JP5339682B2 - 金属酸化物微粒子の製造方法 - Google Patents
金属酸化物微粒子の製造方法 Download PDFInfo
- Publication number
- JP5339682B2 JP5339682B2 JP2007051574A JP2007051574A JP5339682B2 JP 5339682 B2 JP5339682 B2 JP 5339682B2 JP 2007051574 A JP2007051574 A JP 2007051574A JP 2007051574 A JP2007051574 A JP 2007051574A JP 5339682 B2 JP5339682 B2 JP 5339682B2
- Authority
- JP
- Japan
- Prior art keywords
- fine particles
- metal
- metal oxide
- oxide fine
- producing
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Fee Related
Links
Images
Classifications
-
- 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
-
- 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
- C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
-
- 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
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- 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
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G27/00—Compounds of hafnium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- 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
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Description
(Xは、フッ素、塩素、臭素、ヨウ素のいずれか、Rはメチル、エチル、プロピル、イソプロピル、n−ブチル、t−ブチルなどのアルキル基を示す。)
TiCl4+Ti(OiPr)4→TiO 2 (2)
また、金属ハライド、金属アルコキシドの金属種類を変更、組み合わせることで酸化チタン以外の金属酸化物微粒子を生成したり、複数の金属が含まれる複合金属酸化物を生成することも可能である(非特許文献2,3参照)。
xZrCl4+(1−x)Hf(OiPr)4→ZrxHf(1−x)O2 (4)
xTiCl4+(1−x)Zr(OiPr)4→TixZr(1−x)O2 (5)
なお、式3〜5の反応式の右辺では、金属酸化物のみを表示している。
図1に実験系の模式図を示し、これを参照しながら下記で実施例を説明する。
非特許文献1に記述される手順を参考に酸化チタン微粒子の合成を行った。アルゴン雰囲気下、100mL三口フラスコにヘプタデカン26.25g、TOPO9.75mmol、TiCl4を0.33mL(3mmol)加え、マントルヒーターにより300℃に昇温した。熱伝導による加熱のため、300℃に昇温するまでに1時間以上要した。Ti(OiPr)4を0.9mL(3mmol)シリンジによって素早く加え、5分間加熱攪拌した。加熱攪拌後、室温まで冷却した。攪拌しながらアセトン300mL中に反応溶液を滴下した。遠心分離(3000rpm、10分)により上澄み液を除去した後、ヘキサン150mLを加え再分散した。再分散したヘキサン溶液を400mLアセトンに少量ずつ加え再沈殿した。同様の操作を合計3回繰り返した。沈殿物を常温で自然乾燥し、淡黄色粉末を得た。
上記実施例及び比較例によって得られた紛体に対して、X線回折(XRD)測定、透過型電子顕微鏡による観察、赤外線吸収スペクトル分析装置(FTIR−ATR)による分析、熱重量分析(TGA)を行った。また、有機溶媒に対する分散性試験を行った。
ここで、D(110)は結晶子サイズ、K=0.9、λCu−Kα1=0.154056nm、βは回折ピークの半価幅である。
2 マイクロ波反応装置
3 シリンジ
4 冷却管
Claims (6)
- 金属ハライドと金属アルコキシドをホスフィンオキシド存在下で加熱し、金属酸化物微粒子を得る金属酸化物微粒子の製造方法であって、前記加熱をマイクロ波照射によって行い、前記マイクロ波の照射密度は0.1〜50W/cm 3 であることを特徴とする金属酸化物微粒子の製造方法。
- 前記ホスフィンオキシドが、炭素数4以上20以下アルキル基を含有するトリアルキルホスフィンオキシドである請求項1に記載の金属酸化物微粒子の製造方法。
- 前記金属ハライドが四塩化チタン(TiCl4)、前記金属アルコキシドがチタンテトライソプロポキシド(Ti(OiPr)4)、前記ホスフィンオキシドがトリオクチルホスフィンオキシドであることを特徴とする請求項1または2に記載の金属酸化物微粒子の製造方法。
- 前記金属酸化物微粒子の粒子径が1nm以上100nm以下である請求項1乃至3のいずれか一項に記載の金属酸化物微粒子の製造方法。
- 前記金属ハライドと、前記金属アルコキシドとは、非加水分解反応することを特徴とする請求項1乃至4のいずれか一項に記載の金属酸化物微粒子の製造方法。
- 金属ハライドとホスフィンオキシドの混合物にマイクロ波を照射して加熱する工程と、マイクロ波が照射された前記混合物と金属アルコキシドとの混合物にマイクロ波を照射して加熱する工程とを有し、前記マイクロ波の照射密度は0.1〜50W/cm 3 であることを特徴とする金属酸化物微粒子の製造方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007051574A JP5339682B2 (ja) | 2007-03-01 | 2007-03-01 | 金属酸化物微粒子の製造方法 |
PCT/JP2008/054002 WO2008105562A1 (en) | 2007-03-01 | 2008-02-28 | Metal coordination compound and production process thereof |
EP08721422A EP2118001A1 (en) | 2007-03-01 | 2008-02-28 | Metal coordination compound and production process thereof |
CN2008800068011A CN101622194B (zh) | 2007-03-01 | 2008-02-28 | 金属配位化合物及其制备方法 |
US12/526,198 US20100196257A1 (en) | 2007-03-01 | 2008-02-28 | Metal coordination compound and production process thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007051574A JP5339682B2 (ja) | 2007-03-01 | 2007-03-01 | 金属酸化物微粒子の製造方法 |
Publications (3)
Publication Number | Publication Date |
---|---|
JP2008214117A JP2008214117A (ja) | 2008-09-18 |
JP2008214117A5 JP2008214117A5 (ja) | 2012-10-25 |
JP5339682B2 true JP5339682B2 (ja) | 2013-11-13 |
Family
ID=39414913
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2007051574A Expired - Fee Related JP5339682B2 (ja) | 2007-03-01 | 2007-03-01 | 金属酸化物微粒子の製造方法 |
Country Status (5)
Country | Link |
---|---|
US (1) | US20100196257A1 (ja) |
EP (1) | EP2118001A1 (ja) |
JP (1) | JP5339682B2 (ja) |
CN (1) | CN101622194B (ja) |
WO (1) | WO2008105562A1 (ja) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3009402A1 (de) | 2014-10-15 | 2016-04-20 | Justus-Liebig-Universität Gießen | Verfahren zur Herstellung von gemischten Metallhalogenid-Alkoxiden und Metalloxid-Nanopartikeln |
FR3077566A1 (fr) * | 2018-02-02 | 2019-08-09 | Rhodia Operations | Procede de preparation d'un oxyde a base de cerium et/ou de zirconium |
FR3077567A1 (fr) * | 2018-02-02 | 2019-08-09 | Rhodia Operations | Procede de preparation d'un oxyde a base de cerium et/ou de zirconium |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3612546B2 (ja) * | 2002-05-27 | 2005-01-19 | 関西ティー・エル・オー株式会社 | 金属酸化物微粒子を製造する方法 |
