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WO2003014011A1 - Preparation solvothermale de nanoparticules d'oxyde metallique - Google Patents

Preparation solvothermale de nanoparticules d'oxyde metallique Download PDF

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Publication number
WO2003014011A1
WO2003014011A1 PCT/KR2002/001535 KR0201535W WO03014011A1 WO 2003014011 A1 WO2003014011 A1 WO 2003014011A1 KR 0201535 W KR0201535 W KR 0201535W WO 03014011 A1 WO03014011 A1 WO 03014011A1
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WO
WIPO (PCT)
Prior art keywords
zno
ray diffraction
surface area
mvg
sem
Prior art date
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Ceased
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PCT/KR2002/001535
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English (en)
Inventor
Yun Soo Kim
Chang Gyoun Kim
Ki Whan Sung
Jong Tae Lim
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Korea Research Institute of Chemical Technology KRICT
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Korea Research Institute of Chemical Technology KRICT
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Publication of WO2003014011A1 publication Critical patent/WO2003014011A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/18—Methods for preparing oxides or hydroxides in general by thermal decomposition of compounds, e.g. of salts or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G11/00—Compounds of cadmium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

Definitions

  • the present invention relates to a solvothermal method for preparing a nano-sized metal oxide powder comprising pyrolyzing an organic compound of a divalent metal in a solvent.
  • a particulate material having a particle size in the range of several nm to 100 nm is referred to as a nano material which has a high surface area and physical properties quite different from the bulk material.
  • Such nano-material can be used as a new photoelectronic material because of shift of its electron energy levels to shorter wavelengths.
  • a nanoparticle has been conventionally prepared by flame pyrolysis, spray pyrolysis, sol-gel and inverse micelle micro- emulsion methods (see, e.g., G. Westin and M. Nygren, J. Mater. Sci. 27, 1617, 1992).
  • the flame pyrolysis method requires a special pyrolytic apparatus and a delicate process control to avoid the formation of hollow spherical particles.
  • the sol-gel method requires the use of a high-pressure reactor in a super-critical dry process.
  • the micelle emulsion method has an advantage in that the particle size is easily controlled, but has the problems of requiring a large quantity of a surfactant and difficulty in scaling up for large scale production.
  • the solvothermal pyrolysis method involves pyrolysis of a suitable organometallic compound in a solvent, and therefore, it is easy to control the temperature, the particle size and the properties of the final product.
  • the present inventors have endeavored to develop a solvopyrolytic method for producing metal oxide nanoparticle at a relatively low temperature in the absence of added O 2 by way of using a specific precursor.
  • an object of the present invention to provide a solvothermal method for preparing nanoparticles of a divalent metal oxide comprising pyrolyzing a divalent metal precursor having alkyl and alkoxy ligands at a relatively low temperature, with optional use of a capping ligand.
  • a process for preparing a nanoparticle of metal oxide which comprises pyrolyzing a compound of formula (I) in a solvent:
  • M is beryllium, zinc, magnesium or cadmium; and R and R' are each independently a C 1-5 alkyl group.
  • the present invention provides a method for preparing metal oxide nanoparticles by pyrolyzing an alkylmetal alkoxide of formula (I) in a solvent at a relatively low temperature.
  • a compound of formula RMgOR' may be prepared by the method represented by Scheme 1, and a compound of formula RZnOR', by the method illustrated in Scheme 2.
  • X is Cl, Br or I.
  • a compound containing beryllium or cadmium may be similarly prepared by the method of Schemes I or II.
  • the method of the present invention can be performed without added 0 2 or air through pyrolyzing a compound of formula (I) in an organic solvent having a boiling point of 100 to 400 ° C under an inert gas atmosphere.
  • a solvent devoid of water and oxygen can be used and the solvent is preferably selected from dimethoxyethane, hexadecane, tetra(ethyleneglycol)dimethyl ether and dioctyl ether.
  • the pyrolysis is preferably carried out at a temperature below 300 ° C .
  • the size of metal oxide nanoparticles resulting from the pyrolysis may be controlled by further incorporating in the solvent a capping ligand which adsorbs on, and pacifies, the surface of nanoparticles formed.
