KR20130000458A - Treating method of particle surface and particle manufactured by the same - Google Patents

Abstract

PURPOSE: A method for treating a particle surface and a particle prepared by the same are provided to ensure the particle has an excellent magnetic property without surface treatment with silica(TEOS) or polyethylene glycol(PEG) and to enhance dispersibility of the particle in a fat soluble solvent. CONSTITUTION: A method for treating a particle surface for enhancing dispersibility of particles comprises: a step of treating the particles with an acid(a); a step of mixing the acid-treated particles with a water soluble solvent to form a hydroxyl group(-OH)(b); and a step of mixing the particles containing hydroxy groups with a surface treatment containing an organic ligand which binds with the hydroxy group(c). [Reference numerals] (a) Treating particles with acid; (AA) Start; (b) Mixing with a water soluble solvent; (BB) End; (c) Mixing with a surface treatment agent

Description

Particle surface treatment method and the particles produced thereby {TREATING METHOD OF PARTICLE SURFACE AND PARTICLE MANUFACTURED BY THE SAME}

The present invention relates to a particle surface treatment method and a particle produced thereby. More specifically, the present invention relates to a particle surface treatment method for improving dispersibility in polar and nonpolar solvents and to particles produced thereby.

Magnetic nano-sized particles have been applied to various bio industries such as drug delivery materials and contrast agents and to display fields using the characteristics of photonic crystals. As the material of the particles, iron oxide is mainly used.

Since iron oxide is toxic, has low oxidation resistance and is non-hydrophilic, it requires surface treatment with inorganic and organic compounds such as silica (TEOS) and polyethylene glycol (PEG).

However, when silica (TEOS) or PEG is treated on the surface of the iron oxide particles, there is a problem of weakening the magnetic properties of the iron oxide particles, and in the oil-soluble solvent, the dispersibility is remarkably inferior and there is a problem that the individual iron oxide particles are agglomerated with each other.

In addition, since the surface treatment at high pressure and high temperature conditions are dangerous and there is a problem that is not suitable for mass production.

In order to solve the above problems, the present invention does not require surface treatment of silica (TEOS) or polyethyleneglycol (PEG), has excellent magnetic properties, excellent dispersibility in a fat-soluble solvent, and atmospheric pressure. An object of the present invention is to provide a particle surface treatment method capable of mass production even under the following conditions.

Another object of the present invention is to provide a particle produced by the particle surface treatment method.

According to a first aspect of the invention, a particle surface treatment method comprises the steps of acid treating the particles such that the particles have a positive charge, and mixing the acid treated particles with a water-soluble solvent to form a hydroxyl group (-OH) on the particles. Forming a hydroxyl group, and mixing the hydroxyl group-containing particles with a surface treating agent including an organic ligand that binds to the hydroxyl group.

When the particles are magnetic particles, the particles are Cr, Ni, Ti, Zr, Fe, Co, Zn, Gd, Ta, Nb, Pt, Au, Mg, Mn, Pd, Sr, Ag, Ba, Cu, W It may include at least one component of Mo, Sn, Pb.

The particles may include clusters in which a plurality of particles are aggregated. The acid may be hydrochloric acid (HCl), acetic acid (CH ₃ COOH), sulfuric acid (H ₂ SO ₄ ), nitric acid (HNO ₃ ), formic acid, citric acid, citric acid, lactic acid, It may include at least one of amino acids.

When the plurality of particles are dispersed in a water-soluble solvent or a fat-soluble solvent, steric effects may occur between the plurality of particles by the organic ligands formed in the plurality of particles.

The surface treating agent including the organic ligand may include a carboxyl group, a hydroxy group, an amine group, a vinyl group, an acrylate group, an acrylate group, and an alkoxy group. group), a ketone group, an ester group, and an aldehyde group.

