis.
The iron hydroxide solution of step (a) may be prepared by dissolving an iron oxide precursor in distilled water to prepare a precursor aqueous solution, followed by adding a precipitant solution.
The iron oxide precursor is a ferrous salt and specifically includes one or more selected from the group consisting of iron chloride (FeCl 2 ), ferrous sulfate (FeSO 4 ) and iron acetate (Fe (CH 3 COO) 2 ) Can be used.
The concentration of the precursor aqueous solution can determine the size and uniformity of the particles. Therefore, it is preferably 0.01 to 5 moles, more preferably 0.1 to 1 mole.
The precipitant solution is used to prepare a Fe (OH) 2 precipitate of a Fe 2+ ion solution. Specifically, for example, any one or two or more selected from the group consisting of ammonia water, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium hydrogencarbonate and tetramethylammonium can be mixed and used. It is best to use the easiest sodium hydroxide.
The precipitant solution is preferably used to adjust the basicity of the iron hydroxide solution to a basic level, preferably pH 9 to 13, more preferably 10 to 12. When the pH of the iron hydroxide solution is 9 or less, Fe 2+ does not change to Fe (OH) 2 and may remain in some Fe 2+ state. When the pH is above 13, Is in the above range.
In the step (b), when the solution of iron hydroxide is injected into the injection port of the sample, it can be automatically flowed into the pressure pump, and the pressure pump can move the solution of the iron hydroxide into the nozzle chamber of the fine orifice.
As the diameter of the fine orifice nozzle chamber is small, it is possible to generate a high energy by applying a high pressure, but the throughput per minute can be reduced, so that it is not limited. For example, it is preferable to use a material having a diameter of 60 to 250 μm . The temperature of the micro-orifice nozzle chamber is preferably 20 to 80 ° C in order not to affect the physical properties of the iron hydroxide solution, but is not limited thereto.
In the step (c), a high-energy energy is generated due to shear and cavitation by passing the iron hydroxide solution through the fine orifice nozzle chamber, thereby generating OH radicals and H 2 O 2 due to dissociation of water molecules, . In addition, a micro-orifice nozzle chamber that generates high energy can act as an autoclave and affect nucleation and crystal growth.
Since most of the methods for producing nanoparticles react with complex process conditions at high temperatures, there are many restrictions on the conditions of the apparatus. However, the monodisperse iron oxide nanoparticles according to the present invention are produced by passing monodisperse iron oxide nanoparticles at room temperature through an ultra- Nanoparticles can be synthesized. As the process time is shortened, the productivity is expected to be improved and the manufacturing facility is simplified.
The radical reaction of water molecule according to the ultra-high pressure homogenizer of the present invention can be represented by the following
[Reaction Scheme 1]
H 2 O → H + OH
H + H - > H 2
OH + OH - > H 2 O 2
In the
The preparation of the iron oxide nanoparticles by the ultra-high pressure homogenizer of the present invention can be represented by the following
[Reaction Scheme 2]
3Fe (OH) 2 + H 2 O 2 ? Fe 3 O 4 + 4H 2 O
The monodisperse iron oxide is a mixed oxide of FeO + Fe 2 O 3 , and Fe 2+ and Fe 3+ coexist. Therefore, Fe 2+ is oxidized to both prevents the oxidation to Fe 3+ exist with the Fe 2+ and Fe 3+ - the pressure of the ultra-high pressure homogenizer to adjust the reducing
In addition, the number of times of passage may be varied by repeating the process of transferring from the heat exchanger to the high-pressure pump during the steps (b) to (c) several times to produce iron oxide nanoparticles, By repeating 1 to 20 times, the iron oxide can be produced as monodispersed iron oxide nanoparticles, but the present invention is not limited thereto.
The step (d) is a step of washing and drying the precipitate of step (c). The washing is preferably performed using distilled water, methanol, ethanol, or the like, but it is not limited thereto as long as it is a solution that can be easily removed after washing.
The drying is preferably performed at 50 to 100 ° C for 3 to 10 hours in order to remove moisture from the sample.
The monodisperse iron oxide nanoparticles of the present invention have a spherical shape and can produce super magnetic iron oxide nanoparticles having a particle size of 10 to 30 nm.
The monodisperse iron oxide nanoparticles according to the present invention can be easily and uniformly dispersed by using an ultra-high pressure homogenizer, uniform in particle size distribution, high in crystallinity, and capable of controlling the size and physical properties of nanoparticles produced by controlling the pressure and frequency of passage of the ultra- It is characterized by controllability.