  • the capping ligand is an organic compound containing an electron-donating functional group, and it is preferably 1,3-dimethyl- undecanomalonate, dioctylamine, tridodecylmethylamonium iodide, or a mixture thereof.
  • the capping ligand is employed in an amount of 0.05 to 10 equivalents, preferably 0.5 to 5 equivalents, based on the amount of the alkylmetal alkoxide compound.
  • the particulate powder prepared by the pyrolysis of the present invention contains a small, minute amount of elemental metal besides metal oxide, it may be heat treated in an oxidizing atmosphere.
  • metal oxide nanoparticles of a controlled size distribution can be prepared in a large scale and economic way.
  • SEM Coagulated spherical particles with an average size of less than 10 nm.
  • Example 2 The procedure of Example 1 was repeated except for using 0.032 g of dimethoxyethane, to obtain a brown powder which was verified as magnesium oxide nanoparticles having a surface area of 235.93 mVg by X-ray diffraction, SEM and BET methods.
  • SEM Coagulated spherical particles with an average size of less than 10 nm.
  • Example 1 The procedure of Example 1 was repeated except for using 0.080 g of dimethoxyethane, to obtain a brown powder which was verified as magnesium oxide nanoparticles having a surface area of 243.78 mVg by X-ray diffraction, SEM and BET methods.
  • SEM Coagulated spherical particles with an average size less than 10 nm.
  • Example 1 The procedure of Example 1 was repeated except for using 0.80 g of dimethoxyethane, to obtain a brown powder which was verified as magnesium oxide nanoparticles having surface area of 230.18 mVg by X-ray diffraction, SEM and BET methods.
  • SEM Coagulated spherical particles with an average size of less than 10 nm.
  • Example 2 The procedure of as Example 1 was repeated except that dimethoxyethane was not employed, to obtain a brown powder which was verified as magnesium oxide nanoparticles having surface area of 323.51 mVg by X-ray diffraction, SEM and BET methods.
  • SEM Coagulated spherical particles with an average size of less than 10 nm.
  • methylzinc isopropoxide 1.5 g was dissolved in 10 ml of hexane, injected using a syringe into 30 ml of hexadecane refluxing at 300 ° C in a refluxing apparatus, and refluxed for 30 minutes. The mixture was cooled, filtered under an inert gas atmosphere, washed with diethyl ether to remove residual hexadecane, and then dried at room temperature, to obtain 1.2 g of a white powder which was verified as ZnO nanoparticles having a surface area of 65.20 mVg by X-ray diffraction, SEM and BET methods.
  • SEM Coagulated spherical particles with an average size of 50-70 nm.
  • methylzinc isopropoxide 1.5 g was dissolved in 30 ml of hexadecane and heated at 300 °C for 12 hours in a refluxing apparatus. The mixture was cooled, filtered under an inert gas atmosphere, washed with diethyl ether to remove residual hexadecane, and then dried at room temperature, to obtain 1.53 g of a gray powder which was verified as ZnO nanoparticles having a surface area of 127.16 mVg by X-ray diffraction, SEM and BET methods.
  • Example 7 The procedure of Example 7 was repeated except for heating the reaction mixture at 250 °C , to obtain a gray powder (1.25 g) which was verified as ZnO nanoparticles having a surface area of 16.35 mVg by X-ray diffraction, SEM and BET methods.
  • Example 7 The procedure of Example 7 was repeated except for heating the reaction mixture at 200 °C, to obtained a white powder (1.12 g) which was verified as ZnO nanoparticles having a surface area of 93.37 mVg by X-ray diffraction, SEM and BET methods.
  • SEM 40-60 nm coagulated aggregates of spherical particles with an average size less than 10 nm.
  • Example 10 The procedure of Example 10 was repeated except for heating at 150 °C , to obtained a white powder which was verified as ZnO nanoparticles having a surface area of 55.52 mVg by X-ray diffraction, SEM and BET methods.
  • SEM Coagulated spherical particles with an average size of 30-50 nm.
  • Example 8 The procedure of Example 8 was repeated except for dissolving methylzinc isopropoxide in 30 ml of dioctyl ether, to obtain a gray powder (1.15 g) which was verified as ZnO nanoparticles having a surface area of 38.15 mVg by X-ray diffraction, SEM and BET methods.
  • SEM Coagulated spherical particles with an average size of 30-50 nm.
  • Example 12 The procedure of Example 12 was repeated except for heating the reaction mixture at 200 ° C , to obtain a white powder (1.0 g) which was verified as ZnO nanoparticles having a surface area of 21.42 mVg by X-ray diffraction, SEM and BET methods.
  • SEM 20-30 nm coagulated aggregates of spherical particles with an average size less than 10 nm.
