WO2011131768A1 - Verfahren zur herstellung von partikeln - Google Patents
Verfahren zur herstellung von partikeln Download PDFInfo
- Publication number
- WO2011131768A1 WO2011131768A1 PCT/EP2011/056453 EP2011056453W WO2011131768A1 WO 2011131768 A1 WO2011131768 A1 WO 2011131768A1 EP 2011056453 W EP2011056453 W EP 2011056453W WO 2011131768 A1 WO2011131768 A1 WO 2011131768A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- particles
- precipitation
- tool
- comminution
- stress
- Prior art date
Links
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
- C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
-
- 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
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- 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
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Definitions
- the present invention relates to a process for producing particles such as micro- or nanoparticles by a precipitation reaction.
- Particles such as microparticles or nanoparticles, including particle collectives formed from these particles (such as aggregates or agglomerates), are used extensively in many technical fields.
- Advantageous applications for these materials are found in virtually all applications. Examples of such applications include fillers, catalytic processes, paints and coatings, pigments in the paper and printing industry, modifications of materials such as metals and polymers, as well as pharmaceutical, medical and cosmetic products.
- Known methods for the production of particles such as micro- or nanoparticles are precipitation reactions such as S o I gel method, or pyrolytic preparations. These methods are particularly suitable for the production of nanoparticles of oxides, hydroxides or other salts of metals.
- the liquid or gaseous starting material is transported through a high-temperature field, which leads to rapid evaporation of the readily volatile components or to the decomposition reaction.
- the particles subsequently formed by reaction of the gaseous educts can be adjusted specifically in terms of shape, particle size and distribution by changing the reaction parameters such as, for example, educt concentration and flame temperature.
- the resulting particles are only slightly aggregated or agglomerated, it is disadvantageous that these processes are carried out at very high temperatures, the one require appropriate equipment and high energy input and therefore are very expensive.
- the starting materials are added to a suitable liquid precipitation medium in which the starting materials precipitate in a particulate form under reaction conditions in which the reaction product reacts and the reaction product reacts.
- the reaction products often form a gel.
- the advantage of the sol-gel process over pyrolytic processes is that it can be carried out with relatively little effort and is easy to handle.
- the precipitated primary particles assemble into particle collectives, such as agglomerates and aggregates, which can have a size of several micrometers to 100 micrometers.
- the particle collectives formed also have an irregular, coarse structure and a broad particle size distribution.
- large and coarse structures with broad particle size distribution are unsuitable for many applications.
- they Before being used, therefore, they usually have to be subjected to extensive post-processing and conditioning, such as classification and optionally comminution. Nevertheless, the quality of the precipitated product is often insufficient even after extensive post-processing and conditioning for areas of application for which high product quality is required.
- GB 182,696 describes a process for the preparation of colloids and colloidal solutions, which is carried out in a colloid mill.
- the resulting colloids primary particles, aggregates or agglomerates
- the resulting colloids have a size of 1 ⁇ to 1 mm.
- a profiled cone rotates in an outer cone, whereby the rod rotates via a gap between the outer and inner cone as well as different cone angles is mechanically stressed in the gap.
- the resulting stress intensities are comparatively low, especially for smaller particles and particle collectives.
- the reason for this is the stress on aggregates and agglomerates of less than 50 ⁇ m in size due to shearing in the surrounding fluid instead of compressive or shear stresses between the two surfaces of the outer and inner cone.
- the present invention therefore relates to a process for the production of particles, in particular micro- or nanoparticles, by means of a precipitation reaction, in which the educts from which the particles are formed are added to a liquid precipitation medium and, with formation of the precipitates Particles react with each other, the particles precipitate, and the particle collectives formed are subjected parallel to the precipitation reaction of comminution by a load with freely movable grinding media.
- inorganic and organic particles can be obtained.
- the terms “particles” and “particle systems” refer to individual primary particles and to accumulations of two or more individual primary particles, as present, for example, in particle collectives such as aggregates or agglomerates.
- particle collectives such as aggregates or agglomerates.
- aggregates are generally understood aggregations of primary particles, the primary particles are usually connected to each other via solid bridges.
