WO2000078674A1 - Verfahren zur dynamisch-chemischen herstellung von diamantartigen kohlenstoffstrukturen, diamantartige kohlenstoffstrukturen und verwendungen von diamantartigen kohlenstoffstrukturen - Google Patents
Verfahren zur dynamisch-chemischen herstellung von diamantartigen kohlenstoffstrukturen, diamantartige kohlenstoffstrukturen und verwendungen von diamantartigen kohlenstoffstrukturen Download PDFInfo
- Publication number
- WO2000078674A1 WO2000078674A1 PCT/DE2000/001885 DE0001885W WO0078674A1 WO 2000078674 A1 WO2000078674 A1 WO 2000078674A1 DE 0001885 W DE0001885 W DE 0001885W WO 0078674 A1 WO0078674 A1 WO 0078674A1
- Authority
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- Prior art keywords
- diamond
- carbon
- structures
- carbon structures
- type carbon
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/26—Preparation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
Definitions
- the invention relates to methods for the dynamic chemical production of diamond-like carbon structures, in which a hybrid carbon phase is placed in a closed container and is brought to a chemical reaction with an energy carrier in order to form disperse condensed carbon as a reaction product.
- the invention further relates to various diamond-like carbon structures and uses of such carbon structures.
- Dispersed condensed carbon is produced as a phase-changed carbon structure, particularly in the context of synthetic diamond production.
- dynamic processes are also used, which are based on the chemical conversion of high-energy substances and compounds and for the formation of hexagonal and cubic carbon structures mainly in the form of disperse and ultra-disperse systems.
- the basis of the dynamic chemical production of diamond-like carbon structures is formed by the laws that are predominantly involved in the chemical conversion of high-energy substances negative oxygen balance, to be carried out for a short time. They consist essentially in the fact that the condensed carbon released in the chemical reaction of these substances and characterized by the generator gas reaction is exposed to conditions such that a phase change into more structured crystal lattice structures can take place.
- the chemical reaction of carbon-containing energy sources is usually achieved by explosives with a negative oxygen balance and carried out in closed high-pressure containers under conditions of an inert gas atmosphere.
- the atmospheric oxygen must be largely eliminated by vacuuming the container system in order to achieve an inert gas atmosphere through special inert gases or their mixtures, each of which is under functional pressure.
- This inert gas atmosphere is intended to counteract the re-graphitization of the more highly structured carbon phases.
- the present invention has for its object to develop a method for the dynamic chemical production of diamond-like carbon structures, which enables an economical production method with high phase purity.
- diamond-like carbon structures with defined properties are to be provided and new uses of such substances are proposed.
- the task is solved with a generic method, in which the reaction product is exposed to an atomically hydrogen-supported low-temperature plasma and a phase change of Carbon combinations in high-purity cubic lattice structures is achieved.
- a carbon donor system is preferably also introduced.
- This carbon donor system preferably has liquid or gaseous hydrocarbon compounds, particularly good process results having been achieved especially with organic hydrocarbon compounds.
- the invention is based on the knowledge that hybrid carbon systems, previously liquid hydrocarbon compounds in combination with condensed carbon formed during the chemical conversion of the energy sources, can be introduced into a highly energetic and short-term chemical and thermogas dynamic process in such a way that, on the one hand, the formation of condensed carbon supports stoichometrically on the other hand, the covalescence of already formed or depositioned clusters is initiated from the chemical reaction of an energy source used and can be optimally carried out in a complex system.
- the chemical-physical formation process is carried out under conditions of an atomically hydrogen-based low-temperature plasma in supported by ⁇ > 9, 12xl0 17 to the effect that the electron promotion with subsequent hybridization predominantly does not take place according to the diffusion mechanism but according to the martensite mechanism.
- the diamond-like carbon structures produced in this way can be technically shaped in such a way that they are starting materials for the representation of more highly structured carbon systems, such as fullerenes, hyper-fullerenes, nano-tubes, onion-like carbons (OLC) and others. form.
- the invention furthermore relates to diamond-like carbon structures which are distinguished by the fact that the purity of the cubic diamond phase is 99%, preferably 100% (NJC Scan 1 / X-Ray pattern).
- the crystallite sizes of the carbon structures are in the range between 5 nm and 50 nm (X-ray diffraction). Cluster sizes of 50 nm to 20 ⁇ m (scanning electron microscope) and particle diameters in dispersion from 40 nm to 500 nm (photon correlation spectroscopy) were achieved. X-ray amorphous phases do not occur.