  • Example 14 The procedure of Example 14 was repeated except for heating at 150 ° C , to obtain a white powder (1.18 g) which was verified as ZnO nanoparticles having a surface area of 136.42 mVg by X-ray diffraction, SEM and BET methods.
  • ethylzinc isopropoxide 1.5 g was dissolved in 10 ml of anhydrous tetrahydrofuran. 0.55 g (5 equivalents based on ethylzinc isopropoxide) of 1,3- dimethyl-2-undecanomalonate, a capping ligand, was dissolved in 20 ml of tetra(ethyleneglycol)dimethyl ether and heated to 200 ° C. The tetrahydrofuran solution of ethylzinc isopropoxide was injected into the heated tetra(ethyleneglycol)d ⁇ methyl ether solution using a syringe. The reaction mixture was kept at 150 °C for 10 hours and cooled (first precipitation).
  • TEM second precipitated powder
  • Example 16 The procedure of Example 16 was repeated except for dissolving 1,3- dimethyl-2-undecanomalonate in dioctyl ether, to obtain 0.12 g and 0.23 g of a white powder by the first and second precipitation, respectively, which were verified to be ZnO nanoparticles by X-ray diffraction, TEM and BET methods.
  • TEM second precipitated powder
  • the tetra(ethyleneglycol)dimethyl ether solution of ethylzinc isopropoxide was injected into the heated tetra(ethyleneglycol)dimethyl ether using a syringe, and the tetra(ethyleneglycol)dimethyl ether solution of 1,3- dimethyl-2-undecanomalate was also injected 5 minutes later.
  • the reaction mixture was kept at 150 °C for 10 hours and cooled. Then, the mixture was centrifuged at 6000 rpm for 30 minutes to precipitate a white powder, 2.75 g.
  • the obtained powder was washed with diethyl ether, dried at room temperature, and verified to be ZnO nanoparticles by X-ray diffraction, TEM and BET methods. The presence of the capping ligand was confirmed by FT-IR.
  • TEM Spherical particles with an average size less than 10 nm.
  • the tetra(ethyleneglycol)dimethyl ether solution of ethylzinc isopropoxide was injected into the heated tetra(ethyleneglycol)dimethyl ether using a syringe, and the tetra(ethyleneglycol)dimethyl ether solution of 1,3- dimethyl-2-undecanomalate was also injected 5 minutes later.
  • the reaction mixture was kept at 150 °C for 40 minutes and cooled (first precipitation). Then the mixture was centrifuged at 6000 m for 30 minutes to precipitate a light yellow powder, 0.15 g.
  • TEM second precipitated powder
  • Example 19 The procedure of Example 19 was repeated except that the first precipitation was performed for 4 hours, to obtain 0.3 g and 1.52 g of light yellow powders at the first and second precipitation steps, respectively, which were verified as to be ZnO nanoparticles by X-ray diffraction, TEM and BET methods.
  • TEM second precipitated powder
  • TEM second precipitated powder
  • FT-LR second precipitated powder
  • Example 21 The procedure of Example 21 was repeated except for heating dioctylamine to 250 ° C and performing the first precipitation at 200 ° C, to obtain 0.14 g and 0.5 g of white powders at the first and second precipitation steps, respectively, which were verified to be ZnO nanoparticles by X-ray diffraction, TEM and BET methods. The presence of the capping ligand was confirmed by FT-IR.
  • the peak of ZnO(lOl) was overlapped within a wide peak, (surface area: 85.56 mVg) 2)
  • the second precipitated powder showed ZnO characteristic peaks at
  • TEM second precipitated powder
  • FT-LR second precipitated powder
  • Example 22 The procedure of Example 22 was repeated except that the first precipitation was performed at 150 ° C , to obtain 0.16 g and 0.64 g of white powders at the first and second precipitation steps, respectively, which were verified as ZnO nanoparticles by X-ray diffraction, TEM and BET methods. The presence of the capping ligand was confirmed by FT-IR.
  • TEM second precipitated powder
  • ethylzinc isopropoxide 1.5 g was dissolved in 20 ml of tetra(ethyleneglycol)dimethyl ether. 0.5 g of tridodecylmethylammonium iodide (0.07 equivalents based on ethylzinc isopropoxide), a capping ligand, was heated to 250 °C in a refluxing apparatus. The tetra(ethyleneglycol)dimethyl ether solution of ethylzinc isopropoxide was injected into the heated tridodecylmethylammonium iodide using a syringe. The reaction mixture was kept at 150 °C for 4 hours.
  • the mixture was cooled to 100 ° C and the precipitate was separated from the solution using a filtering rod.
  • the precipitate thus obtained was dissolved in ethanol and 200 ml of tertiary distilled water was added thereto to precipitate a light yellow powder (first precipitation).
  • the mixture was centrifuged at 6000 ⁇ m for 30 minutes to obtain a light yellow powder, 0.14 g. 200 ml of tertiary distilled water was added to the supernatant solution to induce a second stage precipitation (second precipitation) and centrifuged at 6000 ⁇ m for 30 minutes, to obtain 0.34 g of a light yellow powder.
  • TEM second precipitated powder