- Agglomerates can consist of both primary particles and aggregates, the bond usually being carried out via nonpolar, polar or electrostatic interactions, in particular by van der Waals forces.
- aggregates and agglomerates are collectively referred to as particle collective.
- the formation of large particle collectives as obtained in the conventional sol-gel process is prevented by carrying out the precipitation in conjunction with a comminution process. It is essential according to the invention that precipitation of the particles and comminution take place in parallel, ie the method according to the invention is a combination of precipitation and comminution by means of freely movable grinding media.
- the method according to the invention with parallel precipitation reaction and comminution results in free-moving milling media which significantly differentiate the size, size distribution, structure and strength of products as they do in a conventional production process obtained by precipitation and subsequent Nachbehandlu ng by crushing processes.
- the term "comminution” is understood to mean a reduction in size of the particles or particle collectives.
- the comminution can take place in the container in which the precipitation is carried out.
- a tool is provided in the container, which contains and moves grinding media.
- precipitation reactor in which the precipitation takes place and the tool for comminution may be connected in a circuit. It can be used grinding media, as they are known for the comminution of the suspensions obtained by the conventional sol-gel method.
- the tool may be a milling tool such as a mill, as is known for the wet comminution of particles or particle collectives.
- the tool may be a stirrer that moves the grinding media so that they can exert stress on the suspension as a result of the movement.
- the tool can be a mill that works with grinding media. Suitable brushes for ball mills, such as ball mills, are known in the art. Basket mills and agitator ball mills having grinding media.
- Basket mills essentially have a grinding basket filled with so-called grinding beads, which is immersed in the suspension for comminution. Through the bottom of the grinding basket runs concentrically a vertically arranged grinding shaft to which a grinding tool and optionally a so-called impeller are attached. The bottom has openings for the circulation of the suspension. The grinding media are set in motion by the grinding tool and thereby impinge on the product particles in between.
- An example of a suitable agitator ball mill is the laboratory agitator ball mill PML2 from Bühler AG with the COSMO process zone, which is a double annular gap system.
- the inventive method can be carried out directly in a stirred ball mill, wherein the precipitation takes place in the grinding chamber.
- precipitation reactor and agitator ball mill can be connected in the circuit.
- grinding media can be used, as they are known per se for wet comminution. These grinding bodies are freely movable bodies in the tool, in contrast to, for example, stress tools which are firmly connected to a rotor shaft.
- the material, the number and the shape of the grinding media can be selected as needed.
- the grinding media can be a round or substantially round z. B. have oval shape. However, they can basically have any shapes.
- the media may consist of silica, alumina, zirconia, steel, silicon carbide, polystyrene or polymethyl methacrylate.
- the particles or particle suspensions obtained by the process according to the invention can be exposed to a further, that is downstream, comminution process, in order to further reduce the particle size, if appropriate.
- the further comminution can be carried out by the same means as the comminution during the precipitation, that is, for example, with grinding tools containing grinding media, such as the already mentioned ball mills.
- the further comminution may also be carried out in another dispersing apparatus such as a dissolver, high-pressure homogenizer, ultrasonic homogenizer, kneader or a three-roll.
- micro- and nanoparticles that is particles in the nanometer and micrometer range, can be produced with the method according to the invention.
- nanoparticles with a diameter of less than 100 nm.
- the particles may consist of inorganic or organic materials.
- inorganic particles are those of oxides, hydroxides or other salts of metals, the term "metal” also including semimetals Concrete examples are Si0 2 , Ti0 2 , Al 2 0 3 , Zr0 2 , ZnO, CaC0 3 and BaS0 4 .
- organic particles are particles of organic semiconductor materials such as phthalocyanine, oligoacenes such as anthracene, tetracene, pentacene, polyvinylcarbazole and tetrafluorotetracyano quinodimethan (TCNQ), etc.
- organic semiconductor materials such as phthalocyanine, oligoacenes such as anthracene, tetracene, pentacene, polyvinylcarbazole and tetrafluorotetracyano quinodimethan (TCNQ), etc.
- the inventive method is also suitable for the production of particles for pharmaceutical purposes z. B. as a drug carrier.
