WO2010067951A1 - 정육면체 또는 팔면체 모양의 페라이트 나노입자 및 그 제조 방법 - Google Patents
정육면체 또는 팔면체 모양의 페라이트 나노입자 및 그 제조 방법 Download PDFInfo
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Definitions
- the present invention relates to a cube or octahedral ferrite nanoparticles and a method for producing the same. More specifically, the present invention relates to a method for preparing ferrite nanocube comprising heating a mixture of superparamagnetic or ferrimagnetic ferrite nanocubes or octahedral ferrite nanoparticles and a metal precursor, surfactant and solvent. .
- Ferrite is a solid solution composed mainly of iron or iron, and has a body centered cubic crystal structure.
- Magnetite Fe 3 O 4
- Magnetite is a ferrimagnetic mineral and is one of several kinds of iron oxides belonging to the spinel group. Magnetite has the largest magnetism among the naturally occurring minerals on Earth, and has been used to make tools such as compasses since ancient times. Traditionally, it has been manufactured by the Massart method in which iron (II) chloride (FeCl 2 ) and iron (III) chloride (FeCl 3 ) are added to an aqueous solution of sodium hydroxide (NaOH). The disadvantage is that it is nonuniform.
- the wustite nanoparticles having the composition of FeO have weak magnetic properties and are not chemically stable because they are antiferromagnetic at room temperature.
- iron (II) acetylacetonate iron (II) acetylacetonate
- oleic acid oleic acid
- oleyl amine oleylamine
- 1,2- dimethyl-hexadecane Disclosed is a method for synthesizing spherical magnetite (Fe 3 O 4 ) nanoparticles by pyrolysis in a mixed solution of 1,2-hexadecanediol and benzyl ether.
- magnetite nanoparticles such as lines are spherical and less than 10 nm in size, they exhibit superparamagnetic and weak magnetic properties at room temperature. Spherical nanoparticles are also difficult to make cubic-shaped arrays.
- the magnetic direction is easily changed by temperature, so the magnetic direction of the individual particles cannot be maintained in a specific direction at room temperature.
- the nanoparticles having ferrimagnetic properties have higher energy required to change the magnetic direction than the thermal energy at room temperature, so that the magnetic direction of the individual particles maintains a specific direction at room temperature.
- the basic object of the present invention is to provide a ferrite nanocube exhibiting superparamagnetic or ferrimagnetic.
- Still another object of the present invention is to provide a cubic array including ferrite nanocubes exhibiting ferrimagnetic.
- Still another object of the present invention is to provide a cube-shaped ferrite nanoparticle having a truncated octahedron or a vertex.
- the basic object of the present invention described above can be achieved by providing a ferrite nanocube exhibiting superparamagnetic or ferrimagnetic.
- nanocube refers to a cube-shaped nanometer-sized particles.
- the ferrite may be magnetite (Fe 3 O 4 ), bimetallic ferrite or magnetite doped with metal.
- the dimetallic ferrite may be CoFe 2 O 4 , MnFe 2 O 4 , NiFe 2 O 4 , ZnFe 2 O 4 or BaFe 12 O 19 , the magnetite doped with the metal is Co, Mn, Ni, Zn or Ba may be doped magnetite.
- the size of the ferrite nanocube of the present invention is preferably 10 nm to 200 nm.
- Another object of the present invention described above can be achieved by providing a cubic array including a ferrite nanocube exhibiting ferrimagnetic.
- cubic array refers to a three-dimensional stack of the magnetite nanoparticles of the present invention. Such regular arrangement of nanoparticles may facilitate access to individual nanoparticles, and thus may help to improve performance of magnetic storage devices and sensors.
- Ferrite constituting the cubic array of the present invention may be a magnetite (magnetite, Fe 3 O 4 ), bimetallic ferrite (magnetite) or a metal doped magnetite.
- the dimetallic ferrite may be CoFe 2 O 4 , MnFe 2 O 4 , NiFe 2 O 4 , ZnFe 2 O 4 or BaFe 12 O 19
- the magnetite doped with the metal is Co, Mn, Ni, Zn or Ba may be doped magnetite.
- Still another object of the present invention described above can be achieved by providing a ferrite nanoparticle having an octahedron having a ferrimagnetic shape or a cube having a truncated vertex.
- Octahedral-shaped nanoparticles unlike spherical nanoparticles that are symmetrical in all directions, can exhibit large magnetism in a specific direction, thus giving them more freedom in measuring and using magnetic properties of nanoparticles. have.
- the iron atoms present at the corners of the octahedron may have a difference in reactivity since the surface energy is higher than that of the iron atoms on the spherical surface.