Surface treatment agent containing the organic ligand, ricinoleic acid (Ricinoleic acid), linoleic acid (Linoleic acid), monostearin (Monostearin), palmitic acid (Palmitic acid), octadecylamine (Octadecylamin), trioctyl phos Trinoctylphosphine oxide, oleic acid, stearic acid, poly methylmethacrylate, polystyrene, sorbitol monooleate, sorbitan trioleate (Sorbitan trioleate), Myristoleic acid, Palmitoleic acid, Sapienic acid, Arachidonic acid, Alpha-Linolenic acid, Eicosa At least one of penicenoic acid (Eicosapentaenoic acid), erucic acid (Erucic acid), docosahexaenoic acid, Trioctylphosphate, hexadecylamino, Hexadecylamino, Fatty acid series, and olefin series artillery Can.

According to a second aspect of the present invention, there is provided a method of acidifying a particle such that the particle has a positive charge, and mixing the acid treated particle with a water-soluble solvent to form hydroxyl (-OH) on the surface of the particle. And surface-treated particles are provided by mixing the particles with the hydroxyl group formed therein with a surface treating agent comprising an organic ligand that binds to the hydroxyl group.

When the particles are magnetic particles, the particles are Cr, Ni, Ti, Zr, Fe, Co, Zn, Gd, Ta, Nb, Pt, Au, Mg, Mn, Pd, Sr, Ag, Ba, Cu, W It may include at least one component of Mo, Sn, Pb.

The particles may include clusters in which a plurality of particles are aggregated. The acid is hydrochloric acid (HCl), acetic acid (CH ₃ COOH), sulfuric acid (H ₂ SO ₄ ), nitric acid (HNO ₃ ), formic acid (citric acid), citric acid, lactic acid, amino acid (Amino acid It may include at least one of).

When the plurality of particles are dispersed in a water-soluble solvent or a fat-soluble solvent, steric effects may occur between the plurality of particles by the organic ligands formed in the plurality of particles.

The surface treating agent including the organic ligand is a carboxyl group, a hydroxy group, an amine group, a vinyl group, an acrylate group, an alcohol group, an alcohol group. ), A ketone group, an ester group, and an aldehyde group.

The surface treatment agent containing the organic ligand is ricinoleic acid (Ricinoleic acid), linoleic acid (Linoleic acid), monostearin (Monostearin), palmitic acid (Palmitic acid), octadecylamine (Octadecylamin), trioctylphosphine Oxygen (Trioctylphosphine oxide), Oleic acid, Stearic acid, Poly methylmethacrylate, Polystyrene, Sorbitol monooleate, Sorbitol trioleate Sorbitan trioleate, Myristoleic acid, Palmitoleic acid, Sapienic acid, Arachidonic acid, Alpha-Linolenic acid, Eicosapenta It contains at least one of Eicosapentaenoic acid, Erucic acid, Docosahexaenoic acid, Trioctylphosphate, Hexadecylamino, Fatty acid series, and olefin series. can do.

The particle surface treatment method according to the present invention is excellent in dispersibility even in a fat-soluble solvent by the steric hindrance effect of the organic ligand while maintaining excellent magnetic properties without surface treatment of silica (TEOS) or polyethylene glycol (PEG). In addition, there is no effect of high pressure production conditions and coating of silica (TEOS) or PEG has the effect of enabling mass production in a simple process.

1 is a flow chart of the particle surface treatment method according to an embodiment of the present invention.
FIG. 2 is an image of iron oxide particles (black) of FIG. 1 and iron oxide particles after step b treatment (red color) analyzed using TF-IR.
3 is an image of the first iron oxide particles (black) and the iron oxide particles after the step c treatment (red) using TF-IR.
FIG. 4 is data obtained by measuring the degree of dispersion between particles according to the steps a (black), b (red), and c (blue) of FIG. 1.
FIG. 5 is an image obtained by analyzing FT-IR of iron oxide particles (black) and iron oxide particles treated after organic ligand (red) in the first embodiment.
6 is data obtained by measuring the degree of dispersion between particles produced by the second embodiment.
FIG. 7 is an image obtained by analyzing FT-IR of iron oxide particles (black) and iron oxide particles treated after organic ligand (red) in the first embodiment.
8 is data obtained by measuring the degree of dispersion between particles prepared by the third embodiment.
FIG. 9 is an image obtained by analyzing FT-IR of iron oxide particles (black) and iron oxide particles treated after organic ligand treatment (red color) according to the fourth embodiment.
10 is data obtained by measuring the degree of dispersion between particles produced by the fourth embodiment.

