KR101814491B1 - Composite particle and method for preparation thereof - Google Patents

Composite particle and method for preparation thereof Download PDF

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Publication number
KR101814491B1
KR101814491B1 KR1020160004096A KR20160004096A KR101814491B1 KR 101814491 B1 KR101814491 B1 KR 101814491B1 KR 1020160004096 A KR1020160004096 A KR 1020160004096A KR 20160004096 A KR20160004096 A KR 20160004096A KR 101814491 B1 KR101814491 B1 KR 101814491B1
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South Korea
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flame
particles
particle
composite
inert gas
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KR1020160004096A
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Korean (ko)
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KR20170084806A (en
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변정훈
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영남대학교 산학협력단
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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
    • B82B3/0061—Methods for manipulating nanostructures
    • 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
    • B82B1/008—Nanostructures not provided for in groups B82B1/001 - B82B1/007
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/08—Ferroso-ferric oxide (Fe3O4)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The present invention relates to a method for preparing composite particles, and more particularly, to a method for preparing composite particles comprising the steps of: providing precursor of a first material into a flame to obtain oxide particles of a first material; Supplying a second material particle made through a low-temperature plasma particle generator in an inert gas flow into the flame to obtain composite particles of an oxide particle and a second material particle of the first material; And controlling the crystal structure of the oxide particles of the first material by applying ultrasonic waves to the flame to simplify the process of the thin film and the fine pattern composed of the composite particles, And Which can minimize the generation of environmentally harmful substances And a method for producing the composite particles.

Description

TECHNICAL FIELD [0001] The present invention relates to a composite particle manufacturing method,

The present invention relates to a method for producing a composite particle, and more particularly, to a method for producing a composite particle capable of controlling a crystal structure.

Generally, in the case of producing a composite particle in which a metal and a metal having different chemical compositions or a metal and a ceramic material are combined, the target reaction material is mixed by using a dry or wet mixing process, The high-energy process is applied to the pretreatment.

However, the process through the above-described general process may contain impurities in preparation of the precursor material, and it is difficult to uniformly mix the materials due to the difference in properties between the material properties, resulting in a problem that the homogeneity of the final product microstructure is relatively lowered .

On the other hand, the composite particles can be largely divided into structural materials and functional materials depending on the application field. Among them, structural materials generally require high strength, so that a high relative density and fine grain are required in sintering. However, when the composite particles are produced according to the conventional high-energy process, a problem arises that a thermal activation reaction in which crystal grains grow inside the material due to a high sintering temperature is accompanied, and when the sintering temperature is high, Molds and the like are limited, and energy efficiency is reduced. In addition, it is difficult to control the crystal structure of the particles and to control the assembly and arrangement of the inorganic-inorganic particles according to need, which makes it difficult to simplify the conventional crystallization, thin film and pattern processes.

In this regard, Korean Patent Laid-Open No. 10-2011-0055890 discloses a method for manufacturing a composite particle using nanotechnology, but does not solve the above problems.

Korean Patent Publication No. 10-2011-0055890

It is an object of the present invention to provide a method for producing a composite particle capable of controlling a crystal structure.

It is another object of the present invention to provide a method for producing new composite particles capable of enhancing productivity and minimizing the generation of environmentally harmful substances by enabling continuous production.

1. providing a precursor of a first material into a flame to obtain oxide particles of a first material; Supplying a second material particle made through a low-temperature plasma particle generator in an inert gas flow into the flame to obtain composite particles of an oxide particle and a second material particle of the first material; And applying ultrasonic waves to the flame to control the crystal structure of the oxide particles of the first material.

2. The method of producing a composite particle according to 1 above, wherein the first material comprises at least one selected from the group consisting of a transition metal, a transition metal, a nonmetal, and a lanthanum source.

3. The method of claim 1, wherein the first material is injected into the flame in the form of a precursor gas or droplet.

4. The method for producing composite particles according to 1 above, wherein the second material particles are particles of a conductor or semiconductor.