- Various parameters of the material can be varied or doped (cloning) through the process control: specific surface values, specific magnetizability, zeta potential, specific electrical Resistance, free energy in relation to water vapor absorption, among others, the following features can be controlled in this way: porosities and sorption properties, characteristics that give definitive crosslinking parameters, surface polarities in a hydrophilic or hydrophobic design, transfer, electrical insulation and semiconductor properties, among others
- High-performance diamond systems are extremely cost-intensive and not optimal and effective for a number of technical applications.
- the described diamond-like carbon structures according to the invention can be produced economically and efficiently by dynamic-chemical hybrid technologies and have a large number of specific properties which make them stand out in comparison with conventional industrial diamond configurations.
- FIGS. 1 to 4 show the results of the nano-polishing according to the invention of a pre-ground surface made of silicon nitride ceramic in comparison to a high-performance diamond grain.
- FIGS. 1 and 2 show a silicon nitride ceramic that was ground and then polished with a commercially available diamond suspension.
- FIGS. 3 and 4 show a nano high-end polish with an aqueous-cationic, short-chain suspension of diamond-like carbon structures on a ground silicon nitride ceramic.
- the diamond-like carbon structures according to the invention are particularly suitable for the following treatment processes:
- the optimal polishing speed is between 0.3 ⁇ m and 5 ⁇ m per minute.
- polishing of complex and non-planar surfaces by means of vibratory grinding (trowalizing) as well as planarizing elements of high-performance and microelectronics are to achieve the desired characteristic and performance characteristics.
- carrier media are aqueous and organic water-soluble suspensions, emulsions, trays, fats, pastes and waxes.
- diamond-like carbon in particular the carbon structures described above, is the use as an electrical insulator.
- the diamond-like carbon structures can be used as a heat transfer medium. It is particularly advantageous if, in addition to the high electrical insulation capabilities, the properties for optimal transfer of thermal energy from one body to the other can be used. This is a typical task for lossy electronic components.
- the invention therefore describes an advantageous application of diamond-like carbon structures, predominantly in nano and micro grain areas as electrical insulating or thermal transfer agents. This is achieved by introducing the carbons into pastes, adhesives, lacquers, greases, solders and in composite material composites primarily for technical-industrial use in the areas of high-performance electronics, microelectronics, as well as electrical engineering and energetics.
- the active heat-emitting surface is currently being enlarged with the help of heat sinks.
- these high-performance components are not flat and therefore have a certain roughness, they are connected to the heat sink by means of a so-called heat-conducting medium.
- these media must have an extraordinarily high electrical insulation capacity and guarantee an optimal adaptation to the corresponding surface without, on the other hand, showing a flow behavior.
- the known media materials such as mica, aluminum oxide, boron nitrite or beryllium oxide have the disadvantage that some of them are highly toxic (for example beryllium oxide) and have a high specific thermal conductivity. This applies in particular to ceramic and polymeric film systems. Viscous systems such as pastes, greases, varnishes, adhesives etc. can usually not be applied during the manufacturing process of the electronic component to be cooled and are therefore difficult to handle.
- diamond-like carbon structures as an electrical insulator of heat transfer media leads to significantly improved characteristics and performance characteristics and ensures optimal processing with the appropriate media carrier in adaptation to the respective component.
- the material according to the invention represents an optimal electrical insulator and leads to the improvement of a number of other performance characteristics of the overall system, such as hardness, dielectric constant, breakdown voltage, specific density, tensile, fracture and push-through strength, elongation, loss factor and others.
- the material according to the invention can be doped in an application-specific manner and can be produced on a large scale and inexpensively.
- the technical reliability and availability as well as the performance of common electronic components can also be significantly increased through optimized power dissipation without design changes to the assemblies and components.
- diamond-like carbon structures in solid, highly disperse form or as a suspension, dispersion or emulsion.
- the carbon Structures on highly structured surfaces and shapes which in particular allow a targeted variation of the required crosslinking, suspending and dispersing properties in order to ensure optimal system characteristics.
- the chemical conversion of the energy source has to take place under conditions of a light vacuum (approx. 2 mm Hg), which is generated by an appropriate vacuum pump. The following process parameters must be observed:
- an atomic hydrogen-based low-temperature plasma is generated at 4,000 K:
- a water vapor plasma is generated via a water reservoir surrounding the energy carrier system under the influence of the process parameters (pressure, temperature, time) specified above.
- the thickness of the water reserve corresponds to three times the diameter of the cylindrical body of the energy source used.
- Process output (process yield) on diamond-like carbon structures according to the invention 10.43% (based on the mass of the energy carrier used)
- gas-liquid carrier mixtures such as, for example, ethylene / butane / propane in a volume ratio of 20/40/40 with a pressure level in the range from before the initiation of the chemical reaction 0.3 Mpa to 0.8 Mpa to be introduced or blown into the high pressure reactor system.
