WO2014142378A1 - Procédé de fabrication de nanoparticules magnétiques, et nanoparticules fabriquées à l'aide de ce dernier - Google Patents

Procédé de fabrication de nanoparticules magnétiques, et nanoparticules fabriquées à l'aide de ce dernier Download PDF

Info

Publication number
WO2014142378A1
WO2014142378A1 PCT/KR2013/002231 KR2013002231W WO2014142378A1 WO 2014142378 A1 WO2014142378 A1 WO 2014142378A1 KR 2013002231 W KR2013002231 W KR 2013002231W WO 2014142378 A1 WO2014142378 A1 WO 2014142378A1
Authority
WO
WIPO (PCT)
Prior art keywords
iron
iii
magnetic nanoparticles
solvent
cerium
Prior art date
Application number
PCT/KR2013/002231
Other languages
English (en)
Korean (ko)
Inventor
현재호
Original Assignee
고센바이오비드 주식회사
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 고센바이오비드 주식회사 filed Critical 고센바이오비드 주식회사
Priority to KR1020147017349A priority Critical patent/KR101516345B1/ko
Publication of WO2014142378A1 publication Critical patent/WO2014142378A1/fr

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
    • H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
    • H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant

Definitions

  • the present invention relates to a method for producing magnetic nanoparticles and to magnetic nanoparticles prepared using the same, and more particularly, to make nanoparticles have high stability and uniform particle distribution, and to induce synthesis and effective dispersion of nanoparticles,
  • the present invention relates to a method of manufacturing magnetic nanoparticles that can improve properties and facilitate mass production, and to magnetic nanoparticles prepared using the same.
  • Nanotechnology is not just an emerging technology due to the size of the object, but is one of the important technical fields because materials with sizes ranging from 1 to 1000 nm exhibit unique properties not found in materials with sizes larger than that. do.
  • the core of the reflective display is a display light transmission control device, and magnetic nanoparticles manufactured by nano technology are used in the display light transmission control device.
  • the display light transmission control device is an optical device that transmits or blocks the light emitted from the display device or the light incident from the outside, it is the magnetic nanoparticles to realize this.
  • the magnetic nanoparticles are raw materials such as bio-sensor for disease diagnosis, MRI contrast agents, hyperthermia, drug delivery systems, and the like, and can safely reduce side effects.
  • bio-sensor for disease diagnosis MRI contrast agents
  • hyperthermia hyperthermia
  • drug delivery systems and the like
  • magnetic nanoparticles must meet some requirements in order to be applied in bio and medical fields.
  • each of the magnetic nanoparticles generates a uniform magnetic field, and in order to exhibit more accurate and uniform characteristics, the magnetic nanoparticles should not aggregate with each other, and have a particle size and spherical particle shape that may have superparamagnetism. It is important to do so.
  • the magnetic nanoparticles in order for the magnetic nanoparticles to respond to external application or minute changes in the induced magnetic field, the magnetic nanoparticles must have improved saturation magnetization value and high susceptibility, and have high chemical stability.
  • the magnetic properties should be designed so as to maintain magnetic properties when the surface of the magnetic nanoparticles having affinity with a living cell or coated with a biocompatible material. That is, the nanoparticles must meet both the magnetic properties and biocompatibility to be finally applied to the bio and medical fields.
  • magnetite magnetite
  • ⁇ -Fe2O3 maghemite
  • VSM vibration susceptibility meter
  • SQUID superconducting quantum interference magnetic measurement device
  • the magnetic nanoparticles to have a high stability and uniform particle distribution and at the same time to improve the magnetic properties, it can be easily applied to the reflective display or bio fields
  • the purpose of the present invention is to provide a method for manufacturing magnetic nanoparticles and magnetic nanoparticles prepared using the same.
  • the surface of the magnetic nanoparticles can be easily modified, and particles of various sizes can be easily manufactured, so that the magnetic nanoparticles can be easily applied to various applications as well as reflective displays or biofields.
  • FIG. 1 is a flow chart showing one embodiment of the method of manufacturing magnetic nanoparticles of the present invention
  • Figure 2 is a flow chart showing another embodiment of the method of manufacturing magnetic nanoparticles of the present invention.