- Particles Si0 2 ; Starting materials: C0 2 (gaseous), sodium silicate (Hu, Quingfu et al., Xiandai Huagong / Modern, Chemical Industry 20 (6), 2000, pp. 31-33); Sodium Metasilicate, Hydrochloric Acid and Cetyltrimethylammonium Bromide (Song X. et al., Proceedings of the Institution of Mechanical Engineers, Part N: Journal of Nanoengineering and Nanosystems 222 (1), 2008, pp. 27-31);
- Particles calcium carbonate; starting materials:
- Titanium Dioxide - Educts Titanium Dioxide - Educts
- Si0 2 nanoparticles are manufactured industrially by mixing a silicate solution with acid in an aqueous solution, typically at a temperature in the range of 60 to 100 ° C.
- the process according to the invention can be carried out in a manner known per se as a batch or semi-batch process.
- a semi-batch process while a part of the solution is placed in the precipitation reactor and the educts then fed continuously.
- the precipitation reaction is usually carried out at a predetermined temperature or a predetermined temperature profile, the temperature or the temperature profile depends on the nature of the particles to be produced and is known for the preparation of the individual particles.
- a precipitation medium aqueous systems, as well as solvent-based systems can be used, as described for. B. be used for the precipitation according to the sol-gel method.
- the precipitation can be carried out with the addition of a stabilizer which prevents the resulting dispersed particles from coagulating again to larger units.
- suitable stabilizers may be used for the present invention.
- suitable stabilizers for stabilizing suspensions to prevent coagulation of dispersed particles are also known per se.
- Suitable stabilizers are organosilane compounds such as (3-glycidyloxypropyl) trimethoxysilane (GLYMO).
- the stabilizer may be added to the precipitation medium at a predetermined time in a single dose or continuously over the time of precipitation. In the one-time addition at a later time in the course of the precipitation smaller particles are obtained as a result of continuous addition from the beginning. This makes it possible to control the particle size via the way in which the stabilizer is added.
- the amount of stabilizer which can be added to the precipitation medium varies depending on the specific application, such as type of starting materials, etc., and can be easily determined by a person skilled in the art for the particular application to be carried out by means of routine experiments.
- the inventive method is particularly suitable for the production of very small particles such as nanoparticles.
- the particle collectives obtained according to the invention also show a much clearer defined and delimited structure compared to the particle collectives obtained by the conventional methods.
- FIG. 6 shows examples of embodiments of the invention
- FIG. 1 The construction of the precipitation plant is shown schematically in FIG. 1
- the educts were added via storage tanks 2, 3 and peristaltic pumps 4, 5.
- the stabilizer was metered in via storage tanks 6 and Syringe pump 7.
- a thermostat F3C Haacke 8 was provided for temperature control.
- the system was connected to a pH meter 9 and a temperature gauge 10, wherein the measurement of the temperature and the pH was carried out directly in the reactor vessel 1.
- the temperature as well as the operating parameter speed, power consumption and precipitation time were recorded by means of a computer.
- the basket mill is a so-called dip mill, which essentially consists of a grinding basket 14 filled with grinding beads, which is immersed in the suspension for dispersion.
- the grinding basket 14 stands still while the grinding shaft 13, on which the impeller, the grinding tool and the dispersing disk 15 are mounted, rotates. Through the grinding tool, the grinding beads are moved in the dip mill.
- the dispersing disk 15 at the end of the Mah lwelle 13 and the built pump ensure the circulation of the ground material (also schematically indicated by arrows).
- Run 3 was carried out in the same way as run 2, except that GLYMO was used as stabilizer.
- the grinding shaft rotated at a peripheral speed of 8 m / s.
- the grinding chamber was filled with 142.2 g of grinding beads of yttrium-stabilized zirconium oxide with an average diameter of 500 ⁇ m.
- V t peripheral speed
- the mean particle size was measured once with the Helos / BF diffraction spectrometer from Sympatec GmbH, which operates with a HeNe laser with a wavelength of 632.8 nm and with particle sizes in the range of 0, 1 ⁇ to 875 ⁇ can be determined in dry and wet samples.
- the particle size analysis in the range of 1 n m to 1 0 ⁇ carried out by means of photon correlation spectroscopy with the spectrometer Nanophox Sympatec GmbH.