- the cube-shaped ferrite nanoparticles in which the octahedron or the vertex are cut off are magnetite (magnetite, Fe 3 O 4 ), bimetallic ferrite, or metal-doped magnetite nanoparticles.
- the dimetallic ferrite may be CoFe 2 O 4 , MnFe 2 O 4 , NiFe 2 O 4 , ZnFe 2 O 4 or BaFe 12 O 19
- the magnetite doped with the metal is Co, Mn, Ni, Zn or Ba may be doped magnetite.
- the size of the cube-shaped ferrite nanoparticles in which the octahedron or the vertex of the present invention is cut is 10 nm to 200 nm.
- Another object of the present invention as described above can be achieved by providing a method for producing a ferrite nanocube comprising heating a mixture of a metal precursor, a surfactant and a solvent.
- the magnetite nanocube can be manufactured.
- the iron precursor is preferably iron nitrate (II) (Fe (NO 3 ) 2 ), iron nitrate (III) (Fe (NO 3 ) 3 ), iron sulfate (II) (FeSO 4 ), iron sulfate (III) ) (Fe 2 (SO 4 ) 3 ), iron (II) acetylacetonate (Fe (acac) 2 ), iron (III) acetylacetonate (Fe (acac) 3 ), iron (II) trifluoroacetylaceto Nate (Fe (tfac) 2 ), iron (III) trifluoroacetylacetonate (Fe (tfac) 3 ), iron (II) acetate (Fe (ac) 2 ), iron (III) acetate (Fe (ac)) 3 ), iron (II) chloride
- CoFe 2 O 4 , MnFe 2 O 4 , NiFe 2 O Bimetallic ferrite nanocubes such as 4 , ZnFe 2 O 4 or BaFe 12 O 19 can be prepared.
- the cobalt precursors are cobalt (II) nitrate (Co (NO 3 ) 2 ), cobalt sulfate (II) (CoSO 4 ), cobalt (II) acetylacetonate (Co (acac) 2 ), cobalt (II) trifluoro Roacetylacetonate (Co (tfac) 2 ), cobalt (II) acetate (Co (ac) 2 ), cobalt chloride (II) (CoCl 2 ), cobalt bromide (II) (CoBr 2 ), cobalt iodide (II) (CoI 2 ), cobalt sulfamate (Co (NH 2 SO 3 ) 2 ), cobalt stearate (II) ((CH 3 (CH 2 ) 16 COO) 2 Co), cobalt oleate (II) ((CH 3 ( CH 2 ) 7 CHCH (CH 2 ) 7 COO) 2 Co),
- the manganese precursors are manganese nitrate (II) (Mn (NO 3 ) 2 ), manganese carbonate (II) (MnCO 3 ) manganese nitrate (III) (Mn (NO 3 ) 3 ), manganese sulfate (II) (MnSO 4 ) , Manganese sulfate (III) (Mn 2 (SO 4 ) 3 ), manganese (II) acetylacetonate (Mn (acac) 2 ), manganese (III) acetylacetonate (Mn (acac) 3 ), manganese (II) Trifluoroacetylacetonate (Mn (tfac) 2 ), iron (III) trifluoroacetylacetonate (Fe (tfac) 3 ), manganese (II) acetate (Mn (ac) 2 ), manganese (III) acetate (Mn (ac)
- the nickel precursor is nickel (II) nitrate (Ni (NO 3 ) 2 ), nickel sulfate (II) (NiSO 4 ), nickel (II) acetylacetonate (Ni (acac) 2 ), nickel (II) Trifluoroacetylacetonate (Ni (tfac) 2 ), nickel (II) acetate (Ni (ac) 2 ), nickel chloride (II) (NiCl 2 ), nickel bromide (II) (NiBr 2 ), nickel iodide ( II) (NiI 2 ), nickel sulfamate (Ni (NH 2 SO 3 ) 2 ), nickel stearate (II) ((CH 3 (CH 2 ) 16 COO) 2 Ni), nickel oleate (II) ((CH 3 (CH 2 ) 7 CHCH (CH 2 ) 7 COO) 2 Ni), nickel laurate (II) ((CH 3 (CH 2 ) 10
- the zinc precursor is zinc nitrate (II) (Zn (NO 3 ) 2 ), zinc sulfate (II) (ZnSO 4 ), zinc (II) acetylacetonate (Zn (acac) 2 ), zinc (II) trifluor Roacetylacetonate (Zn (tfac) 2 ), zinc (II) acetate (Zn (ac) 2 ), zinc chloride (II) (ZnCl 2 ), zinc bromide (II) (ZnBr 2 ), zinc iodide (II) (ZnI 2 ), zinc sulfamate (Zn (NH 2 SO 3 ) 2 ), zinc stearate (II) ((CH 3 (CH 2 ) 16 COO) 2 Zn), zinc oleate (II) ((CH 3 ( CH 2 ) 7 CHCH (CH 2 ) 7 COO) 2 Zn), zinc laurate (II) ((CH 3 (CH 2
- the iron precursor used in the ferrite nanocube production method of the present invention is preferably iron nitrate (II) (Fe (NO 3 ) 2 ), iron nitrate (III) (Fe (NO 3 ) 3 ), iron sulfate (II) ) (FeSO 4 ), iron sulfate (III) (Fe 2 (SO 4 ) 3 ), iron (II) acetylacetonate (Fe (acac) 2 ), iron (III) acetylacetonate (Fe (acac) 3 ) , Iron (II) trifluoroacetylacetonate (Fe (tfac) 2 ), iron (III) trifluoroacetylacetonate (Fe (tfac) 3 ), iron (II) acetate (Fe (ac) 2 ), Iron (III) acetate (Fe (ac) 3 ), iron (II) chloride (FeCl 2 ),
- the cobalt precursor, manganese precursor, nickel precursor, zinc precursor or barium precursor is used in a small amount compared to the amount of the iron precursor used in the preparation of the ferrite nanocube.