Since the present invention does not use a toxic surfactant or other dispersant, it does not require a separation process of iron oxide nanoparticles. Instead of using a hydrothermal synthesis reaction at a high temperature by adding an oxidizing agent, a radical reaction by an ultra- It is possible to simplify the manufacturing process, shorten the processing time, and produce iron oxide nanoparticles in an environmentally friendly manner.
The monodispersed iron oxide nanoparticles of the present invention exhibit uniform particle size distribution and high crystallinity, and thus can be applied to magnetic iron oxide nanoparticles such as magnetic sensors, magneto-optical elements, magnetic ink, heavy metal waste water treatment, MRI contrast agent, drug delivery system, And can be usefully used in fields.
1 is a schematic diagram of an ultra-high pressure homogenizer used in the present invention.
Figure 2 shows the interior of the micro-orifice nozzle chamber of the inventive ultra-high pressure homogenizer.
3 is a flowchart illustrating a process for preparing iron oxide nanoparticles according to the present invention.
4 is a graph showing the results of analysis of iron oxide nanoparticles prepared according to Examples 1 to 9 and Comparative Example 1 by the powder X-ray diffractometer.
FIG. 5 is a graph showing the sizes of iron oxide particles calculated by Scherrer's formula from powder X-ray diffraction analysis of iron oxide nanoparticles prepared according to Examples 1 to 9 and Comparative Example 1 according to the present invention.
6 is a transmission electron micrograph of the iron oxide nanoparticles prepared in Examples 1, 4 and 7 and Comparative Example 1 according to the present invention.
7 is a transmission electron micrograph of the iron oxide nanoparticles prepared in Examples 7, 8 and 9 and Comparative Example 1 according to the present invention.
8 is a transmission electron micrograph of the iron oxide nanoparticles prepared in Example 9 and Comparative Example 2 according to the present invention.
9 is a graph showing the magnetic properties of the iron oxide nanoparticles prepared in Examples 1, 4, 7, 8 and 9 and Comparative Examples 1 and 2 according to the present invention.
Hereinafter, the present invention will be described in more detail by way of examples, but the present invention is not limited to the following examples.
[Example 1]
2.01 g of ferrous chloride (Junsei) was added to 100 ml of aqueous solution to prepare a 0.1 M ferrous chloride solution. A 0.85 M sodium hydroxide solution prepared by dissolving 1.02 g of sodium hydroxide (Phenoxygen) in 30 ml of distilled water was added to 100 ml of the 0.1 M ferrous chloride aqueous solution prepared above, and the mixture was mixed at room temperature for 5 minutes to prepare a green ferric hydroxide suspension . The ferrous hydroxide suspension was passed once through an ultra-high pressure homogenizer (Il Shin autoclave, NH-300) at a pressure of 500 bar to obtain a black precipitate. The precipitate was washed with distilled water and ethanol to remove residual ions, and then dried at 80 DEG C for 6 hours to obtain iron oxide nanoparticles. The results of measuring the physical properties by the above method are shown in Tables 1, 4 to 6 and 9.
[Example 2]
The iron oxide nanoparticles were prepared in the same manner as in Example 1 except that the ferrous hydroxide suspension was passed through the ultra-high pressure homogenizer three times in Example 1. The results of measuring the physical properties by the above method are shown in Tables 1, Is shown in Fig.
[Example 3]
Iron oxide nanoparticles were prepared in the same manner as in Example 1 except that the ferrous hydroxide suspension was passed through an ultra-high pressure homogenizer five times in Example 1, and the physical properties of the iron oxide nanoparticles were measured. The results are shown in Tables 1, 4, 5, Is shown in Fig.
[Example 4]
Iron oxide nanoparticles were prepared in the same manner as in Example 1 except that the pressure was applied at 1,000 bar in Example 1, and physical properties of the iron oxide nanoparticles were measured. The results are shown in Tables 1, 4 to 6 and 9 .
[Example 5]
Iron oxide nanoparticles were prepared in the same manner as in Example 1 except that the pressure of 1,000 bar was applied to the suspension of Example 1 and the ferrous hydroxide suspension was passed through the ultra-high pressure homogenizer three times. 1, Figs. 4 and 5, and Fig.
[Example 6]
Iron oxide nanoparticles were prepared in the same manner as in Example 1 except that the pressure of 1,000 bar was applied to the suspension of Example 1 and the suspension of ferrous hydroxide was passed through the ultra-high pressure homogenizer five times. 1, Figs. 4 and 5, and Fig.
[Example 7]
Iron oxide nanoparticles were prepared in the same manner as in Example 1 except that the pressure was applied at 1,500 bar in Example 1, and physical properties of the iron oxide nanoparticles were measured. The results are shown in Tables 1, 4 to 7, and FIG.