- liquid organic carbon donor systems of the aliphatic series such as limiting hydrocarbons or monohydric or polyhydric alcohols (for example ethylene glycol) in the form of a, are maintained while maintaining the above-described conditions for generating a low-temperature water vapor plasma supported by atomic hydrogen before initiating the chemical reaction Jacket inserted between the cylindrical body of the energy source and water reserve in the system.
- the mass (M ⁇ s ) of the carbon donor system can be determined as follows:
- M ⁇ s A x M / 100-A
- A % of the carbon donor system in the overall reaction system
- M mass of energy source + mass of carbon donor, where A (%) must be in the range from 13.8 to 15.1.
- This process step provides diamond-like carbon structures according to the invention with predominantly the following properties:
- Example 3 all parameters of Example 3 are retained and unsaturated alcohols (such as, for example, propargyl alcohol or allyl alcohol) or aromatic compounds (such as, for example, benzene, nitrobenzene or acetonitrile) are used as carbon donor systems.
- unsaturated alcohols such as, for example, propargyl alcohol or allyl alcohol
- aromatic compounds such as, for example, benzene, nitrobenzene or acetonitrile
- the value of A (%) to be used must be between 12.8 and 17.3.
- the resulting diamond-like carbon structures have the following characteristics:
- an aqueous slurry made of DLSC material (for example manufactured with the technology levels of Examples 1 to 4) and 5 to 8% water (deionized) is established in the high-pressure reactor unit in the form of a casing of the cylindrical energy carrier system.
- the mass of the slurry system must be at least 1.35 times the mass of the energy source.
- the resulting diamond-like carbon structures are in polycrystalline form (PK-DLSC) with typically spread X-ray pattern peaks at (1 1 1), (220) and (31 1).
- the X-ray pattern is in Figure 6 shown.
- the crystallite sizes are in the range from 5 to 20 nm and are correspondingly polycrystallized via sp 3 hybridization.
- the polycrystals thus present with a 100% purity of the cubic crystal lattice phase move in grain size ranges from approximately 0.5 ⁇ m to 15 ⁇ m, a median of 3.43 ⁇ m and standard deviations of less than 2.41 ⁇ m being achieved can be.
- FIG. 7 shows the grain size distribution diagram. The process output of this technological process is approximately 50%.
- the so-called DLSC materials described in mono- and polycrystalline form represent a new generation of highly structured carbon systems, the general characteristics and performance characteristics of which correspond to the cubic crystal lattice phase of pure diamond and, moreover, a number of specific, chemical-physical and, above all, doped have variable properties.
- the present material thus allows relevant technical interfaces for the transition to hyperstructured from a morphological point of view Realize carbon systems, in particular to fullerene, hyper-fullerene in the form of onion-like carbons and nano-tubes.
- the material can be used both in its own form and in combination with other materials (composites), compared to known substances and conventional substances, especially for the application fields listed below:
- the DLSC For the surface treatment of hard and super-hard materials, the DLSC must be entered in specially designed carrier media. This is illustrated using the following examples:
- Aqueous suspensions of sprays based on cationic short-chain suspending aids with degrees of polymerization from approx. 100 to 5,000.
- Carrier / blowing agent polyglycol, propane, butane
- Carrier / blowing agent - as (3) -
- Thermal management systems as foils, adhesives, potting compounds, pastes, solders, tapes
- Abrasive and tribological systems as suspensions, emulsions, waxes, sprays, desiccants ...