- the cobalt-doped magnetite, the manganese-doped magnetite, and the nickel may be used. This doped magnetite, zinc doped magnetite or barium doped magnetite can be produced.
- the surfactant is preferably selected from any one or a mixture thereof selected from the group consisting of carboxylic acid, alkylamine, alkyl alcohol or alkyl phosphine.
- the carboxylic acid is preferably octanoic acid (decanoic acid), decanoic acid (decanoic acid), lauric acid (lauric acid), hexadecanoic acid, oleic acid (oleic acid), stearic acid (stearic acid), benzoic acid (benzoic acid) and biphenylcarboxylic acid (biphenylcarboxylic acid) is selected from any one or a mixture thereof.
- the alkylamine is preferably octylamine, trioctylamine, decylamine, decylamine, dodecylamine, dodecylamine, tetratradecylamine, hexadecylamine, hexadecylamine, oleyl One selected from the group consisting of oleylalmine, octadecylamine, tribenzylamine or triphenylamine, or a mixture thereof.
- alkyl alcohol is preferably octyl alcohol (octylalcohol), decanol (decanol), hexadecanol (hexadecanol), hexadecandiol (hexadecandiol), oleyl alcohol (oleyl alcohol) or phenol (phenol) in the group Selected from any one or mixtures thereof.
- octyl alcohol octylalcohol
- decanol decanol
- hexadecanol hexadecanol
- hexadecandiol hexadecandiol
- oleyl alcohol oleyl alcohol
- phenol phenol
- alkyl phosphine is preferably selected from any one or a mixture thereof selected from the group consisting of triphenylphosphine and trioctylphosphine.
- the solvent is selected from organic solvents having a boiling point of 100 ° C. or more and a molecular weight of 100 to 400, preferably hexadecane, hexadecene, octadecane, octadecane, octadecene, icosan (eicosane), eicosene, phenanthrene, pentacene, anthracene, biphenyl, phenyl ether, octyl ether, decyl ether decyl ether, benzyl ether, or squalene (squalene) is selected from any one selected from the group consisting of or a mixture thereof.
- the heating temperature is 100 °C to below the boiling point of the solvent used, the heating rate is 0.5 °C / min to 50 °C / min, the pressure of the heating step is preferably maintained at 0.5 atm to 10 atm, respectively.
- the molar ratio of the iron precursor and the surfactant is 1: 0.1 to 1:20, and the molar ratio of the iron precursor and the solvent is preferably maintained at 1: 1 to 1: 1,000.
- the heating reaction time is significantly shortened, more octahedral ferrite nanoparticles are produced.
- the heating reaction time is slightly shortened, cube-shaped ferrite nanoparticles having cut off vertices are produced.
- the heating reaction time is too long, the surface of the nanoparticles is roughened.
- Ferrite nanoparticles of 20 nm or more are known to have ferrimagnetic properties at room temperature. Therefore, if the magnetic direction of the ferrite nanoparticles of the present invention is used as a unit of information, information can be stored by adjusting the magnetic direction of the nanoparticles.
- the cubic array also provides access to all the attached nanoparticles through two movements in the horizontal and vertical directions.
- hexagonal arrays of hexagonal arrays require two more diagonal movements in addition to the horizontal movement to access individual nanoparticles. Therefore, by using the cubic array of the present invention it is possible to configure a path for accessing the nanoparticles more simply and efficiently.
- 1 is a photograph of magnetite nanoparticles of various shapes according to the present invention.