[Example 8]
Iron oxide nanoparticles were prepared in the same manner as in Example 1, except that the pressure of 1,500 bar was applied to the suspension of Example 1, and the ferrous hydroxide suspension was passed through the ultra-high pressure homogenizer three times. 1, Figs. 4, 5, 7 and Fig. 9.
[Example 9]
Iron oxide nanoparticles were prepared in the same manner as in Example 1 except that the pressure of 1,500 bar was applied to the suspension of Example 1 and the ferrous hydroxide suspension was passed through the ultra-high pressure homogenizer five times. 1, 4, 5 and 7 to 9.
[Comparative Example 1]
2.01 g of ferrous chloride (Junsei) was added to 100 ml of aqueous solution to prepare a 0.1 M ferrous chloride solution. 0.85 M sodium hydroxide solution prepared by dissolving 1.02 g of sodium hydroxide (Phenoxygen) in 30 ml distilled water was added to 100 ml of the 0.1 M ferrous chloride aqueous solution prepared above, and the mixture was uniformly stirred at room temperature for 1 hour to obtain a precipitate. The precipitate was washed with distilled water and ethanol to remove residual ions, and then dried at 80 DEG C for 6 hours to obtain iron oxide nanoparticles. The results of measuring the physical properties by the above method are shown in Table 1, Figs. 4 to 7, and Fig.
[Comparative Example 2]
2.01 g of ferrous chloride (Junsei) was added to 100 ml of aqueous solution to prepare a 0.1 M ferrous chloride solution. A 0.85 M sodium hydroxide solution prepared by dissolving 1.02 g of sodium hydroxide (tertiary octane) in 30 ml of distilled water was added to 100 ml of the 0.1 M ferrous chloride aqueous solution prepared above, and ultrasonic irradiation was performed at a power of 250 W for 1 hour at room temperature To obtain a precipitate. The precipitate was washed with distilled water and ethanol to remove residual ions, and then dried at 80 DEG C for 6 hours to obtain iron oxide nanoparticles. The results of measuring the physical properties by the above method are shown in Tables 1, 8 and 9.
[Comparative Example 3]
2.01 g of ferrous chloride (Junsei) was added to 100 ml of aqueous solution to prepare a 0.1 M ferrous chloride solution. A 0.85 M sodium hydroxide solution prepared by dissolving 1.02 g of sodium hydroxide (Phenoxygen) in 30 ml of distilled water was added to 100 ml of the 0.1 M ferrous chloride aqueous solution prepared above, stirred at room temperature for 30 minutes, and a ferrous hydroxide suspension was prepared . A precipitate was obtained by irradiating the ferric hydroxide aqueous solution at an irradiation dose of 300 kGy at a current of 3.0 mA with an electron beam energy of 1.0 MeV. The precipitate was washed with distilled water and ethanol to remove residual ions, and then dried at 60 ° C. for 6 hours to obtain iron oxide nanoparticles. Table 1 shows the results of measuring the physical properties by the above method.
[Table 1]
Crystal Structure Analysis of Iron Oxide Nanoparticles
Crystallinity of the iron oxide nanoparticles prepared by the manufacturing method of the present invention was analyzed using a powder X-ray diffractometer (Rigaku, SmartLab) and the results are shown in FIG.
As shown in FIG. 4, the particles produced in the above example were shown as iron oxide (Fe 3 O 4 ), but in the case of Comparative Example 1 in which the ultra-high pressure homogenizer was not passed, iron oxide and FeOOH were mixed. From these results, it was confirmed that the iron oxide prepared using the ultra - high pressure homogenizer had high crystallinity and was synthesized as pure iron oxide free of impurities.
From the powder X-ray diffraction analysis results, the average particle size of the iron oxide nanoparticles prepared using the Scherrer formula was determined. The average particle size is shown in FIG. 5, and it is confirmed that the particle size can be controlled according to the pressure and the number of passes of the ultra-high pressure homogenizer.
In FIG. 5, it was confirmed that the particle size of Example 9 was larger than that in Example 3 when the ultra-high pressure homogenizer was passed five times at 1,500 bar and then passed three times at 1,500 bar. This seems to be a phenomenon that the crystal growth rate accelerates from the fifth pass. Particle size depends on nucleation time and crystal growth time. The shorter the nucleation time and the longer the crystal growth time, the smaller the particle size. Therefore, the particle size is increased again because the crystal growth is accelerated more than 1500
Size and morphology analysis of iron oxide nanoparticles
The size and shape of the iron oxide nanoparticles prepared by the manufacturing method of the present invention were analyzed with a transmission electron microscope (TEM, FEI, TecnaiG 2 F30 S-Twin), and the results are shown in FIGS. 6, 7 and 8 .