  • the iron precursor, the solvent, the ligand, and the tertiary distilled water are mixed at room temperature to proceed with the mixing step (S1) where the basic reaction is performed, and to increase the dispersibility in the solution mixed in the mixing step (S1).
  • the solution mixed in the dispersion step (S2) to 150 ⁇ 300 °C to continue the reaction for a predetermined time while the color of the solution from yellow to black
  • the change step (S3) to identify the change to
  • the separation step (S4) to separate the magnetic nanoparticles by using a centrifugal separator or a magnetic solution in the change step (S3) to sequentially
  • the magnetic nanoparticles to be obtained by the present invention are prepared.
  • the iron precursor, the solvent, the ligand, the tertiary distilled water, and the polymer material are mixed and heated to 150 to 300 ° C. to maintain the reaction for a predetermined time while changing the color of the solution from yellow to black.
  • step (S10) even if the solution is changed to black in the mixing change step (S10) using a centrifuge or a magnetic separation step (S4) to separate the magnetic nanoparticles in sequence, the magnetic properties are Improved magnetic nanoparticles can be prepared.
  • the normal temperature means, but is not limited to, 20 to 30 °C that the operator can react most comfortably without raising or lowering the temperature in the present invention. That is, the temperature may be lower or higher depending on the surrounding conditions and environment.
  • the iron precursor, the solvent, the ligand, and the third distilled water are mixed at room temperature to perform a basic reaction.
  • the iron precursor is iron (II), iron (III), iron nitrate (II) [Fe (NO3) 2], iron nitrate hexahydrate as an additive material containing iron capable of obtaining magnetism in order to obtain magnetic nanoparticles.
  • the solvent is an additive material for dissolving the iron precursor to liquefy, and may include a polymer solvent, an ionic liquid solvent, a halogen hydrocarbon solvent, an alcohol solvent, an aromatic solvent, a heterocyclic solvent, a sulfoxide solvent, an amide solvent, a hydrocarbon solvent, It consists of either an ether solvent or water.
  • the solvent is acetate, ethyl acetate, butyl acetate, ethylene glycol, ethylene glycol, diethylene glycol, triethylene glycol, Tetra ethylene glycol, ethanol, 2-butoxy ethanol, di propylene glycol, ketone, methyl isobutyl ketone , Ethyl methyl ketone, acetone, alcohol, alcohol, butanol, propanol, methanol, acetonitrile, acetonitrile, acetonitrile, chloroform (chloroform), ether, diethylehter, phenyl ether, octyl ether, decyl ether, benzyl ether, pyridine, die Methyl sulfoxide, N, N-di N, N-Dimethylformamide, Squalene, Tetrahydrofuran, Dichloromethane, Amine, Hexane, Hexadecane, Hexade
  • the ligand is a substance added to the base reaction with the iron precursor, sodium acetate, ammonia water, ammonium hydroxide, sodium hexane sulfonate, sodium bicarbonate, sodium alginate, phosphine, diphosphine, triphenylphosphine, tri-o -Tolylphosphine, tri-m-tolylphosphine, tri-p-tolylphosphine, tris (pentafluorophenyl) phosphine, tris (p-fluorophenyl) phosphine, tris (o-methoxyphenyl) Phosphine, tris (m-methoxyphenyl) phosphine, tris (p-methoxyphenyl) phosphine, tris (2,4,6-trimethoxyphenyl) phosphine, tri (m-chlorophenyl) phosphine , Tri (p-chlorophenyl
  • the tertiary distilled water is added to adjust the size of the prepared magnetic nanoparticles to be a mixture having a desired viscosity, and the water having a pH and a conductivity value of 18.2 megaohms through the ultrafilter. use.
  • the iron precursor and the ligand are added at a ratio of 1: 0.1 to 1: 100, preferably at a ratio of 1: 1 to 1:10, and the solvent is preferably added to 10 to 100,000mL. .
  • the third distilled water it is preferable to add 10 to 50,000mL bar, since the size of the finally prepared magnetic nanoparticles can be adjusted according to the amount of the third distilled water, according to the size of the predetermined magnetic nanoparticles 3 It controls the amount of secondary distilled water and easily prepares magnetic nanoparticles of various sizes.
  • the dispersing step (S2) is a step of making a mixture containing the nanoparticles dispersed therein by increasing the dispersibility by adding a polymer material to the mixture is mixed in the mixing step (S1) and the base reaction is made, the polymer material As the polyvinyl pyrrolidone (PVP (polyvinyl pyrrolidone)) is used.
  • PVP polyvinyl pyrrolidone
  • the iron precursor and the polymer material are added at a ratio of 1: 0.01 to 1:20, but preferably at a ratio of 1: 0.1 to 1: 5.
  • the polyvinyl pyrrolidone [PVP (polyvinyl pyrrolidone)]