- Figure 3 shows an X-ray diffraction pattern for the magnetite nanocube according to the present invention.
- Figure 4 is a photograph showing a cubic array of magnetite nanocube according to the present invention.
- FIG. 5 is a magnetization curve for a magnetite nanocube having a size of 80 nm according to the present invention.
- FIG. 6 is a magnetization curve of a magnetite nanocube having a size of 25 nm according to the present invention.
- FIG. 7 shows that the magnetite is changed from superparamagnetic to ferrimagnetic according to the size of the magnetite nanocube according to the present invention, and the nanocube is changed from a single domain to a multidomain.
- Iron (II) acetylacetonate (0.706 g, 2 mmol) was added to the mixture of oleic acid (1.129 g) and benzyl ether (10.4 g). The mixed solution was depressurized using a vacuum pump to remove residual air. The solution was then heated to 290 ° C. at a rate of 20 ° C./min with stirring. And held at 290 ° C. for 30 minutes. After cooling to 100 °C and the solution was washed with a mixture of toluene and hexane (n-hexane). The solution was centrifuged to obtain magnetite nanoparticles of 80 nm size.
- a magnetite nanocube having a size of 100 nm was obtained when the other conditions were the same as in Example 1 except that the temperature increase rate was 10 ° C / min.
- Example 2 Except for 20.8 g of benzyl ether and 2 minutes of heating time, the same conditions as in Example 1 were carried out to obtain a magnetite nanocube having a size of 20 nm.
- a magnetite nanocube having a size of 130 nm was obtained under the same conditions as in Example 1 except that 7.8 g of benzyl ether and heating time were 1 hour.
- a magnetite nanocube having a size of 160 nm was obtained under the same conditions as in Example 1 except for 5.2 g of benzyl ether and 2 hours of heating time.
- Example 2 Increasing the amount of oleic acid added in the reaction conditions of Example 1 to 1.271g, to obtain a nanoparticle having a chamfered octahedron and a cornered cube shape of about 70 nm size. Increasing the amount of oleic acid added to 1.412 g further increased the proportion of nanoparticles having an octagonal shape with a corner.
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Abstract
Description
Claims (42)
- 초상자성(superparamagnetic) 또는 페리자성(ferrimagnetic)을 나타내는 페라이트 나노큐브(nanocube).
- 제1항에 있어서, 상기 페라이트가 Fe3O4인 것임을 특징으로 하는 페라이트 나노큐브.
- 제1항에 있어서, 상기 페라이트가 이금속성 페라이트인 것임을 특징으로 하는 페라이트 나노큐브.
- 제3항에 있어서, 상기 이금속성 페라이트가 CoFe2O4, MnFe2O4, NiFe2O4, ZnFe2O4 및 BaFe12O19로 이루어진 군으로부터 선택되는 것임을 특징으로 하는 페라이트 나노큐브.
- 제1항에 있어서, 상기 페라이트가 금속이 도핑된 Fe3O4인 것임을 특징으로 하는 페라이트 나노큐브.
- 제5항에 있어서, 상기 금속이 Co, Mn, Ni, Zn 및 Ba으로 이루어진 군으로부터 선택되는 것임을 특징으로 하는 페라이트 나노큐브.
- 제1항에 있어서, 상기 마그네타이트 나노큐브의 크기가 10 nm 내지 200 nm인 것임을 특징으로 하는 페라이트 나노큐브.
- 페리자성을 나타내는 페라이트 나노큐브를 포함하는 큐빅 어레이(cubic array).
- 제8항에 있어서, 상기 페라이트가 Fe3O4인 것임을 특징으로 하는 큐빅 어레이.
- 제8항에 있어서, 상기 페라이트가 이금속성 페라이트인 것임을 특징으로 하는 큐빅 어레이.
- 제10항에 있어서, 상기 이금속성 페라이트가 CoFe2O4, MnFe2O4, NiFe2O4, ZnFe2O4 및 BaFe12O19로 이루어진 군으로부터 선택되는 것임을 특징으로 하는 큐빅 어레이.
- 제8항에 있어서, 상기 페라이트가 금속이 도핑된 Fe3O4인 것임을 특징으로 하는 큐빅 어레이.
- 제12항에 있어서, 상기 금속이 Co, Mn, Ni, Zn 및 Ba으로 이루어진 군으로부터 선택되는 것임을 특징으로 하는 큐빅 어레이.
- 페리자성을 띠는 팔면체 또는 꼭지점이 잘려나간 정육면체 형상의 페라이트 나노입자.
- 제14항에 있어서, 상기 페라이트가 Fe3O4인 것임을 특징으로 하는 팔면체 또는 꼭지점이 잘려나간 정육면체 형상의 페라이트 나노입자.