The grid was a 3 mm diameter copper grid coated with carbon.
As shown in FIGS. 6 and 7, the iron oxide nanoparticles prepared in Examples 1, 4, 7, 8, and 9 according to the present invention showed spherical shapes, and the average sizes of the iron oxide nanoparticles were 24, 22, 20, 17, and 22 nm, respectively. However, the particles produced in Comparative Example 1 were not single phase such as spherical iron oxide and rod-shaped FeOOH, and the size distribution was also observed to be non-uniform.
As shown in FIG. 8, it was confirmed that the iron oxide particles produced by the ultrasonic irradiation of Comparative Example 2 also showed sticky FeOOH.
6, 7 and 8, iron oxides prepared by the examples according to the present invention have spherical shapes and iron oxide single phases, while the comparative iron oxides produced by simple agitation and ultrasonic irradiation have rod shapes ≪ / RTI > of FeOOH were present together and had an uneven particle size distribution. In addition, it was confirmed that the iron oxides synthesized through the examples were made with particles of 25 nm or less.
Analysis of magnetic properties of monodisperse iron oxide nanoparticles
In order to examine the magnetic properties of the iron oxide nanoparticles produced by the production method of the present invention, magnetic characteristics were analyzed with a vibrating sample magnetometer at room temperature and shown in FIG. 9 and Table 1.
In Examples 7 and 8, it was confirmed that the coercive force and the residual magnetization value were zero and that the super magnetism characteristics were obtained. Also, the magnetization value measured at 10 KOe is much smaller than the saturation magnetization value of 92 emu / g for the bulk sample. The reduction of the magnetization value at the ㎚ size was confirmed to be due to the incomplete crystallographic structure and the spin tilt due to the surface effect caused by the reduction of the particle size.
10: Sample inlet
11: Pressure pump
12: Pressure gauge
13: Heat exchanger
14: Outlet
15: recirculation transfer pipe
20: fine orifice nozzle chamber
21: Orifice
Claims (10)
b) washing and drying the precipitate of step a)
Wherein the monodisperse iron oxide nanoparticles are prepared by using an ultra-high pressure homogenizer.
Wherein the iron hydroxide solution is prepared by dissolving an iron oxide precursor in distilled water to prepare a precursor aqueous solution and then adding a precipitation agent solution to prepare a solution of iron hydroxide, wherein the ultra-high pressure homogenizer is used.
Wherein the iron oxide precursor is any one selected from ferrous chloride (FeCl 2 ), ferrous sulfate (FeSO 4 ), and iron acetate (Fe (CH 3 COO) 2 ).
Wherein the precipitant solution is one or more selected from the group consisting of ammonia water, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium hydrogencarbonate and tetramethylammonium.
Wherein the precursor aqueous solution has a concentration of 0.01 to 5 moles.
Wherein the micro-orifice nozzle chamber included in the ultra-high pressure homogenizer has a diameter of 60 to 250 占 퐉.
Wherein the micro-orifice nozzle chamber temperature is 20 to 80 ° C.
Wherein the precipitate obtained in the step a) is repeatedly passed through the ultra-high pressure homogenizer for 1 to 20 times, thereby producing a monodisperse iron oxide nanoparticle using an ultra-high pressure homogenizer.
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| PCT/KR2014/011747 WO2015182840A1 (en) | 2014-05-30 | 2014-12-03 | Method for preparing monodispersed iron oxide nanoparticles using super-high pressure homogenizer and monodispersed iron oxide nanoparticles prepared thereby |
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| KR101882731B1 (en) | 2017-05-08 | 2018-07-30 | 한국지역난방공사 | Apparatus for reducing iron oxide inside of heat transporting pipe and |
| KR102006215B1 (en) * | 2018-01-31 | 2019-08-01 | 충남대학교산학협력단 | Method of manufacturing iron oxide nanoparticles using a high-pressure homogenizer |
| KR20200045716A (en) | 2018-10-23 | 2020-05-06 | 한국기초과학지원연구원 | Method for manufacturing magnetite nanoparticles of spindle structure |
| KR20220100393A (en) | 2021-01-08 | 2022-07-15 | 한밭대학교 산학협력단 | Iron oxide nanoclusters for hyperthermia and method for manufacturing the same |
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| WO2015182840A1 (en) | 2015-12-03 |
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