  • the molecular weight is 55K and uses a molecular weight of 1,000 to 1,500,000, polyvinyl pyrrolidone [PVP (polyvinyl) having an appropriate molecular weight according to the mol concentration of the mixture pyrrolidone)].
  • polymer material polyvinyl pyrrolidone [PVP (Polyvinyl Pyrrolidone)], alginic acid (Alginic Acid), chitosan (Chitosan), carboxy methyl cellulose [CMC (Carboxy Methyl Cellulose)], acrylamide (Acrylamide) alone And copolymers, polyacrylic acid [PAA (Polyacrylic Acid)], polyethylene oxide, polyvinyl alcohol, polyvinyl alcohol-polyvinyl acetate copolymer, poly (N-vinylpyrrolidone), Polyhydroxyethylacrylate, polyaspartic acid [PAA (Poly Aspartic Acid)], carbomer, polyalkylene glycol [PAG (Poly Alkylen Glycol)], polyethylene glycol [PEG (Polyethylen Glycol)], polyalkyl Ethylene oxide [PAO (Polyalkylene oxides)], polyoxyethylene [
  • the molecular weight is limited to 1,000 to 1,500,000 as described above, but is not limited thereto.
  • the higher the molecular weight the higher the dispersibility, but the use of a polymer material having a molecular weight that is too high compared to the mol concentration may result in adverse effects. It is preferable to use a polymer material having the same molecular weight between 1,000 and 1,500,000.
  • the changing step (S3) after heating the mixture to increase the dispersion force through the dispersing step (S2) to 150 ⁇ 300 °C using a heating mantle, watching the reaction for a predetermined time while the heated mixture color is yellow It is a step to visually identify whether the color is changed from black to black.
  • the preset time is preferably about 1 to 24 hours, and may be 48 to 72 hours depending on other requirements.
  • the heating of the mixture is to heat the solvent to the boiling point to allow the mixture to react.
  • the nanoparticles dispersed in the dispersion step (S2) is reacted by heat and magnetized (magnetite).
  • the magnetization means that the nanoparticles are magnetic, so that the color of the heated mixture is changed from the first yellow to black.
  • the separation step (S4) is a step of separating magnetic nanoparticles having magnetic properties from the mixture by using a centrifuge or magnetic in the mixture that has undergone the change step (S3).
  • the method for separating the magnetic nanoparticles using the centrifuge or the magnetic may be any one of methods that are commonly used, and a detailed description thereof will be omitted.
  • the washing step (S5) by removing the impurities by washing the magnetic nanoparticles separated in the separation step (S4) with a polar solvent, the magnetic nanoparticles have a high stability and uniform particle distribution.
  • the polar solvent is to use ethanol.
  • the polar solvent may be any one of ethanol, alcohol, liquid ammonia, acetone, methanol, chloroform, ethyl acetate, ether, tetrahydrofuran, potassium hydroxide, sodium hydroxide, dichloromethane and water.
  • washing step (S5) it is preferable to wash three times with a polar solvent.
  • the washing is not limited to three washings, but the washing may be performed once to several times, and all simple modifications to the number of washings will fall within the scope of the present invention.
  • the magnetic nanoparticles may be prepared in a state in which the washing step (S5) is not performed, it is preferable to proceed with the washing step (S5) to have a high stability and uniform particle distribution as described above.
  • the method of washing the magnetic nanoparticles may be any one of methods that are commonly used, a detailed description thereof will be omitted.
  • the washing step (S5) may proceed to the method using a centrifuge which is one of the conventional methods, the separation of the magnetic nanoparticles in the separation step (S4) to complete the washing is within the scope of the present invention. something to do. This is because the separation step (S4) proceeds by dividing into primary, secondary, etc. and proceeds with the separation and washing together.
  • the separation step (S4) and washing step ( S5) may be prepared to produce magnetic nanoparticles (see FIG. 2).
  • the iron precursor, the solvent, the ligand, the tertiary distilled water, and the polymer material are mixed, and the mixture is heated to 150 to 300 ° C. using a heating mantle to maintain the reaction for a predetermined time while the color of the solution is yellow to black. Proceed with the mixed change step (S10) to visually identify the change to.
  • the preset time is preferably about 1 to 24 hours, and may be 48 to 72 hours depending on other requirements.
  • the magnetic nanoparticles may be manufactured by performing the separation step (S4) and the washing step (S5).
  • the magnetic nanoparticles may be manufactured without performing the washing step (S5).