- 제14항에 있어서, 상기 페라이트가 이금속성 페라이트인 것임을 특징으로 하는 팔면체 또는 꼭지점이 잘려나간 정육면체 형상의 페라이트 나노입자.
- 제16항에 있어서, 상기 이금속성 페라이트가 CoFe2O4, MnFe2O4, NiFe2O4, ZnFe2O4 및 BaFe12O19로 이루어진 군으로부터 선택되는 것임을 특징으로 하는 팔면체 또는 꼭지점이 잘려나간 정육면체 형상의 페라이트 나노입자.
- 제14항에 있어서, 상기 페라이트가 금속이 도핑된 Fe3O4인 것임을 특징으로 하는 팔면체 또는 꼭지점이 잘려나간 정육면체 형상의 페라이트 나노입자.
- 제18항에 있어서, 상기 금속이 Co, Mn, Ni, Zn 및 Ba으로 이루어진 군으로부터 선택되는 것임을 특징으로 하는 팔면체 또는 꼭지점이 잘려나간 정육면체 형상의 페라이트 나노입자.
- 제14항에 있어서, 상기 페라이트 나노입자의 크기가 10 nm 내지 200 nm인 것임을 특징으로 하는 팔면체 또는 꼭지점이 잘려나간 정육면체 형상의 페라이트 나노입자.
- 금속 전구체, 계면활성제 및 용매의 혼합물을 가열하는 단계를 포함하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 금속 전구체가 철 전구체인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제22항에 있어서, 상기 철 전구체가 질산철(Ⅱ)(Fe(NO3)2), 질산철(Ⅲ)(Fe(NO3)3), 황산철(Ⅱ)(FeSO4), 황산철(Ⅲ)(Fe2(SO4)3), 아이언(Ⅱ) 아세틸아세토네이트(Fe(acac)2), 아이언(Ⅲ) 아세틸아세토네이트(Fe(acac)3), 아이언(Ⅱ) 트리플루오로아세틸아세토네이트(Fe(tfac)2), 아이언(Ⅲ) 트리플루오로아세틸아세토네이트(Fe(tfac)3), 아이언(Ⅱ) 아세테이트(Fe(ac)2), 아이언(Ⅲ) 아세테이트(Fe(ac)3), 염화철(Ⅱ)(FeCl2), 염화철(Ⅲ)(FeCl3), 브롬화철(Ⅱ)(FeBr2), 브롬화철(Ⅲ)(FeBr3), 요오드화철(Ⅱ)(FeI2), 요오드화철(Ⅲ)(FeI3), 과염소산철(Fe(ClO4)3), 아이언 설파메이트(Fe(NH2SO3)2), 스테아르산철(Ⅱ)((CH3(CH2)16COO)2Fe), 스테아르산철(Ⅲ)((CH3(CH2)16COO)3Fe), 올레산철(Ⅱ)((CH3(CH2)7CHCH(CH2)7COO)2Fe), 올레산철(Ⅲ)((CH3(CH2)7CHCH(CH2)7COO)3Fe), 라우르산철(Ⅱ)((CH3(CH2)10COO)2Fe), 라우르산철(Ⅲ)((CH3(CH2)10COO)3Fe), 펜타카르보닐철(Fe(CO)5), 엔니카르보닐철(Fe2(CO)9), 및 디소듐 테트라카르보닐철 (Na2[Fe(CO)4])로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 금속 전구체가 코발트 전구체, 망간 전구체, 니켈 전구체, 아연 전구체 및 바륨 전구체로 이루어진 군에서 선택되는 어느 하나와 철 전구체의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제24항에 있어서, 상기 코발트 전구체가 질산코발트(Ⅱ)(Co(NO3)2), 황산코발트(Ⅱ)(CoSO4), , 코발트(Ⅱ) 아세틸아세토네이트(Co(acac)2), 코발트(Ⅱ) 트리플루오로아세틸아세토네이트(Co(tfac)2), 코발트(Ⅱ) 아세테이트(Co(ac)2), 염화코발트(Ⅱ)(CoCl2), 브롬화코발트(Ⅱ)(CoBr2), 요오드화코발트(Ⅱ)(CoI2), 코발트 설파메이트(Co(NH2SO3)2), 스테아르산코발트(Ⅱ)((CH3(CH2)16COO)2Co), 올레산코발트(Ⅱ)((CH3(CH2)7CHCH(CH2)7COO)2Co), 라우르산코발트(Ⅱ)((CH3(CH2)10COO)2Co) 및 디 코발트 옥타카르보닐(Co2(CO)8)로 이루어진 군에서 선택되는 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제24항에 있어서, 상기 망간 전구체가 질산망간(Ⅱ)(Mn(NO3)2), 탄산망간(II)(MnCO3) 질산망간(Ⅲ)(Mn(NO3)3), 황산망간(Ⅱ)(MnSO4), 황산망간(Ⅲ)(Mn2(SO4)3), 망간(Ⅱ) 아세틸아세토네이트(Mn(acac)2), 망간(Ⅲ) 아세틸아세토네이트(Mn(acac)3), 망간(Ⅱ) 트리플루오로아세틸아세토네이트(Mn(tfac)2), 