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

Selon l'invention, une nanoparticule d'oxyde métallique est préparée par pyrolyse d'un composé de formule (I) dans un solvant. Dans cette formule, M est béryllium, zinc, magnésium ou cadmium, et R et R' sont indépendamment un groupe alkyle C1-5.
PCT/KR2002/001535 2001-08-10 2002-08-10 Preparation solvothermale de nanoparticules d'oxyde metallique Ceased WO2003014011A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR2001/48336 2001-08-10
KR10-2001-0048336A KR100457824B1 (ko) 2001-08-10 2001-08-10 용액 열분해법에 의한 나노 크기 2가 금속 산화물 분말의제조

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WO2003014011A1 true WO2003014011A1 (fr) 2003-02-20

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100457824B1 (ko) * 2001-08-10 2004-11-18 한국화학연구원 용액 열분해법에 의한 나노 크기 2가 금속 산화물 분말의제조
DE102008058040A1 (de) 2008-11-18 2010-05-27 Evonik Degussa Gmbh Formulierungen enthaltend ein Gemisch von ZnO-Cubanen und sie einsetzendes Verfahren zur Herstellung halbleitender ZnO-Schichten
WO2010139910A1 (fr) * 2009-06-05 2010-12-09 Centre National De La Recherche Scientifique (C.N.R.S.) Procédé de préparation d'une composition hydrocompatible de nanocristaux d'oxyde(s) métallique(s)
US8211388B2 (en) 2006-02-16 2012-07-03 Brigham Young University Preparation of uniform nanoparticles of ultra-high purity metal oxides, mixed metal oxides, metals, and metal alloys
US9079164B2 (en) 2012-03-26 2015-07-14 Brigham Young University Single reaction synthesis of texturized catalysts
US9114378B2 (en) 2012-03-26 2015-08-25 Brigham Young University Iron and cobalt based fischer-tropsch pre-catalysts and catalysts
US9289750B2 (en) 2013-03-09 2016-03-22 Brigham Young University Method of making highly porous, stable aluminum oxides doped with silicon