  • the washing step (S5) may be performed to have a high stability and a uniform particle distribution as described above. desirable.
  • Magnetic nanoparticles prepared as described above, the diameter of the center is 1 ⁇ 1,000nm, has a superparamagnetic, paramagnetic, diamagnetic, ferromagnetic, antiferromagnetic, ferrimagnetic and hydrophilic, reflective display and bio and various applications It can be easily applied and used.
  • the superparamagnetism can be controlled by using a magnetic force and can be redispersed when the magnetic force is lost, and thus can be used in various fields requiring magnetic nanoparticles having the superparamagnetism.
  • hydrophilic property can be used in the field of biotechnology that requires magnetic nanoparticles having hydrophilic properties by dissolving in water.
  • reaction was carried out for 3 hours after raising the temperature to 220 °C while maintaining the stirring. At this time, it was confirmed that the color of the solution was changed from yellow to black, and that the change was completely black, the reaction was completed by the heat and the magnetite was changed (S3).
  • the magnetic nanoparticles and the solution were separated using a centrifuge (S4), and the separated magnetic nanoparticles were washed three times with ethanol, a polar solvent (S5), to provide high stability and uniform particle distribution. Magnetic nanoparticles having improved magnetic properties.
  • reaction was carried out for 3 hours after raising the temperature to 220 °C while maintaining the stirring. At this time, it was confirmed that the color of the solution was changed from yellow to black, and that the change was completely black, the reaction was completed by the heat and the magnetite was changed (S3).
  • the magnetic nanoparticles and the solution were separated using a centrifuge (S4), and the separated magnetic nanoparticles were washed three times with ethanol (S5) to have high stability and uniform particle distribution and magnetic properties. Magnetic nanoparticles with improved properties were prepared.
  • reaction was carried out for 3 hours after raising the temperature to 220 °C while maintaining the stirring. At this time, it was confirmed that the color of the solution was changed from yellow to black, and that the change was completely black, the reaction was completed by the heat and the magnetite was changed (S3).
  • the magnetic nanoparticles and the solution were separated using a centrifuge (S4), and the separated magnetic nanoparticles were washed three times with ethanol (S5) to have high stability and uniform particle distribution and magnetic properties. Magnetic nanoparticles with improved properties were prepared.
  • reaction was carried out for 3 hours after raising the temperature to 220 °C while maintaining the stirring. At this time, it was confirmed that the color of the solution was changed from yellow to black, and that the change was completely black, the reaction was completed by the heat and the magnetite was changed (S3).
  • the magnetic nanoparticles and the solution were separated using a centrifuge (S4), and the separated magnetic nanoparticles were washed three times with ethanol (S5) to have high stability and uniform particle distribution and magnetic properties. Magnetic nanoparticles with improved properties were prepared.
  • the method of manufacturing the magnetic nanoparticles of the present invention and the magnetic nanoparticles prepared by using the same cause a basic reaction by mixing an iron precursor, a solvent, a ligand, and tertiary distilled water, increase the dispersibility by mixing a polymer material, and then heat and magnetize the magnetic nanoparticles.
  • a basic reaction by mixing an iron precursor, a solvent, a ligand, and tertiary distilled water
  • increase the dispersibility by mixing a polymer material and then heat and magnetize the magnetic nanoparticles.
  • By separating the particles it is possible to produce magnetic nanoparticles having high stability and uniform particle distribution and improved magnetic properties.
  • FIG. 1 is a flow chart showing an embodiment of the present invention method for manufacturing magnetic nanoparticles
  • Figure 2 is a flow chart showing another embodiment of the method of manufacturing magnetic nanoparticles of the present invention.
  • the present invention provides a method for preparing magnetic nanoparticles, a mixing step of mixing an iron precursor, a solvent, a ligand, and tertiary distilled water at room temperature for a basic reaction; And, in the solution mixed in the mixing step, the dispersion step of mixing the polymer material to increase the dispersion force; And, changing the step of identifying that the color of the solution is changed from yellow to black while continuing the reaction for a predetermined time by heating the solution mixed in the dispersion step to 150 ⁇ 300 °C; And a separation step of separating the magnetic nanoparticles using a centrifugal separator or a magnet from the solution changed to black in the changing step. Characterized in that comprises a.