아이언(Ⅲ) 트리플루오로아세틸아세토네이트(Fe(tfac)3), 망간(Ⅱ) 아세테이트(Mn(ac)2), 망간(Ⅲ) 아세테이트(Mn(ac)3), 염화망간(Ⅱ)(MnCl2), 브롬화망간(Ⅱ)(MnBr2), 요오드화망간(Ⅱ)(MnI2), 과염소산망간(Mn(ClO4)3), 망간 설파메이트(Mn(NH2SO3)2), 스테아르산망간(Ⅱ)((CH3(CH2)16COO)2Mn), 스테아르산망간(Ⅲ)((CH3(CH2)16COO)3Mn), 올레산망간(Ⅱ)((CH3(CH2)7CHCH(CH2)7COO)2Mn), 올레산망간(Ⅲ)((CH3(CH2)7CHCH(CH2)7COO)3Mn), 라우르산망간(Ⅱ)((CH3(CH2)10COO)2Mn), 라우르산철(Ⅲ)((CH3(CH2)10COO)3Mn), 데카카르보닐다이망간(Mn2(CO)10) 및 망간(Ⅱ) 메톡사이드(Mn(OMe)2)로 이루어진 군에서 선택되는 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제24항에 있어서, 상기 니켈 전구체가 질산니켈(Ⅱ)(Ni(NO3)2), 황산니켈(Ⅱ)(NiSO4), , 니켈(Ⅱ) 아세틸아세토네이트(Ni(acac)2), 니켈(Ⅱ) 트리플루오로아세틸아세토네이트(Ni(tfac)2), 니켈(Ⅱ) 아세테이트(Ni(ac)2), 염화니켈(Ⅱ)(NiCl2), 브롬화니켈(Ⅱ)(NiBr2), 요오드화니켈(Ⅱ)(NiI2), 니켈 설파메이트(Ni(NH2SO3)2), 스테아르산니켈(Ⅱ)((CH3(CH2)16COO)2Ni), 올레산니켈(Ⅱ)((CH3(CH2)7CHCH(CH2)7COO)2Ni), 라우르산니켈(Ⅱ)((CH3(CH2)10COO)2Ni) 및 니켈 테트라카르보닐(Ni(CO)4)로 이루어진 군에서 선택되는 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제24항에 있어서, 상기 아연 전구체가 질산아연(Ⅱ)(Zn(NO3)2), 황산아연(Ⅱ)(ZnSO4), , 징크(Ⅱ) 아세틸아세토네이트(Zn(acac)2), 징크(Ⅱ) 트리플루오로아세틸아세토네이트(Zn(tfac)2), 징크(Ⅱ) 아세테이트(Zn(ac)2), 염화아연(Ⅱ)(ZnCl2), 브롬화아연(Ⅱ)(ZnBr2), 요오드화아연(Ⅱ)(ZnI2), 징크 설파메이트(Zn(NH2SO3)2), 스테아르산아연(Ⅱ)((CH3(CH2)16COO)2Zn), 올레산아연(Ⅱ)((CH3(CH2)7CHCH(CH2)7COO)2Zn), 라우르산아연(Ⅱ)((CH3(CH2)10COO)2Zn) 및 징크(Ⅱ) 터셔리부톡사이드(Zn(t-butoxide)2)로 이루어진 군에서 선택되는 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제24항에 있어서, 상기 바륨 전구체가 질산바륨(Ⅱ)(Ba(NO3)2), 황산바륨(Ⅱ)(BaSO4), , 바륨(Ⅱ) 아세틸아세토네이트(Ba(acac)2), 바륨(Ⅱ) 트리플루오로아세틸아세토네이트(Ba(tfac)2), 바륨(Ⅱ) 아세테이트(Ba(ac)2), 염화바륨(Ⅱ)(BaCl2), 브롬화바륨(Ⅱ)(BaBr2), 요오드화바륨(Ⅱ)(BaI2), 바륨 설파메이트(Ba(NH2SO3)2), 스테아르산바륨(Ⅱ)((CH3(CH2)16COO)2Ba), 올레산바륨(Ⅱ)((CH3(CH2)7CHCH(CH2)7COO)2Ba), 라우르산바륨(Ⅱ)((CH3(CH2)10COO)2Co) 및 바륨(Ⅱ) 이소프로폭사이드(Ba(i-Pr)2) 이루어진 군에서 선택되는 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제24항에 있어서, 상기 철 전구체가 질산철(Ⅱ)(Fe(NO3)2), 질산철(Ⅲ)(Fe(NO3)3), 황산철(Ⅱ)(FeSO4), 황산철(Ⅲ)(Fe2(SO4)3), 아이언(Ⅱ) 아세틸아세토네이트(Fe(acac)2), 아이언(Ⅲ) 아세틸아세토네이트(Fe(acac)3), 아이언(Ⅱ) 트리플루오로아세틸아세토네이트(Fe(tfac)2), 아이언(Ⅲ) 트리플루오로아세틸아세토네이트(Fe(tfac)3), 아이언(Ⅱ) 아세테이트(Fe(ac)2), 아이언(Ⅲ) 아세테이트(Fe(ac)3), 염화철(Ⅱ)(FeCl2), 염화철(Ⅲ)(FeCl3), 브롬화철(Ⅱ)(FeBr2), 브롬화철(Ⅲ)(FeBr3), 요오드화철(Ⅱ)(FeI2), 요오드화철(Ⅲ)(FeI3), 과염소산철(Fe(ClO4)3), 아이언 설파메이트(Fe(NH2SO3)2), 스테아르산철(Ⅱ)((CH3(CH2)16COO)2Fe), 