DETAILED DESCRIPTION OF THE INVENTION The following detailed description of the invention refers to the accompanying drawings that illustrate specific embodiments in which the invention may be practiced. These embodiments are described in sufficient detail to enable those skilled in the art to practice the invention. It should be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. The terms first, second, etc. may be used to describe various elements, but the elements should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In this application, the terms "comprise" or "having" are intended to indicate that there is a feature, number, step, operation, component, or combination thereof described in the specification, but one or more other features or numbers, It should be understood that it does not exclude in advance the possibility of the presence or addition of steps, actions, components or combinations thereof. Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art.

Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the meaning in the context of the relevant art and are to be interpreted as ideal or overly formal in meaning unless explicitly defined in the present application Do not.

Magnetic Nanoparticles Manufacturing

First, prior to the description of the particle surface treatment method of the present invention, it will be described from the production method of the particles used therein. The manufacturing method of the particle | grains demonstrated below demonstrated the Example of the particle used for the particle surface treatment method of this invention, and should not be interpreted limited to the following Example.

The particles used in the particle surface treatment method of the present invention may have magnetic properties. For example, the particles are Cr, Ni, Ti, Zr, Fe, Co, Zn, Gd, Ta, Nb, Pt, Au, Mg, Mn, Pd, Sr, Ag, Ba, Cu, W, Mo, Sn It may include at least one component of Pb. The particles may comprise an oxidized state. In addition, the magnetic particles may contain different kinds of metals. For example, the magnetic particles may be represented by the following general formulas (1) to (4).

Formula 1

M (M is a magnetic metal atom or alloy thereof)

Formula 2

M _a O _b (0 <a≤20, 0 <b≤20, M is a magnetic metal atom or alloy thereof)

Formula 3

M _c M ' _d (0 <c≤20, 0 <d≤20, M is a magnetic metal atom or alloy thereof; M' is a Group 2 element, transition metal, Group 13 element, Group 14 element, 15 An element selected from the group consisting of a group element, a lanthanide element, and an actinium group element)

Formula 4

M _a M ' _e O _b (0 <a≤20, 0 <e≤20, 0 <b≤20, M is a magnetic metal atom or alloy thereof; M' is a Group 2 element, transition metal, 13 An element selected from the group consisting of a group element, a group 14 element, a group 15 element, a lanthanide element, and an actinium element)

Formulas 1 and 3 are magnetic particles composed of a single metal or an alloy and at least two kinds of metals, and Formulas 2 and 4 represent magnetic particles made of a metal oxide including a single metal or an alloy and two or more kinds of metals.

In the method of preparing the particles, first, the magnetic precursor and the anionic ligand are added to the solvent to dissolve to prepare an amorphous metal gel solution.

Here, the magnetic precursor is a metal nitrate-based compound, a metal sulfate-based compound, a metal fluoroacetoacetate-based compound, a metal halide (MX _a , M = Cr, Ni, Ti, Zr, Fe, Co, Zn, Gd, Ta, Nb, Pt, Au, Mg, Mn, Pd, Sr, Ag, Ba, Cu, W, Mo, Sn, Pb, X = F, Cl, Br, I, 0 <a≤5) The compound may be selected from the group consisting of a compound, a metal perchloroate-based compound, a metal sulfamate-based compound, a metal styreate-based compound, and an organometallic-based compound, but is not limited thereto.

The anionic ligands include neutral ligands such as alkyltrimethylammonium halide-based cationic ligands, alkyl acids, trialkylphosphines, trialkylphosphine oxides, alkyl amines and alkyl thiols, sodium alkyl sulfates, sodium alkyl carboxylates and sodium alkyls. It may be selected from the group consisting of anionic ligands such as phosphate and sodium acetate, but is not necessarily limited thereto.