  • the washing step of washing the magnetic nanoparticles separated in the separation step with a polar solvent It is preferable that further comprises.
  • the polar solvent is made of any one of ethanol, alcohol, liquid ammonia, acetone, methanol, chloroform, ethyl acetate, ether, tetrahydrofuran, potassium hydroxide, sodium hydroxide, dichloromethane and water.
  • the iron precursor is iron (II), iron (III), iron nitrate (II), iron nitrate hexahydrate (II), iron nitrate (III), iron nitrate hexahydrate (III), iron sulfate (II), sulfuric acid Iron lactate (II), iron sulfate (III), iron chloride (II), iron chloride tetrahydrate (II), iron chloride (III), iron chloride hexahydrate, iron iodide (II), iron iodide tetrahydrate (II), iron iodide ( III), iron (II) acetylacetonate iron, iron (III) acetylacetonate iron, iron (II) trifluoroacetylacetonate, iron (III) trifluoroacetylacetonate, iron (II) acetate, iron (III) acetate, iron perchlorate, iron sulfamate, iron pentacarbonyl
  • the solvent may be any one of a polymer solvent, an ionic liquid solvent, a halogen hydrocarbon solvent, an alcohol solvent, an aromatic solvent, a heterocyclic solvent, a sulfoxide solvent, an amide solvent, a hydrocarbon solvent, an ether solvent, and water. Is done.
  • the solvent is acetate, ethyl acetate, butyl acetate, ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, ethanol, 2-butoxy ethanol, dipropylene glycol, ketone, methyl isobutyl ketone, ethyl methyl Ketones, acetone, alcohols, butanol, propanol, methanol, acetonitrile, acetonitrile, chloroform, ether, diethyl ether, phenyl ether, octyl ether, decyl ether, benzyl ether, pyridine, dimethyl sulfoxide, N, N Any of dimethylformamide, squalene, tetrahydrofuran, dichloromethane, amine, hexane, hexadecane, hexadecene, octadecane, octadecen
  • the ligand is sodium acetate, ammonia water, ammonium hydroxide, sodium hexane sulfonate, sodium bicarbonate, sodium alginate, phosphine, diphosphine, triphenylphosphine, tri-o-tolylphosphine, tri-m-tolylphosphine, Tri-p-tolylphosphine, tris (pentafluorophenyl) phosphine, tris (p-fluorophenyl) phosphine, tris (o-methoxyphenyl) phosphine, tris (m-methoxyphenyl) phosphine , Tris (p-methoxyphenyl) phosphine, tris (2,4,6-trimethoxyphenyl) phosphine, tri (m-chlorophenyl) phosphine, tri (p-chlorophenyl) phosphine, tri (p-chlor
  • the polymer material may be polyvinyl pyrrolidone, alginic acid, chitosan, carboxymethyl cellulose, homopolymer and copolymer of acrylamide, polyacrylic acid, polyethylene oxide, polyvinyl alcohol, polyvinyl alcohol-polyvinyl acetate copolymer, Poly (N-vinylpyrrolidone), polyhydroxyethylacrylate, polyaspartic acid, carbomer, polyalkylene glycol, polyethylene glycol, polyalkylene oxide, polyoxyethylene, gelatin, carboxyl group-containing monomer unit, sulfonic acid It consists of either a group containing monomer unit and a phosphoric acid group containing monomer unit.
  • the polymer material it is preferable to use a polymer of 1,000 to 1,500,000 in order to increase the initial dispersion.
  • the iron precursor and the ligand are added at a ratio of 1: 0.1 to 1: 100, and the iron precursor and the polymer are added at a ratio of 1: 0.01 to 1:20.
  • the tertiary distilled water may adjust the amount of mixing to control the size of the magnetic nanoparticles.
  • the magnetic nanoparticles of the present invention the iron precursor, the solvent, the ligand, the tertiary distilled water by mixing at room temperature mixing step of the base reaction; And, in the solution mixed in the mixing step, the dispersion step of mixing the polymer material to increase the dispersion force; And, changing the step of identifying that the color of the solution is changed from yellow to black while continuing the reaction for a predetermined time by heating the solution mixed in the dispersion step to 150 ⁇ 300 °C; And a separation step of separating the magnetic nanoparticles using a centrifugal separator or a magnet from the solution changed to black in the changing step.
  • the magnetic nanoparticles preferably have a central diameter of 1 to 1,000 nm and have superparamagnetic, paramagnetic, diamagnetic, ferromagnetic, antiferromagnetic and ferrimagnetic properties and hydrophilicity dispersed in a polar solvent.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biomedical Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Power Engineering (AREA)
  • Compounds Of Iron (AREA)
  • Hard Magnetic Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