5. The method of producing a composite particle according to item 1 above, wherein the flame is an inverse diffusion flame or a diffusion flame.

6. The method of producing a composite particle according to item 1 above, wherein the fuel of the flame is hydrogen or a hydrocarbon gas.

7. The method of producing a composite particle according to 1 above, wherein the inert gas comprises at least one selected from the group consisting of nitrogen, argon and helium.

8. The method of producing composite particles according to 1 above, wherein the supply of the second material particles into the flame is carried out by bringing the inert gas flow into the flame.

9. The process of claim 1, wherein oxygen is added to the inert gas stream within 5 vol% for feeding the first material into the flame

10. The method of producing a composite particle according to 1 above, wherein the ultrasonic wave has a frequency of 103 to 108 Hz.

11. The method of claim 1, wherein the ultrasonic wave is performed with a probe for applying ultrasonic waves, and the tip diameter of the probe is 0.06 to 6 times the flame diameter.

12. The method of producing composite particles according to 1 above, wherein the application intensity of the ultrasonic waves is 0.02 to 2 kW / cm < 2 >.

13. The method of claim 1, further comprising coating the composite particle with a biocompatible organic material.

The method of producing the composite particles of the present invention enables control of the crystal structure and can be applied to various fields.

Also, the method for producing a composite particle according to the present invention By making continuous production possible, productivity can be improved The occurrence of environmentally harmful substances can be minimized.

1 is a TEM photograph of Fe 3 O 4 and Au / Fe 3 O 4 as a composite particle.
FIG. 2 is a TEM and SEM photograph of Ag-TiO 2 poly ethylene glycol (PEG), which is a composite particle coated with TiO 2 and an organic material having a biocompatibility.

The present invention relates to a method for producing oxide particles, comprising: supplying a precursor of a first material into a flame to obtain oxide particles of a first material; Supplying a second material particle made through a low-temperature plasma particle generator in an inert gas flow into the flame to obtain composite particles of an oxide particle and a second material particle of the first material; And controlling the crystal structure of the oxide particles of the first material by applying ultrasonic waves to the flame, whereby the thin film process and the fine pattern process can be simplified by attaching the substrate to the substrate immediately after the production, And Which can minimize the generation of environmentally harmful substances And a method for producing the composite particles.

Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed. And shall not be construed as limited to such matters.

First, the precursor of the first material is supplied into the flame to obtain oxide particles of the first material.

This step is a step for obtaining oxide particles of the first material. In one embodiment, the precursor of the first material is vaporized by dissolving or dispersing the precursor in an appropriate solvent such as water, an acid / base solution or an organic solvent, and then the gas is introduced into the flame, To obtain fine droplets (droplets), and the droplets of the droplets can be introduced into the flame to form oxide particles. Through this step, fine oxide particles free from waste water generation can be continuously obtained.

In addition, the oxide particles produced through this step may be crystalline.

In one embodiment of the present invention, the first material is not particularly limited as long as the precursor solution or gas in the flame can form oxide particles, and the first material may be a transition metal, a pre-metal, a non-metal, and a lanthanum source And at least one selected from the group. For example, metal, and more preferably titanium (Ti) or iron (Fe).

The precursor of the first substance used in the present invention may be, for example, a salt compound of the first substance. It is preferable that such a salt compound can be dissolved or dispersed in an appropriate solvent. As such a solvent, water, an acid and base solution, and an organic solvent such as alcohol, acetone, and ether may be used.

The method of supplying the precursor of the first material into the flame can be performed using, for example, a carrier gas. As such a carrier gas, an inert gas such as argon may be used.

Also, according to a preferred embodiment of the present invention, the efficiency of the flame in which the composite particles are formed may be maintained higher by adding oxygen within 5 vol% to the stream of the inert gas. Preferably 0.05 to 5% by volume of oxygen can be added.