The solvent may be selected from the group consisting of an organic solvent, an aromatic solvent, a heterocyclic solvent, a sulfoxide solvent, an amide solvent, a hydrocarbon solvent, an ether solvent, a polymer solvent, an ionic liquid solvent, a halogen hydrocarbon solvent, an alcohol solvent, and water. However, the present invention is not limited thereto. In some cases, two or more kinds selected from the anion ligands may be used together or sequentially.

In this case, in addition to a single kind of magnetic precursor, metal halides (MX _a , M = Cr, Ni, Ti, Zr, Fe, Co, Zn, Gd, Ta, Nb, Pt, Au, Mg, Mn, Pd, Sr, Ag, Ba, Cu, W, Mo, Sn, Pb, X = F, Cl, Br, I, 0 <a ≤ 5) heterogeneous precursor consisting of a compound of the series may be further included. The dissimilar precursor metal M added is a metal of a different kind from the metal contained in the magnetic precursor. As a result, magnetic particles containing different metals can be produced. The heterogeneous precursor is preferably added in an amount of 1 to 99 parts by weight per 100 parts by weight of the magnetic precursor, but is not necessarily limited thereto. As the heterogeneous precursor is contained in the magnetic precursor, the magnetic properties of the finally obtained particles may be enhanced or variously deformed into superparamagnetism, paramagnetic, ferromagnetic, antiferromagnetic, ferrimagnetic, and diamagnetic. Can be adjusted to specific characteristics.

Subsequently, the prepared amorphous metal gel solution is heated to phase change into magnetic particles having crystallinity. For example, the amorphous metal gel solution can be heated at 30 ° C to 200 ° C to form magnetic particles having a more stable crystal structure. In addition, as the magnetic particles are heated again at 100 ° C. to 350 ° C. to proceed with a reduction reaction, magnetic clusters in which the magnetic particles are agglomerated with each other may be prepared.

According to the method described above, particles having magnetic properties such as magnetite (Fe ₃ O ₄ ), hematite (α-Fe ₂ O ₃ ), and magnetite (γ-Fe ₂ O ₃ ) can be produced.

In addition, the particles may have an average particle size of 1 ~ 200nm, it is also possible to produce a cluster consisting of a plurality of the particles are not an individual single particles.

Particle surface treatment

Hereinafter, a particle surface treatment method according to an embodiment of the present invention will be described.

1 is a flow chart of the particle surface treatment method according to an embodiment of the present invention.

Referring to FIG. 1, in the particle surface treatment method according to an embodiment of the present invention, first, (a) the particles are acid treated. (B) The acid treated particles are then mixed with a water soluble solvent. Next, it mixes with (c) surface treating agent. Hereinafter, each step will be described in detail.

In the step (a) of acid treating the particles, the acidic material may be variously applied in consideration of acidity according to the components of the magnetic particles. For example, the acid may be hydrochloric acid (HCl), acetic acid (CH ₃ COOH), sulfuric acid (H ₂ SO ₄ ), nitric acid (HNO ₃ ), formic acid, citric acid, citric acid, lactic acid, It may include at least one of amino acids.

The acid may react with the particles to etch some of the surface of the particles. At this time, the surface of the etched particles may be partially charged with (+) charge.

In order to advance the reaction more effectively, the particles may be mixed with the acid and then stirred using a disperser.

Subsequently, the particles charged with the (+) charge are mixed with a water-soluble solvent (step b). The water-soluble solvent includes a precursor capable of introducing hydroxyl (-OH) to the particles charged with the (+) charge. For example, when the water-soluble solvent is water, the water may be temporarily bonded to the surface of the particles charged with the (+) charge. As the dehydrogenation of the bound water occurs, hydroxyl groups can be introduced to the surface of the particles. Particles into which the hydroxyl groups have been introduced may have increased dispersibility than the initial particles before acid treatment.

The organic ligand is then bound to the hydroxyl group of the particle (step c). For example, the particles into which the hydroxyl group is introduced may be mixed with a substance containing the organic ligand and stirred using a disperser. The organic ligand may include a long alkyl chain and a carboxyl group, an amine group, a vinyl group, or a phenyl group at the terminal of the alkyl chain. As the carboxyl group and the hydroxyl group of the particle surface are bonded, long alkyl chains may be formed on the surface of the particle.