La présente invention porte sur un procédé pour fabriquer des nanoparticules magnétiques et sur des nanoparticules fabriquées à l'aide de ce dernier. La présente invention est caractérisée en ce qu'elle comprend : une étape de mélange consistant à mélanger un précurseur de fer, un solvant, un liant et de l'eau distillée tertiaire à température ambiante, et suivie d'une réaction de base ; une étape de dispersion consistant à ajouter une matière polymère destinée à renforcer la force de dispersion dans la solution mélangée dans l'étape de mélange, et suivie d'un mélange ; une étape de changement consistant, tout en chauffant la solution mélangée dans l'étape de dispersion à 150-300 °C et en maintenant une réaction pendant un temps prédéterminé, à identifier le changement de couleur, du jaune au noir, de la solution ; et une étape de séparation consistant à séparer les nanoparticules magnétiques de la solution, dont la couleur est passée au noir dans l'étape de changement, à l'aide d'une centrifugeuse ou d'un magnétisme. En outre, la présente invention est caractérisée par des nanoparticules magnétiques fabriquées par le procédé. De cette façon, la présente invention a pour effet de fabriquer des nanoparticules magnétiques ayant une haute stabilité, une répartition de particule uniforme et des caractéristiques magnétiques améliorées, par mélange du précurseur de fer, du solvant, du liant et de l'eau distillée tertiaire à température ambiante pour entraîner une réaction de base, par mélange de la matière polymère avec celui-ci pour améliorer la force de dispersion, par exécution d'un chauffage pour assurer la magnétisation, puis par séparation des nanoparticules magnétiques.
PCT/KR2013/002231 2013-03-14 2013-03-19 Procédé de fabrication de nanoparticules magnétiques, et nanoparticules fabriquées à l'aide de ce dernier WO2014142378A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020147017349A KR101516345B1 (ko) 2013-03-14 2013-03-19 자성나노입자 제조방법 및 이를 이용해 제조된 자성나노입자