In the present invention, the flame may be an inverse diffusion flame or a diffusion flame, but according to an embodiment of the present invention, it may preferably be a reverse diffusion flame. The inverse diffusion flame is created as oxygen and fuel escape from the nozzle. As the fuel supply source, hydrogen gas may be used, and more preferably hydrogen gas or hydrocarbon gas. As the oxygen supply source, a mixed gas in which oxygen or oxygen is mixed can be used.

The inverse diffusion flame process according to an embodiment of the present invention can be performed by adjusting the oxidizer, the precursor, the type of fuel, the flow rate, and the like as needed. For example, the residence time in the flame and the size and temperature of the diffusion flame can be controlled by controlling the type and flow rate of the fuel, the flow rate of the oxygen and the ratio to the fuel, the oxidizer, the kind of the precursor, and the flow rate. When it is necessary to control the characteristics of the reactants or the concentration of oxygen as necessary, nitrogen (N 2 ), argon (Ar) or hydrogen (H 2 ) / nitrogen, hydrogen / A mixed gas such as argon may be used as the carrier gas.

Next, the second material particles produced through the low temperature plasma particle generator in the inert gas flow are supplied into the flame to obtain composite particles of the oxide particles of the first material and the second material particles.

In this step, the oxide particles of the first material and the second material particles forming the composite particle are supplied into the flame. When the second material particles are supplied into the flame, oxide particles of the first material may be generated on the surface of the second material particles using the second material particles as reaction nuclei to form composite particles, The oxide particles may adhere to the second material particles under high temperature flame conditions to form composite particles.

In the present invention, the second material particles can be produced through a low temperature plasma particle generator in an inert gas flow.

The low-temperature plasma particle generator is a method of vaporizing a metal component by high temperature generated by a low-temperature plasma. When a high pressure is applied to both metal electrodes, a low-temperature plasma is generated. May be condensed after vaporization to form a second material particle.

At this time, the interval between both electrodes may be in the range of 0.5 mm to 10 mm. For example, when the distance between the metal electrodes is 1 mm, when a high voltage of 2.5 kV to 3 kV is applied, a high temperature of about 5000 ° C is generated, and the components of the electrode are vaporized to form aerosol particles of the second material particles . The vaporized electrode component may be cooled by the rapidly lowering environmental temperature during the movement of the inert gas to the outside of the low temperature plasma region, which is lower in temperature than the point of generation of the low temperature plasma, and may be granulated through the condensation process.

The high voltage power source applied to the target electrode may be a direct current or an alternating current, and in the case of alternating current, the power application examples such as a square wave, a triangle wave, and an offset control may be more various.

The inert gas used in one embodiment of the present invention may include at least one selected from the group consisting of argon, nitrogen, and helium. An inert gas is used as the carrier gas of the second material particles. In one embodiment of the present invention, the inert gas may serve to transport the second material particles to the flame.

In one embodiment of the present invention, the second material particles are preferably conductor particles or semiconductor particles.

The type of the second material particles used in the present invention is not particularly limited as long as it is nanoparticles that can be produced by the low-temperature plasma, but it may preferably be an anti-oxidation metal or a transition metal. For example, , Silver, platinum, palladium, alloys of two or more of them, and preferably gold and silver may be used alone. These may be used alone or in combination of two or more. Also, in the case of a semiconductor, particles can be produced by the low-temperature plasma. Therefore, at least one of B, Si, Ge, As, Sb and Te may be used as the second material.

The concentration of the second material particles is not particularly limited, and can be used, for example, at a concentration of 10 3 to 10 16 / cm 3 in number concentration. If the concentration of water is less than 10 3 / cm 3, the number of metal nanoparticles is low and the process yield is low. If the concentration is more than 10 16 / cm 3, particles may collide with each other and cause agglomeration.