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US5378665A (en) * 1992-10-30 1995-01-03 General Atomics Crystalline yttrium aluminate and process for making
US5782954A (en) * 1995-06-07 1998-07-21 Hoeganaes Corporation Iron-based metallurgical compositions containing flow agents and methods for using same
US5952421A (en) * 1995-12-27 1999-09-14 Exxon Research And Engineering Co. Synthesis of preceramic polymer-stabilized metal colloids and their conversion to microporous ceramics
US5980977A (en) * 1996-12-09 1999-11-09 Pinnacle Research Institute, Inc. Method of producing high surface area metal oxynitrides as substrates in electrical energy storage
US6268014B1 (en) * 1997-10-02 2001-07-31 Chris Eberspacher Method for forming solar cell materials from particulars

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US5958361A (en) * 1993-03-19 1999-09-28 Regents Of The University Of Michigan Ultrafine metal oxide powders by flame spray pyrolysis
FR2755136B1 (fr) * 1996-10-25 1999-01-22 Virsol Procede de preparation de nanoparticules de methylidene malonate, nanoparticules contenant eventuellement une ou plusieurs molecules biologiquement actives et compositions pharmaceutiques les contenant
DE19754304A1 (de) * 1997-12-08 1999-06-10 Hoechst Ag Polybetain-stabilisierte Platin-Nanopartikel, Verfahren zu ihrer Herstellung und Verwendung für Elektrokatalysatoren in Brennstoffzellen
WO2000027754A1 (fr) * 1998-11-09 2000-05-18 Nanogram Corporation Particules d'oxyde metallique
KR100457824B1 (ko) * 2001-08-10 2004-11-18 한국화학연구원 용액 열분해법에 의한 나노 크기 2가 금속 산화물 분말의제조

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5378665A (en) * 1992-10-30 1995-01-03 General Atomics Crystalline yttrium aluminate and process for making
US5782954A (en) * 1995-06-07 1998-07-21 Hoeganaes Corporation Iron-based metallurgical compositions containing flow agents and methods for using same
US5952421A (en) * 1995-12-27 1999-09-14 Exxon Research And Engineering Co. Synthesis of preceramic polymer-stabilized metal colloids and their conversion to microporous ceramics
US5980977A (en) * 1996-12-09 1999-11-09 Pinnacle Research Institute, Inc. Method of producing high surface area metal oxynitrides as substrates in electrical energy storage
US6268014B1 (en) * 1997-10-02 2001-07-31 Chris Eberspacher Method for forming solar cell materials from particulars

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100457824B1 (ko) * 2001-08-10 2004-11-18 한국화학연구원 용액 열분해법에 의한 나노 크기 2가 금속 산화물 분말의제조
US8211388B2 (en) 2006-02-16 2012-07-03 Brigham Young University Preparation of uniform nanoparticles of ultra-high purity metal oxides, mixed metal oxides, metals, and metal alloys
DE102008058040A1 (de) 2008-11-18 2010-05-27 Evonik Degussa Gmbh Formulierungen enthaltend ein Gemisch von ZnO-Cubanen und sie einsetzendes Verfahren zur Herstellung halbleitender ZnO-Schichten
WO2010139910A1 (fr) * 2009-06-05 2010-12-09 Centre National De La Recherche Scientifique (C.N.R.S.) Procédé de préparation d'une composition hydrocompatible de nanocristaux d'oxyde(s) métallique(s)
FR2946266A1 (fr) * 2009-06-05 2010-12-10 Centre Nat Rech Scient Procede de preparation d'une composition hydrocompatible de nanocristaux d'oxydes(s) metallique(s) et composition hydrocompatible obtenue
US9162900B2 (en) 2009-06-05 2015-10-20 Centre National De La Recherche Scientifique (C.N.R.S.) Method for preparing a water-compatible composition of metal oxide nanocrystals and the water-compatible composition obtained
US9079164B2 (en) 2012-03-26 2015-07-14 Brigham Young University Single reaction synthesis of texturized catalysts
US9114378B2 (en) 2012-03-26 2015-08-25 Brigham Young University Iron and cobalt based fischer-tropsch pre-catalysts and catalysts
US9289750B2 (en) 2013-03-09 2016-03-22 Brigham Young University Method of making highly porous, stable aluminum oxides doped with silicon

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KR100457824B1 (ko) 2004-11-18
KR20030014019A (ko) 2003-02-15

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