스테아르산철(Ⅲ)((CH3(CH2)16COO)3Fe), 올레산철(Ⅱ)((CH3(CH2)7CHCH(CH2)7COO)2Fe), 올레산철(Ⅲ)((CH3(CH2)7CHCH(CH2)7COO)3Fe), 라우르산철(Ⅱ)((CH3(CH2)10COO)2Fe), 라우르산철(Ⅲ)((CH3(CH2)10COO)3Fe), 펜타카르보닐철(Fe(CO)5), 엔니카르보닐철(Fe2(CO)9), 및 디소듐 테트라카르보닐철 (Na2[Fe(CO)4])로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 계면활성제가 카르복시산, 알킬아민, 알킬알콜 및 알킬포스핀으로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제31항에 있어서, 상기 카르복시산이 옥탄산(octanoic acid), 데칸산(decanoic acid), 라우르산(lauric acid), 헥사데칸산(hexadecanoic acid), 올레산(oleic acid), 스테아르산(stearic acid), 벤조산(benzoic acid) 및 바이페닐카르복시산(biphenylcarboxylic acid)으로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제31항에 있어서, 상기 알킬아민이 옥틸아민(octylamine), 트리옥틸아민(trioctylamine), 데실아민(decylamine), 도데실아민(dodecylamine), 테트라데실아민(tetradecylamine), 헥사데실아민(hexadecylamine), 올레일아민(oleylalmine), 옥타데실아민(octadecylamine), 트리벤질아민(tribenzylamine) 및 트리페닐아민(triphenylamine)으로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제31항에 있어서, 상기 알킬알콜이 옥틸알콜(octylalcohol), 데칸올(decanol), 헥사데칸올(hexadecanol), 헥사데칸디올(hexadecandiol), 올레일알콜(oleyl alcohol) 및 페놀(phenol)로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제31항에 있어서, 상기 알킬포스핀이 트리페틸포스핀(triphenylphosphine) 및 트리옥틸포스핀(trioctylphosphine)으로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 용매가 끓는점이 100℃ 이상이고 분자량이 100 내지 400인 유기 용매인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제36항에 있어서, 상기 용매가 헥사데칸(hexadecane), 헥사데센(hexadecene), 옥타데칸(octadecane), 옥타데센(octadecene), 아이코산(eicosane), 아이코센(eicosene), 페난트렌(phenanthrene), 펜타센(pentacene), 안트라센(anthracene), 바이페닐(biphenyl), 페닐 에테르(phenyl ether), 옥틸 에테르(octyl ether), 데실 에테르(decyl ether), 벤질 에테르(benzyl ether) 및 스쿠알렌(squalene)으로 이루어진 군에서 선택되는 어느 하나 또는 이들의 혼합물인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 가열 온도가 100℃ 내지 사용된 용매의 비등점 이하인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 가열 속도가 0.5℃/min 내지 50℃/min인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 가열 단계의 압력이 0.5기압 내지 10기압인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 금속 전구체와 상기 계면활성제의 몰비율이 1:0.1 내지 1:20인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
- 제21항에 있어서, 상기 금속 전구체와 상기 용매의 몰비율이 1:1 내지 1:1,000인 것임을 특징으로 하는 페라이트 나노큐브 제조 방법.