- Each sample was measured four times for 120 s at 120 ° C and the individual measurements were cumulatively combined into one measurement.
- the width of the particle size distribution was determined by the polydispersity index (PDI), the determination of the PDI by means of photon correlation spectroscopy as stated above.
- the PDI is a measure of the breadth of the particle size distribution. For monodisperse systems, this value is 1.
- the primary particle size in Run 1 was about 60 nanometers and the mean particle diameter x 50 17 ⁇ .
- a primary particle size of about 50 nm and a mean particle diameter x 50 of only 2 ⁇ were found.
- the PDI was significantly larger for runs 2 and 3 with about 0.39 for run 2 and 0.37 for run 3 than for run 1 with about 0.27.
- the SEM image of Run 2 in Figure 5 clearly shows the aggregate size of about 2 ⁇ obtained, the resulting aggregates are partially agglomerated as a result of drying.
- precipitation and comminution are carried out in the same container, wherein integrated into the precipitation reactor, for example, a basket mill 14 can be provided as a tool for comminution.
- Variant 3 is an example of a process according to the invention, wherein precipitation reactor 18 and comminution tool, for example an agitator ball mill 16, 17, are connected in the circuit.
- Precipitation reaction and comminution are carried out in one process stage.
- the medium with freshly formed particles is fed to the tool for comminution, and the medium is recirculated to the precipitation reactor 18.
- 17 lines are provided for this purpose between precipitation reactor 18 and agitator ball mill 16 ,.
- a pump 19 may be provided between precipitation reactor 18 and shredding tool.
- Precipitation reaction and comminution occur parallel to each other.
- educts and optionally additives are added to the precipitation reactor in parallel with comminution.
- the products can be removed from the tool for comminution, indicated in the figure by a branch in the line at the exit of the agitator ball mill 16, 17.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Silicon Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE112011101392.2T DE112011101392B4 (de) | 2010-04-24 | 2011-04-21 | Verfahren zur Herstellung von Partikeln |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE201010018279 DE102010018279A1 (de) | 2010-04-24 | 2010-04-24 | Verfahren und Vorrichtung zur Herstellung von Nanopartikeln |
DE102010018279.6 | 2010-04-24 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2011131768A1 true WO2011131768A1 (de) | 2011-10-27 |
Family
ID=44343790
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2011/056453 WO2011131768A1 (de) | 2010-04-24 | 2011-04-21 | Verfahren zur herstellung von partikeln |
Country Status (2)
Country | Link |
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DE (2) | DE102010018279A1 (de) |
WO (1) | WO2011131768A1 (de) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE1021762B1 (fr) * | 2013-12-18 | 2016-01-15 | Societe Industrielle Liegeoise Des Oxydes Sa | Composition d'additif de vulcanisation |
CN108751211A (zh) * | 2018-07-07 | 2018-11-06 | 河源市极致知管信息科技有限公司 | 一种改性石英砂的制备方法 |
CN108821297A (zh) * | 2018-07-07 | 2018-11-16 | 河源市极致知管信息科技有限公司 | 一种硅微粉的制备方法 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB182696A (en) | 1921-07-15 | 1922-07-13 | Hermann Plauson | Process for preparing colloids and colloidal solutions |
FR2641268A1 (fr) * | 1989-01-05 | 1990-07-06 | Bruggemann Kg L | Oxyde de zinc, carbonate de zinc et carbonate de zinc basique, leur procede de fabrication et leur utilisation |