Here, the material containing the organic ligand is ricinoleic acid (Ricinoleic acid), linoleic acid (Linoleic acid), monostearin (Monostearin), palmitic acid (Palmitic acid), octadecylamine (Octadecylamin), trioctyl phos Trinoctylphosphine oxide, oleic acid, stearic acid, polymethylmethacrylate, polystyrene, sorbitol monooleate, sorbitan trioleate ( Sorbitan trioleate, Myristoleic acid, Palmitoleic acid, Sapienic acid, Arachidonic acid, Alpha-Linolenic acid, Eicosapenta It contains at least one of Eicosapentaenoic acid, Erucic acid, Docosahexaenoic acid, Trioctylphosphate, Hexadecylamino, Fatty acid series, and olefin series. The.

When a plurality of particles prepared by the surface treatment method as described above are dispersed in a water-soluble solvent or a fat-soluble solvent, a steric effect is generated between the plurality of particles by the organic ligand formed on the plurality of particles. .

For example, when a plurality of the particles prepared are exposed to an external strong magnetic field on a solvent, the particles in the solvent phase may be repulsed by a steric hindrance effect caused by the alkyl chain in response to magnetic attraction between the particles. It can be easily dispersed. In addition, the repulsive force can be controlled between the particles by treating a molecule having polarization at the end of the alkyl chain.

By using the electrostatic, magnetic and steric hindrance effects, the photonic crystal structure color can be expressed by changing the spacing of the particles, which can be applied to the display field. In addition, the prepared particles have a dispersibility in a fat-soluble solvent, it is possible to encapsulate through a coacervation method using the O / W emulsification method. Therefore, the encapsulated particles can be formed into a desired pattern by using a screen printing method, and it is also applicable to a functional film by applying it on a transparent film.

The particle surface treatment method according to the present invention does not surface-treat silica (TEOS) or polyethylene glycol (PEG), and maintains excellent magnetic properties, but has excellent dispersibility even in a fat-soluble solvent by a steric hindrance effect. In addition, high-pressure production conditions and coating of silica or PEG are not required, allowing mass production in a simple process.

Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only for illustrating the present invention, it is obvious to those skilled in the art that the scope of the present invention is not limited to these examples.

<First Example >

<Production of Magnetic Iron Oxide Particles>

50 g of iron chloride hydrate, 50 g of sodium hydroxide, and 50 g of water were added to 1000 ml ethylene glycol as an organic solvent and dissolved at 90 ° C. The solution was refluxed at a high temperature of 190 ° C. and a black precipitate was obtained after the reaction was completed. This was centrifuged at 4,000 rpm for 30 minutes using a centrifugal separator, and then purified by washing with ethanol and water to obtain magnetic iron oxide particles having an average particle size of 200 nm.

< Of hydroxyl (-OH)  Surface Treatment>

5 g of magnetic iron oxide particles were mixed with 200 ml of 1 M hydrochloric acid (HCl), followed by stirring for 10 minutes using a disperser. The surface potential of the iron oxide particles was not detected before mixing with hydrochloric acid, but the surface potential of the iron oxide particles after mixing with hydrochloric acid was 33.6 mV. Therefore, as the surface of the iron oxide particles are etched, the surface of the particles may be confirmed to be charged with a partial (+) charge.

The etched iron oxide particles were then mixed with an aqueous solvent to remove the remaining hydrochloric acid. At this time, the iron oxide particles charged with the (+) charge undergoes a dehydrogenation reaction with the water molecules present in the aqueous solvent, and a plurality of hydroxyl groups (-OH) are bonded to the surface. Here, after mixing with the aqueous solvent, the surface potential of the iron oxide particles was detected to be -23.5 mV.

FIG. 2 is an image of iron oxide particles (black) of FIG. 1 and iron oxide particles after step b treatment (red color) analyzed using TF-IR. Referring to FIG. 2, after the steps a and b, the detection peaks in the typical 3,400 cm ⁻¹ to 3,650 cm ⁻¹ band of the hydroxyl group can be identified. Therefore, it can be confirmed that the hydroxyl group was introduced to the surface of the iron oxide particles.