The particle size of the second material particles generated through the low-temperature plasma particle generator is not particularly limited, and may be, for example, 100 nm or less, preferably 1 nm to 20 nm. When the diameter of the second material particle is less than 1 nm, the transfer efficiency due to the inert gas may be drastically deteriorated. If the diameter of the second material particle is more than 20 nm, the adhesion between the second material particle and the oxide particle of the first material Is reduced.

The second material particles thus produced are supplied into the flame by the flow of an inert gas and combine with the oxide particles of the first material to form composite particles.

In the present invention, ultrasonic waves are applied to the flame to control the crystal structure of the oxide particles of the first material.

For example, when ultrasonic waves are applied to the composite particles in the flame through a probe for applying ultrasonic waves, the crystal characteristics of the oxide particles of the first material can be controlled and the degree of bonding with the second material particles can be controlled. Accordingly, if there is a specific crystal property required according to the specific use of the composite particle according to the present invention, the composite particle having the first oxide particle having the crystal structure required in this step can be obtained.

The frequency intensity of the ultrasonic waves may range from 10 3 to 10 8 Hz. If the frequency is less than 10 3 Hz, there may be a problem that the minimum disturbance frequency for controlling the crystal characteristic is insufficient. If the frequency is more than 10 8 Hz, the maximum disturbance energy for controlling the crystal characteristic may be exceeded.

According to an embodiment of the present invention, the diameter of a tip of a probe for applying an ultrasonic wave may be 0.06 to 6 times the diameter of the flame, and ultrasonic waves may be applied. At this time, an irradiation intensity, Probe tip area for power / ultrasonic application) may vary within a range of 0.02 to 2 kW / cm 2 to vary the size and crystal structure of the oxide particles of the first material. The size of the oxide particles and the crystal structure control can be more effectively performed in the tip diameter range or the ultrasonic wave application intensity range.

If necessary, the method may further comprise coating the composite particle with a biocompatible organic material in the present invention.

Examples of the biocompatible organic material include biocompatible polymers, and specific examples thereof include polyethylene glycol (PEG), but the present invention is not limited thereto.

The method of coating the composite particle with the biocompatible organic material is not particularly limited, and may be performed, for example, by spraying a fissile organic droplet on the composite particle.

As described above, the composite particles prepared according to the present invention can be used for industrial materials such as photocatalysts and solar cells, and can be coated with an organic material having biocompatibility such as PEG (polyethylene glycol) to improve biocompatibility, And medical materials for diagnosis.

It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to be illustrative of the invention and are not intended to limit the scope of the claims. It will be apparent to those skilled in the art that such variations and modifications are within the scope of the appended claims.

Example 1. Composite particles (Au / Fe 3 O 4 )

FeCl 2 was vaporized and then fed into a diffusion flame using argon. The diffusion flame was maintained by continuously injecting the oxygen mixed gas into the fuel using hydrogen supplied to the nozzle.

       Next, gold nanoparticles were produced through a low-temperature plasma particle generator while flowing 1 L / min of argon gas. At this time, the working conditions of the low temperature plasma particle generator having gold, resistance of 0.5 MΩ, electric capacity of 1.0 nF, load current of 2 mA, applied voltage of 3 kV and frequency of 667 Hz are provided.

In addition, the gold nanoparticles thus prepared were passed through the argon gas flow so as to continuously reach the diffusion flame, thereby preparing composite particles.

Then, ultrasonic waves were applied to the flame to control the crystal characteristics of the iron oxide particles and control the binding frequency in the course of forming the composite particles of the iron oxide particles and the gold nanoparticles. The ultrasonic wave was performed at an intensity of 750 W, and the probe for applying ultrasonic waves had a tip of 13 mm diameter and was positioned at the center of the flame in the flame direction.

The frequency of the ultrasonic waves was 2 x 10 4 Hz and the applied intensity was 0.34 kW / cm 2 .

Finally, composite particles (Au / Fe 3 O 4 ) were obtained, and a low-high-power TEM image of Au / Fe 3 O 4 is shown in FIG.