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EP09832037.7A EP2377810A4 (en) | 2008-12-12 | 2009-09-25 | REGULAR HEXAHEDIC OR OCTAEDRIC FERRITE NANOPARTICLES AND PROCESS FOR PRODUCTION THEREOF |
US13/139,412 US20110303869A1 (en) | 2008-12-12 | 2009-09-25 | Cubic or octahedral shaped ferrite nanoparticles and method for preparing thereof |
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JP5425152B2 (ja) * | 2011-09-30 | 2014-02-26 | 富士フイルム株式会社 | 磁気記録媒体 |
KR101412084B1 (ko) * | 2012-02-27 | 2014-06-26 | 서울대학교산학협력단 | 페라이트 나노입자 집합체 및 이의 제조방법 |
ITTO20120306A1 (it) * | 2012-04-06 | 2013-10-07 | Fond Istituto Italiano Di Tecnologia | Nanocristalli di ferrite e loro usi |
CN103570079B (zh) * | 2013-11-01 | 2014-12-10 | 中北大学 | 一种自燃烧法制备纳米铁氧体的方法 |
CN103833343B (zh) * | 2014-03-01 | 2015-08-26 | 南通飞来福磁铁有限公司 | 一种纳米稀土永磁铁氧体材料 |
WO2016080329A1 (ja) * | 2014-11-18 | 2016-05-26 | 日油株式会社 | 鉄石鹸、その製造方法およびその鉄石鹸を含有する熱可塑性樹脂組成物 |
KR101686339B1 (ko) * | 2015-07-21 | 2016-12-13 | 건양대학교산학협력단 | 열분해법을 이용한 자성나노입자의 제조방법 |
RU2625981C1 (ru) * | 2016-09-16 | 2017-07-20 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный технологический институт (технический университет)" | Способ получения нанопорошков феррита кобальта и микрореактор для его реализации |
RU2664062C2 (ru) * | 2016-12-26 | 2018-08-14 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Способ получения кластеров из наночастиц магнетита |
US20200243230A1 (en) * | 2017-02-24 | 2020-07-30 | Nano Theranostics, Inc | Doped magnetic nanoparticles |
CN107151135B (zh) * | 2017-05-16 | 2020-11-13 | 天长市中德电子有限公司 | 一种绿色照明用纳米软磁铁氧体及其制备方法 |
CN107720836A (zh) * | 2017-11-17 | 2018-02-23 | 金川集团股份有限公司 | 一种镍铁氧体磁性材料及其制备方法 |
CN109264787B (zh) * | 2018-09-20 | 2020-10-30 | 济南大学 | 一种ZnFe2O4立方块体结构的制备方法及所得产品 |
WO2020222133A1 (en) * | 2019-04-30 | 2020-11-05 | Fondazione Istituto Italiano Di Tecnologia | Method for the gram-scale preparation of cubic ferrite nanocrystals for biomedical applications |
CN110808137B (zh) * | 2019-11-13 | 2021-08-17 | 山东师范大学 | 一种磁性富集材料、水体细菌检测试剂盒及应用 |
CN110993938B (zh) * | 2019-12-21 | 2022-08-30 | 河南电池研究院有限公司 | 一种锂离子电池用铁基复合氧化物负极材料及其制备方法 |
CN111548618A (zh) * | 2020-06-29 | 2020-08-18 | 江西伟普科技有限公司 | 一种金属负载碳/聚合物基电磁屏蔽材料及其制备方法 |
CN111592744A (zh) * | 2020-06-29 | 2020-08-28 | 江西伟普科技有限公司 | 一种金属负载碳/聚合物基电磁屏蔽材料及其制备方法 |
CN114538524A (zh) * | 2022-03-19 | 2022-05-27 | 合肥中镓纳米技术有限公司 | 一种四氧化三铁八面体纳米晶的制备方法及应用 |
CN115838187B (zh) * | 2022-12-14 | 2024-06-04 | 西安超磁纳米生物科技有限公司 | 一种微波辅助有机相超小铁氧体纳米颗粒及制备方法 |
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2014
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Publication number | Publication date |
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EP2377810A1 (en) | 2011-10-19 |
JP2012511495A (ja) | 2012-05-24 |
JP2015017036A (ja) | 2015-01-29 |
KR20100068122A (ko) | 2010-06-22 |
KR101628948B1 (ko) | 2016-06-09 |
WO2010068073A3 (ko) | 2010-09-10 |
US20110303869A1 (en) | 2011-12-15 |
WO2010068073A2 (ko) | 2010-06-17 |
EP2377810A4 (en) | 2014-03-05 |
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