<Organic Ligand  Introduction>

5 g of iron oxide particles into which the hydroxyl group was introduced were mixed with 200 ml of oleic acid, dispersed for 30 minutes using a disperser, and then stirred for 4 hours to prepare iron oxide particles surface-treated with oleic acid.

3 is an image of the first iron oxide particles (black) and the iron oxide particles after the step c treatment (red) using TF-IR. Referring to FIG. 3, detection peaks of typical 2,850 cm ⁻¹ to 3,000 cm ⁻¹ and 1,375 cm ⁻¹ to 1,450 cm ⁻¹ bands of an alkyl group that is a molecule constituting oleic acid can be confirmed. In addition, the detection peak of the typical 1710 cm ^-1 band of the carboxyl group which is a molecule constituting oleic acid can be confirmed. Therefore, it can be confirmed that oleic acid is treated on the surface of the magnetic particles.

FIG. 4 is data obtained by measuring the degree of dispersion between particles according to the steps a (black), b (red), and c (blue) of FIG. 1.

Referring to FIG. 4, if the degree of dispersion between the iron oxide particles is improved, the iron oxide particles should not be agglomerated with each other and should be close to 200 nm, which is the size of the initial iron oxide particles. In addition, if the degree of dispersion between the iron oxide particles is improved, the uniform particle density (Intensity) should appear as a large value. As the particle surface treatment of the present invention proceeded, it was confirmed that the particles gradually approached the 200 nm band, which is the size of the initial iron oxide particles, and the particle intensity having the size of the initial iron oxide particles gradually increased. Through these results, it was confirmed that the dispersibility of the particles increases as the particle surface treatment proceeds, respectively.

<2nd Example >

This second embodiment was carried out in the same manner as the preparation of the magnetic iron oxide nanoparticles of the first embodiment, the surface treatment of the hydroxyl group. Hereinafter, the organic ligand treatment and data analysis according to the second embodiment will be described.

200 g of organic ligand precursor was prepared by mixing 5 wt% of 10 g octadecyl amine solid in 190 g tetrachloroethylene, which is a nonpolar solvent.

5 g of iron oxide particles having a hydroxylated surface were mixed with the organic ligand precursor, dispersed for 30 minutes using a disperser, and stirred with a stirrer for 4 hours to prepare iron oxide particles surface-treated with octadecyl amine.

FIG. 5 is an image obtained by analyzing FT-IR of iron oxide particles (black) and iron oxide particles treated after organic ligand (red) in the first embodiment. Referring to FIG. 5, the detection peaks of the typical 2,850 cm ⁻¹ to 3,000 cm ⁻¹ and 1,375 cm ⁻¹ to 1,450 cm ⁻¹ bands of the alkyl group which are the molecules constituting the octadecyl amine can be confirmed. In addition, the detection peaks of the typical 3,300 cm ^-1 to 3,500 cm ^-1 and 1,600 cm ^-1 band of the amine group which is a molecule constituting the octadecyl amine can be confirmed. Therefore, it can be confirmed that the surface of the magnetic particles is treated with octadecyl amine.

6 is data obtained by measuring the degree of dispersion between particles produced by the second embodiment.

Referring to FIG. 6, black shows a dispersion degree between particles as a step a, a red step b, and a blue step c are performed.

As the particle surface treatment of the present invention proceeded, it was confirmed that the particles gradually approached the 200 nm band, which is the size of the initial iron oxide particles, and the particle intensity having the size of the initial iron oxide particles gradually increased. Through these results, it was confirmed that the dispersibility of the particles increases as the particle surface treatment proceeds, respectively.

<Third Example >

This third embodiment was carried out in the same manner as the preparation of the magnetic iron oxide nanoparticles of the first embodiment, the surface treatment of the hydroxyl group. Hereinafter, the organic ligand treatment and data analysis thereof according to the third embodiment will be described.

200 g of an organic ligand precursor was prepared by mixing 20 g of polystyrene solid (10 wt%) in 180 g of tetrachloroethylene, which is a nonpolar solvent.