WO2009093561A1 (ja) * | 2008-01-22 | 2009-07-30 | Osaka Prefecture University Public Corporation | コロイドを前駆体もしくは/および中間体とする無機ナノ粒子の製造方法 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0673620B2 (ja) * | 1990-07-03 | 1994-09-21 | 浅田鉄工株式会社 | 分散装置 |
DE102006047302A1 (de) * | 2006-10-06 | 2008-04-10 | Clariant International Limited | Gleitmittel für Wintersportgeräte |
-
2010
- 2010-04-24 DE DE201010018279 patent/DE102010018279A1/de not_active Withdrawn
-
2011
- 2011-04-21 WO PCT/EP2011/056453 patent/WO2011131768A1/de active Application Filing
- 2011-04-21 DE DE112011101392.2T patent/DE112011101392B4/de active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB182696A (en) | 1921-07-15 | 1922-07-13 | Hermann Plauson | Process for preparing colloids and colloidal solutions |
FR2641268A1 (fr) * | 1989-01-05 | 1990-07-06 | Bruggemann Kg L | Oxyde de zinc, carbonate de zinc et carbonate de zinc basique, leur procede de fabrication et leur utilisation |
DE3900243A1 (de) | 1989-01-05 | 1990-07-12 | Brueggemann L Kg | Zinkoxid, zinkcarbonat und basisches zinkcarbonat, verfahren zu ihrer herstellung und deren verwendung |
WO2009093561A1 (ja) * | 2008-01-22 | 2009-07-30 | Osaka Prefecture University Public Corporation | コロイドを前駆体もしくは/および中間体とする無機ナノ粒子の製造方法 |
Non-Patent Citations (13)
Title |
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BOGOEVSKI S., PERIODICA POLYTECHNICA: CHEMICAL ENGINEERING, vol. 44, no. 2, 2000, pages 133 - 140 |
FRACH ET AL., VAKUUM IN FORSCHUNG UND PRAXIS, vol. 19, no. 6, 2007, pages 20 - 27 |
HU, QUINGFU ET AL.: "Xiandai Huagong/Modern", vol. 20, 2000, CHEMICAL INDUSTRY, pages: 31 - 33 |
KEIS ET AL., SOL. ENERGY MATER. SOL. CELLS, vol. 73, 2002, pages 51 |
LIN ET AL., JOURNAL OF POWER SOURCES |
NIEMANN B. ET AL., JOURNAL OF COLLOID AND INTERFACE SCIENCE, vol. 342, no. 2, 2010, pages 361 - 371 |
S. MENDE ET AL: "Mechanical production and stabilization of submicron particles in stirred media mills", POWDER TECHNOLOGY, vol. 132, no. 1, 1 May 2003 (2003-05-01), pages 64 - 73, XP055004765, ISSN: 0032-5910, DOI: 10.1016/S0032-5910(03)00042-1 * |
SCHILDE C ET AL: "Effect of fluid@?particle-interactions on dispersing nano-particles in epoxy resins using stirred-media-mills and three-roll-mills", COMPOSITES SCIENCE AND TECHNOLOGY, ELSEVIER, UK, vol. 70, no. 4, 1 April 2010 (2010-04-01), pages 657 - 663, XP026911978, ISSN: 0266-3538, [retrieved on 20100104], DOI: 10.1016/J.COMPSCITECH.2009.12.021 * |
SHI Y ET AL: "CoFe2O4 nanoparticles prepared by the mechanochemical method", JOURNAL OF ALLOYS AND COMPOUNDS, ELSEVIER SEQUOIA, LAUSANNE, CH, vol. 308, no. 1-2, 10 August 2000 (2000-08-10), pages 290 - 295, XP004214943, ISSN: 0925-8388, DOI: 10.1016/S0925-8388(00)00921-X * |
SONG X. ET AL.: "Proceedings of the Institution of Mechanical Engineers", JOURNAL OF NANOENGINEERING AND NANOSYSTEMS, vol. 222, no. 1, 2008, pages 27 - 31 |
VARMA S. ET AL., MATERIALS CHEMISTRY AND PHYSICS, vol. 126, no. 1-2, 2011, pages 232 - 236 |
WANG Z. ET AL., MATERIALS SCIENCE AND ENGINEERING B, vol. 48, no. 3, 1997, pages 211 - 214 |
YOSHIKAZU TODAKA ET AL: "Synthesis of Ferrite Nanoparticles by Mechanochemical Processing Using a Ball Mill", MATERIALS TRANSACTIONS, SENDAI, JP, vol. 44, no. 2, 20 February 2003 (2003-02-20), pages 277 - 284, XP008140831, ISSN: 1345-9678, Retrieved from the Internet <URL:http://www.jim.or.jp/journal/e/44/02/277.html> * |
Also Published As
Publication number | Publication date |
---|---|
DE112011101392A5 (de) | 2013-01-31 |
DE112011101392B4 (de) | 2014-11-06 |
DE102010018279A1 (de) | 2011-10-27 |
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