US7144840B2 (en) * | 2004-07-22 | 2006-12-05 | Hong Kong University Of Science And Technology | TiO2 material and the coating methods thereof |
CN1317193C (zh) * | 2005-07-07 | 2007-05-23 | 上海交通大学 | 微波制备二氧化钛纳米管的方法 |
-
2007
- 2007-03-01 JP JP2007051574A patent/JP5339682B2/ja not_active Expired - Fee Related
-
2008
- 2008-02-28 US US12/526,198 patent/US20100196257A1/en not_active Abandoned
- 2008-02-28 EP EP08721422A patent/EP2118001A1/en not_active Withdrawn
- 2008-02-28 CN CN2008800068011A patent/CN101622194B/zh active Active
- 2008-02-28 WO PCT/JP2008/054002 patent/WO2008105562A1/en active Application Filing
Also Published As
Publication number | Publication date |
---|---|
WO2008105562A1 (en) | 2008-09-04 |
CN101622194A (zh) | 2010-01-06 |
JP2008214117A (ja) | 2008-09-18 |
CN101622194B (zh) | 2012-06-06 |
EP2118001A1 (en) | 2009-11-18 |
US20100196257A1 (en) | 2010-08-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Dastan | Effect of preparation methods on the properties of titania nanoparticles: solvothermal versus sol–gel | |
Leyva-Porras et al. | Low-temperature synthesis and characterization of anatase TiO2 nanoparticles by an acid assisted sol–gel method | |
Sathyaseelan et al. | Structural, optical and morphological properties of post-growth calcined TiO2 nanopowder for opto-electronic device application: Ex-situ studies | |
Horti et al. | Synthesis and photoluminescence properties of titanium oxide (TiO2) nanoparticles: Effect of calcination temperature | |
Thamaphat et al. | Phase characterization of TiO2 powder by XRD and TEM | |
Taziwa et al. | Influence of carbon modification on the morphological, structural, and optical properties of zinc oxide nanoparticles synthesized by pneumatic spray pyrolysis technique | |
Karkare | Choice of precursor not affecting the size of anatase TiO2 nanoparticles but affecting morphology under broader view | |
Horti et al. | Photoluminescence properties of SnO2 nanoparticles: effect of solvents | |
US5973175A (en) | Hydrothermal process for making ultrafine metal oxide powders | |
WO1997015526A1 (en) | Hydrothermal process for making ultrafine metal oxide powders | |
Ramazani et al. | Effect of nitric acid on particle morphology of the nano-TiO2 | |
Yahaya et al. | Recent characterisation of sol-gel synthesised TiO2 nanoparticles | |
JP2008518873A (ja) | 二酸化チタンナノ粒子の合成 | |
Barkhade et al. | Optical properties of Fe doped TiO2 nanocomposites synthesized by sol-gel technique | |
JP6468457B2 (ja) | 酸化チタン粒子およびその製造方法 | |
JP5339682B2 (ja) | 金属酸化物微粒子の製造方法 | |
Tsuzuki et al. | UV-shielding ceramic nanoparticles synthesised by mechanochemical processing | |
AU2003304660B2 (en) | Synthesis of ultrafine rutile phase titanium dioxide particles at low temperature | |
Athar | Metal oxide nanopowder | |
Selvi et al. | Effect of shell ZnO on the structure and optical property of TiO 2 core@ shell hybrid nanoparticles | |
Calatayud et al. | Hydrothermal-mediated synthesis of orange Cr, Sb-containing TiO2 nano-pigments with improved microstructure | |
US7413726B2 (en) | Synthesis of ultrafine rutile phase titanium dioxide particles | |
Prabu et al. | Micro strain and morphological studies of anatase and rutile phase TiO2 nanocrystals prepared via sol-gel and solvothermal method—a comparative study | |
Hafez et al. | Synthesis, characterization and color performance of novel Co2+-doped alumina/titania nanoceramic pigments | |
Xia et al. | Formation of TiO2 nanomaterials via titanium ethylene glycolide decomposition |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
RD04 | Notification of resignation of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7424 Effective date: 20100201 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20100301 |
|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20100301 |
|
RD01 | Notification of change of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7421 Effective date: 20100630 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20120907 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20121225 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20130225 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20130416 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20130617 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20130723 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20130806 |
|
LAPS | Cancellation because of no payment of annual fees |