5 g of iron oxide particles surface-treated with a hydroxyl group were mixed with the organic ligand precursor, dispersed for 30 minutes using a disperser, and stirred with a stirrer for 4 hours to prepare iron oxide particles surface-treated with polystyrene.

FIG. 7 is an image obtained by analyzing FT-IR of iron oxide particles (black) and iron oxide particles treated after organic ligand (red) in the first embodiment. Referring to FIG. 7, detection peaks of the typical 2,850 cm ⁻¹ to 3,000 cm ⁻¹ band of the alkyl group constituting polystyrene can be confirmed. In addition, the detection peak of the typical 700 cm ^-1 to 900 cm ^-1 band of the phenyl group constituting polystyrene can be confirmed. Therefore, it can be confirmed that polystyrene has been treated on the surface of the magnetic particles.

8 is data obtained by measuring the degree of dispersion between particles prepared by the third embodiment.

Referring to FIG. 8, black is represented by a, red is represented by b, and blue is represented by c.

As the particle surface treatment of the present invention proceeded, it was confirmed that the particles gradually approached the 200 nm band, which is the size of the initial iron oxide particles, and the particle intensity having the size of the initial iron oxide particles gradually increased. Through these results, it was confirmed that the dispersibility of the particles increases as the particle surface treatment proceeds, respectively.

<Fourth Example >

This fourth embodiment was carried out in the same manner as the preparation of the magnetic iron oxide nanoparticles of the first embodiment, the surface treatment of the hydroxyl group. Hereinafter, the organic ligand treatment and data analysis according to the fourth embodiment will be described.

200 g of an organic ligand precursor was prepared by mixing with 5 wt% of 10 g monostearin solid content in 190 g tetrachloroethylene, which is a nonpolar solvent.

5 g of iron oxide particles surface-treated with a hydroxyl group were mixed with the organic ligand precursor, dispersed for 30 minutes using a disperser, and stirred with a stirrer for 4 hours to prepare iron oxide particles surface-treated with monostearine.

FIG. 9 is an image obtained by analyzing FT-IR of iron oxide particles (black) and iron oxide particles treated after organic ligand treatment (red color) according to the fourth embodiment. Referring to FIG. 9, the detection peaks of the typical 2,850 cm ⁻¹ to 3,000 cm ⁻¹ and 1,375 cm ⁻¹ to 1,450 cm ⁻¹ bands of the alkyl group which are the molecules constituting monostearin can be confirmed. In addition, the detection peak of the typical 1,670 cm ^-1 to 1,780 cm ^-1 band of the carbonyl group constituting the monostearin (Monostearin) can be confirmed. Therefore, it can be confirmed that monostearin (Monostearin) is treated on the surface of the magnetic particles.

10 is data obtained by measuring the degree of dispersion between particles produced by the fourth embodiment.

Referring to FIG. 10, black indicates a dispersion degree between particles as a step a, a red step b, and a blue step c are performed.

As the particle surface treatment of the present invention proceeded, it was confirmed that the particles gradually approached the 200 nm band, which is the size of the initial iron oxide particles, and the particle intensity having the size of the initial iron oxide particles gradually increased. Through these results, it was confirmed that the dispersibility of the particles increases as the particle surface treatment proceeds, respectively.

Claims (14)