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR20130027614 2013-03-15
KR10-2013-0027614 2013-03-15

Publications (1)

Publication Number Publication Date
WO2014142378A1 true WO2014142378A1 (fr) 2014-09-18

Family

ID=51537018

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2013/002231 WO2014142378A1 (fr) 2013-03-14 2013-03-19 Procédé de fabrication de nanoparticules magnétiques, et nanoparticules fabriquées à l'aide de ce dernier

Country Status (2)

Country Link
KR (1) KR101516345B1 (fr)
WO (1) WO2014142378A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104342430A (zh) * 2014-09-30 2015-02-11 嘉兴学院 一种负载离子液体中空液芯微囊化细胞及其应用
CN110624519A (zh) * 2019-10-16 2019-12-31 刘勇 一种磁性强、疏水性高的壳聚糖-硬脂酸复合吸油材料
CN110787831A (zh) * 2019-11-15 2020-02-14 南宁师范大学 双孔氮化碳复合磁性光催化剂的制备方法
CN113558217A (zh) * 2021-08-24 2021-10-29 温州快鹿集团公司 一种味精的精制工艺
CN114100536A (zh) * 2021-11-26 2022-03-01 珠海市钯金电子科技有限公司 一种复合微球颗粒及使用该颗粒的电路板沉镍钯金方法
CN114854054A (zh) * 2022-04-02 2022-08-05 阜阳德润磁材科技有限公司 磁颗粒制备工艺
CN116698671A (zh) * 2023-06-05 2023-09-05 南京工业大学 一种磁纳米毛刷及其制备方法
CN116984623A (zh) * 2023-09-26 2023-11-03 之江实验室 一种基于分段式水热法的二维铋纳米晶体合成方法

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101686339B1 (ko) * 2015-07-21 2016-12-13 건양대학교산학협력단 열분해법을 이용한 자성나노입자의 제조방법
KR101729687B1 (ko) * 2016-08-19 2017-05-22 주식회사 아모라이프사이언스 초상자성 나노복합체의 제조방법 및 이를 이용하여 제조된 초상자성 나노복합체
KR101990215B1 (ko) * 2017-12-12 2019-06-17 고려대학교 산학협력단 균일하게 실리카 코팅된 자성 마이크로 입자의 합성 및 이의 올레핀 산화반응을 위한 불균일상 촉매로의 응용
KR101989385B1 (ko) * 2017-12-22 2019-06-14 한국세라믹기술원 막대형 페라이트 자성입자 제조방법
KR102430475B1 (ko) * 2019-01-18 2022-08-08 주식회사 오트로닉 페라이트 소결 자석의 제조 방법 및 페라이트 소결 자석
KR102610891B1 (ko) * 2019-10-24 2023-12-06 주식회사 오트로닉 페라이트 소결 자석의 제조 방법
KR102634542B1 (ko) * 2021-06-15 2024-02-07 전남대학교 산학협력단 표면개질된 자성나노입자 제조 방법 및 이로부터 제조된 표면개질된 자성나노입자

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060099740A (ko) * 2005-03-14 2006-09-20 한국화학연구원 수용성 산화철 나노 입자 및 이의 제조방법
KR100684629B1 (ko) * 2006-01-27 2007-02-22 요업기술원 마그네타이트 나노 분말의 제조방법
KR20090026093A (ko) * 2007-09-06 2009-03-11 애니젠 주식회사 조영 및 약물운반용 다기능 복합체
KR20110123988A (ko) * 2010-05-10 2011-11-16 연세대학교 산학협력단 자성 나노입자를 포함하는 복합체 및 그 제조 방법
KR20120020861A (ko) * 2010-08-31 2012-03-08 한화케미칼 주식회사 산화철 나노캡슐, 이의 제조방법 및 이를 포함하는 자기공명영상진단 조영제

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060099740A (ko) * 2005-03-14 2006-09-20 한국화학연구원 수용성 산화철 나노 입자 및 이의 제조방법
KR100684629B1 (ko) * 2006-01-27 2007-02-22 요업기술원 마그네타이트 나노 분말의 제조방법
KR20090026093A (ko) * 2007-09-06 2009-03-11 애니젠 주식회사 조영 및 약물운반용 다기능 복합체
KR20110123988A (ko) * 2010-05-10 2011-11-16 연세대학교 산학협력단 자성 나노입자를 포함하는 복합체 및 그 제조 방법
KR20120020861A (ko) * 2010-08-31 2012-03-08 한화케미칼 주식회사 산화철 나노캡슐, 이의 제조방법 및 이를 포함하는 자기공명영상진단 조영제