Example 2. Composite particles (Ag-TiO 2 Manufacture of @PEG

TiCl 4 was vaporized and then fed into a diffusion flame using argon. The diffusion flame was maintained by continuously injecting the oxygen mixed gas into the fuel using hydrogen supplied to the nozzle.

       Next, silver nanoparticles were produced through a low-temperature plasma particle generator while flowing 1 L / min argon gas. At this time, the operating conditions of the low-temperature plasma particle generator having the anode and the cathode material are silver, the resistance is 0.5 MΩ, the electric capacity is 1.0 nF, the load current is 2 mA, the applied voltage is 3 kV and the frequency is 667 Hz.

In addition, the prepared silver microparticles were allowed to reach the diffusion flame continuously in the argon gas flow, thereby preparing composite particles.

Ultrasonic waves were applied to the flame to control the crystal characteristics of the titanium dioxide particles and control the binding frequency in the course of forming the composite particles of the titanium dioxide particles and the silver microparticles. The ultrasonic wave was performed at an intensity of 750 W, and the probe for applying ultrasonic waves had a tip of 13 mm diameter and was positioned at the center of the flame in the flame direction. The frequency of the ultrasonic waves was 2 x 10 4 Hz and the applied intensity was 0.34 kW / cm 2 .

A composite particle (Ag-TiO 2 ) was obtained from the flame, followed by spraying with a flame (using a gas in which Ag-TiO 2 was present as a PEG spray working fluid) to impart bio- , Ag-TiO 2 @ PEG was obtained, and a photograph of Ag-TiO 2 @ PEG TEM was shown in FIG. 2 together with SEM photograph and EDX graph.

Claims (13)

Providing a precursor of the first material into the flame to obtain oxide particles of the first material;
Supplying a second material particle made through a low temperature plasma particle generator in an inert gas flow into the flame to obtain composite particles of the oxide particles of the first material and the second material particles; And
And applying ultrasonic waves to the composite particles in the flame to control the crystal structure of the oxide particles of the first material.
The method of claim 1, wherein the first material comprises at least one selected from the group consisting of a transition metal, a pre-metal, a non-metal, and a lanthanum source.
The method of claim 1, wherein the first material is injected into the flame in the form of a precursor gas or droplet.
The method of claim 1, wherein the second material particles are particles of a conductor or semiconductor.
The method of claim 1, wherein the flame is an inverse diffusion flame or a diffusion flame.
The method of claim 1, wherein the fuel of the flame is hydrogen or a hydrocarbon gas.
The method of claim 1, wherein the inert gas comprises at least one selected from the group consisting of nitrogen, argon, and helium.
The method of claim 1, wherein the supply of the second material particles into the flame is carried out by allowing the inert gas flow to reach the flame.
The method of claim 1, further comprising adding 5 vol% or less of oxygen to the inert gas stream for feeding the first material into the flame.
The method of claim 1, wherein the ultrasonic wave has a frequency of 10 3 to 10 8 Hz.
The method of claim 1, wherein the ultrasonic wave is performed with a probe for applying ultrasonic waves, and the tip diameter of the probe is 0.06 to 6 times the flame diameter.
The method of producing a composite particle according to claim 1, wherein the application intensity of the ultrasonic waves is 0.02 to 2 kW / cm 2 .
The method of claim 1, further comprising coating the composite particle with a biocompatible organic material.
KR1020160004096A 2016-01-13 2016-01-13 Composite particle and method for preparation thereof KR101814491B1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013220967A (en) * 2012-04-14 2013-10-28 Sumitomo Chemical Co Ltd Method for producing complex metal oxide
JP2015086413A (en) * 2013-10-29 2015-05-07 大陽日酸株式会社 Method of producing composite superfine particle

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013220967A (en) * 2012-04-14 2013-10-28 Sumitomo Chemical Co Ltd Method for producing complex metal oxide
JP2015086413A (en) * 2013-10-29 2015-05-07 大陽日酸株式会社 Method of producing composite superfine particle

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