As a particle surface treatment method for improving the dispersibility of particles,
Acid treating the particles such that the particles have a positive charge,
Mixing the acid treated particles with a water-soluble solvent to form a hydroxyl group (-OH) on the particles;
And mixing the particles on which the hydroxyl group is formed with a surface treating agent comprising an organic ligand that binds to the hydroxyl group. The method of claim 1,
When the particles are magnetic particles, the particles are Cr, Ni, Ti, Zr, Fe, Co, Zn, Gd, Ta, Nb, Pt, Au, Mg, Mn, Pd, Sr, Ag, Ba, Cu, W Particle surface treatment method comprising at least one component of Mo, Sn, Pb. The method of claim 1,
The particle surface treatment method, characterized in that the plurality of particles (cluster) formed by agglomeration. The method of claim 1,
The acid is hydrochloric acid (HCl), acetic acid (CH3COOH), sulfuric acid (H2SO4), nitric acid (HNO3), formic acid (citric acid), citric acid (Lactic acid), amino acid (Amino acid) Particle surface treatment method comprising at least one. The method of claim 1,
When the plurality of particles is dispersed in a water-soluble solvent or a fat-soluble solvent, a steric effect is generated between the plurality of particles by the organic ligand formed on the plurality of particles. The method of claim 1,
Surface treatment agent containing the organic ligand,
Carboxyl group, hydroxyl group, amine group, Amin group, vinyl group, acrylate group, acrylate group, alkoxy group, ketone group, A particle surface treatment method comprising at least one of an ester group and an aldehyde group. The method of claim 1,
Surface treatment agent containing the organic ligand,
Ricinoleic acid, linoleic acid, monostearine, monostearin, palmitic acid, octadecylamine, trioctylphosphine oxide, oleic acid Oleic acid, stearic acid, poly methylmethacrylate, polystyrene, sorbitol monooleate, sorbitan trioleate, myristoleic acid acid), Palmitoleic acid, Sapienic acid, Arachidonic acid, Alpha-Linolenic acid, Eicosapentaenoic acid, Eleucine Particle surface treatment room comprising at least one of acid (Erucic acid), docosahexaenoic acid (Docosahexaenoic acid), trioctylphosphate (Trioctylphosphate), hexadecylamino, Fatty acid series, olefin series . Acid treating the particles so that the particles have a positive charge,
Mixing the acid treated particles with a water-soluble solvent to form hydroxyl (-OH) on the surface of the particles;
Surface-treated particles to increase the dispersibility, characterized in that the prepared by the step of mixing with the surface treatment agent comprising an organic ligand that is bonded to the hydroxyl group formed particles. 9. The method of claim 8,
When the particles are magnetic particles, the particles are Cr, Ni, Ti, Zr, Fe, Co, Zn, Gd, Ta, Nb, Pt, Au, Mg, Mn, Pd, Sr, Ag, Ba, Cu, W Surface-treated particles to increase dispersibility, comprising at least one component of Mo, Sn, Pb. 9. The method of claim 8,
The particles are surface-treated particles to increase the dispersibility, characterized in that the cluster (cluster) consisting of a plurality of particles aggregated. 9. The method of claim 8,
The acid is hydrochloric acid (HCl), acetic acid (CH ₃ COOH), sulfuric acid (H ₂ SO ₄ ), nitric acid (HNO ₃ ), formic acid (citric acid), citric acid (Lactic acid), amino acid (Amino acid) Particles surface-treated to increase dispersibility, characterized in that it comprises at least one. 9. The method of claim 8,
When the plurality of particles are dispersed in a water-soluble solvent or a fat-soluble solvent, a steric effect is generated between the plurality of particles by the organic ligands formed on the plurality of particles. Surface treated particles. 9. The method of claim 8,
Surface treatment agent containing the organic ligand,
Carboxyl group, hydroxyl group, amine group, amine group, vinyl group, acrylate group, alcohol group, alcohol group, ketone group, Particles surface-treated to increase dispersibility, characterized in that it comprises at least one of an ester group and an aldehyde group. 9. The method of claim 8,
Surface treatment agent containing the organic ligand,
Ricinoleic acid, linoleic acid, monostearine, monostearin, palmitic acid, octadecylamine, trioctylphosphine oxide, oleic acid Oleic acid, stearic acid, poly methylmethacrylate, polystyrene, sorbitol monooleate, sorbitan trioleate, myristoleic acid acid), Palmitoleic acid, Sapienic acid, Arachidonic acid, Alpha-Linolenic acid, Eicosapentaenoic acid, Eleucine Improving dispersibility, characterized in that it comprises at least one of acid (Erucic acid), docosahexaenoic acid (Docosahexaenoic acid), trioctylphosphate (Trioctylphosphate), hexadecylamino, Fatty acid series, olefin series top Sea surface treated particles.

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