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104342430A (zh) * 2014-09-30 2015-02-11 嘉兴学院 一种负载离子液体中空液芯微囊化细胞及其应用
CN110624519A (zh) * 2019-10-16 2019-12-31 刘勇 一种磁性强、疏水性高的壳聚糖-硬脂酸复合吸油材料
CN110624519B (zh) * 2019-10-16 2022-11-22 盐城神华机械制造有限公司 一种磁性强、疏水性高的壳聚糖-硬脂酸复合吸油材料
CN110787831A (zh) * 2019-11-15 2020-02-14 南宁师范大学 双孔氮化碳复合磁性光催化剂的制备方法
CN113558217A (zh) * 2021-08-24 2021-10-29 温州快鹿集团公司 一种味精的精制工艺
CN114100536A (zh) * 2021-11-26 2022-03-01 珠海市钯金电子科技有限公司 一种复合微球颗粒及使用该颗粒的电路板沉镍钯金方法
CN114854054A (zh) * 2022-04-02 2022-08-05 阜阳德润磁材科技有限公司 磁颗粒制备工艺
CN116698671A (zh) * 2023-06-05 2023-09-05 南京工业大学 一种磁纳米毛刷及其制备方法
CN116698671B (zh) * 2023-06-05 2023-11-21 南京工业大学 一种磁纳米毛刷及其制备方法
CN116984623A (zh) * 2023-09-26 2023-11-03 之江实验室 一种基于分段式水热法的二维铋纳米晶体合成方法
CN116984623B (zh) * 2023-09-26 2024-02-09 之江实验室 一种基于分段式水热法的二维铋纳米晶体合成方法

Also Published As

Publication number Publication date
KR20140122223A (ko) 2014-10-17
KR101516345B1 (ko) 2015-05-04

Similar Documents

Publication Publication Date Title
WO2014142378A1 (fr) Procédé de fabrication de nanoparticules magnétiques, et nanoparticules fabriquées à l'aide de ce dernier
Wang et al. Synthesis and characterization of a novel magnetic carrier with its composition of Fe3O4/carbon using hydrothermal reaction
Caruntu et al. Reactivity of 3d transition metal cations in diethylene glycol solutions. Synthesis of transition metal ferrites with the structure of discrete nanoparticles complexed with long-chain carboxylate anions
Esmaeili et al. Modified single-phase hematite nanoparticles via a facile approach for large-scale synthesis
Fontaíña-Troitiño et al. Room-temperature ferromagnetism in antiferromagnetic cobalt oxide nanooctahedra
Sangregorio et al. A new method for the synthesis of magnetoliposomes
Ma et al. Electrospinning fabrication of high-performance magnetic@ photoluminescent bifunctional coaxial nanocables
Zhou et al. Coating and structural locking of dipolar chains of cobalt nanoparticles
WO2010067951A1 (fr) Nanoparticules de ferrite hexaédrique ou octaédrique régulières et procédé de production de celles-ci
CN111155197B (zh) 一种磁性纤维材料及其制备方法和应用
Wang et al. Preparation and characterization of magnetic hollow PMMA nanospheres via in situ emulsion polymerization
WO2015182840A1 (fr) Procédé de préparation de nanoparticules d'oxyde de fer monodispersées au moyen d'un homogénéisateur à ultra haute pression et nanoparticules d'oxyde de fer monodispersées préparées par ce procédé
CN102134762B (zh) 一种聚乙烯吡咯烷酮/Fe3O4复合纤维的制备方法
CN102391603A (zh) 一种新型磁性高分子水凝胶的制备方法
CN102010190A (zh) 一维棒状尖晶石铁氧体制备方法
Rittikulsittichai et al. Preparation, characterization, and utilization of multi-functional magnetic-fluorescent composites for bio-imaging and magnetic hyperthermia therapy
Xu et al. Synthesis of raspberry-like magnetic polystyrene microspheres
CN109399727B (zh) 含金属原子簇的磁性氧化铁纳米颗粒及其制备和应用
Zhan et al. Superparamagnetic polyimide/γ-Fe2O3 nanocomposite films: preparation and characterization
KR20090033940A (ko) 중금속 흡착제를 위한 자성 나노입자/고분자 코어-셀구조의 나노복합체의 제조
Kumar et al. One-step synthesis of superparamagnetic Fe 3 O 4@ PANI nanocomposites
Roskov et al. Magnetic field-induced alignment of nanoparticles in electrospun microfibers
Ali et al. Size and shape control synthesis of iron oxide–based nanoparticles: current status and future possibility
CN109735962B (zh) 一种原位制备四氧化三铁磁性纳米纤维的方法
Yao et al. Synthesis and self‐assembly of multiple‐responsive magnetic nanogels

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 20147017349

Country of ref document: KR

Kind code of ref document: A

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 13877784

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 13877784

Country of ref document: EP

Kind code of ref document: A1