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10081682T DE10081682D2 (de) | 1999-06-18 | 2000-06-14 | Verfahren zur dynamisch-chemischen Herstellung von diamantartigen Kohlenstoffstrukturen, diamantartige Kohlenstoffstrukturen und Verwendungen von diamantartigen Kohlenstoffstrukturen |
AU59644/00A AU5964400A (en) | 1999-06-18 | 2000-06-14 | Method for the chemodynamic production of diamond-type carbon structures, diamond-type carbon structures and uses of diamond-type carbon structures |
EP00945626A EP1194373A1 (de) | 1999-06-18 | 2000-06-14 | Verfahren zur dynamisch-chemischen herstellung von diamantartigen kohlenstoffstrukturen, diamantartige kohlenstoffstrukturen und verwendungen von diamantartigen kohlenstoffstrukturen |
JP2001504849A JP2003502266A (ja) | 1999-06-18 | 2000-06-14 | ダイアモンド状の炭素構造の動的化学的製造方法、ダイアモンド状の炭素構造、ダイアモンド状の炭素構造の使用 |
Applications Claiming Priority (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19927895 | 1999-06-18 | ||
DE19927893 | 1999-06-18 | ||
DE19927894.6 | 1999-06-18 | ||
DE19927894 | 1999-06-18 | ||
DE19927895.4 | 1999-06-18 | ||
DE19927893.8 | 1999-06-18 | ||
DE19955971.6 | 1999-11-19 | ||
DE19955971A DE19955971A1 (de) | 1999-06-18 | 1999-11-19 | Verfahren zur dynamisch-chemischen Herstellung von diamantartigen Kohlenstoffstrukturen, diamantartige Kohlenstoffstrukturen und Verwendungen von diamantartigen Kohlenstoffstrukturen |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2000078674A1 true WO2000078674A1 (de) | 2000-12-28 |
Family
ID=27438966
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/DE2000/001885 WO2000078674A1 (de) | 1999-06-18 | 2000-06-14 | Verfahren zur dynamisch-chemischen herstellung von diamantartigen kohlenstoffstrukturen, diamantartige kohlenstoffstrukturen und verwendungen von diamantartigen kohlenstoffstrukturen |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP1194373A1 (de) |
JP (1) | JP2003502266A (de) |
CN (1) | CN1368936A (de) |
AU (1) | AU5964400A (de) |
DE (1) | DE10081682D2 (de) |
WO (1) | WO2000078674A1 (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014076910A (ja) * | 2012-10-09 | 2014-05-01 | Sumitomo Electric Ind Ltd | ダイヤモンド多結晶体およびその製造方法、ならびに工具 |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101373640B1 (ko) | 2011-06-06 | 2014-03-12 | 노부오 오마에 | 양파 모양 카본의 제작 방법 |
CN106573212B (zh) * | 2014-05-28 | 2020-10-27 | 晶胞金刚石有限责任公司 | 组合合成金刚石晶胞和金刚石块 |
Citations (6)
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US4767608A (en) * | 1986-10-23 | 1988-08-30 | National Institute For Research In Inorganic Materials | Method for synthesizing diamond by using plasma |
WO1990005701A1 (en) * | 1988-11-16 | 1990-05-31 | Andrew Carey Good | Diamond production |
DE4038190A1 (de) * | 1989-12-11 | 1991-06-13 | Gen Electric | Einkristalliner diamant sehr hoher thermischer leitfaehigkeit |
JPH04333599A (ja) * | 1991-05-09 | 1992-11-20 | Tokyo Daiyamondo Kogu Seisakusho:Kk | 超微粒子ダイヤモンド共析被膜を施した機器 |
JPH0558784A (ja) * | 1991-09-02 | 1993-03-09 | Toyota Central Res & Dev Lab Inc | ダイヤモンドの析出方法 |
TW224076B (en) * | 1992-03-05 | 1994-05-21 | Nat Science Committee | A gas phase reaction method to synthesize high quality diamond membrane at low temperature |
-
2000
- 2000-06-14 JP JP2001504849A patent/JP2003502266A/ja active Pending
- 2000-06-14 AU AU59644/00A patent/AU5964400A/en not_active Abandoned
- 2000-06-14 DE DE10081682T patent/DE10081682D2/de not_active Expired - Fee Related
- 2000-06-14 EP EP00945626A patent/EP1194373A1/de not_active Withdrawn
- 2000-06-14 WO PCT/DE2000/001885 patent/WO2000078674A1/de not_active Application Discontinuation
- 2000-06-14 CN CN00811524A patent/CN1368936A/zh active Pending
Patent Citations (6)
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US4767608A (en) * | 1986-10-23 | 1988-08-30 | National Institute For Research In Inorganic Materials | Method for synthesizing diamond by using plasma |
WO1990005701A1 (en) * | 1988-11-16 | 1990-05-31 | Andrew Carey Good | Diamond production |
DE4038190A1 (de) * | 1989-12-11 | 1991-06-13 | Gen Electric | Einkristalliner diamant sehr hoher thermischer leitfaehigkeit |
JPH04333599A (ja) * | 1991-05-09 | 1992-11-20 | Tokyo Daiyamondo Kogu Seisakusho:Kk | 超微粒子ダイヤモンド共析被膜を施した機器 |
JPH0558784A (ja) * | 1991-09-02 | 1993-03-09 | Toyota Central Res & Dev Lab Inc | ダイヤモンドの析出方法 |
TW224076B (en) * | 1992-03-05 | 1994-05-21 | Nat Science Committee | A gas phase reaction method to synthesize high quality diamond membrane at low temperature |
Non-Patent Citations (13)
Title |
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BUERKI P R ET AL: "CO2-LASER-INDUCED VAPOR-PHASE SYNTHESIS OF HN-DIAMOND NANOPARTICLESAT 0.6 - 2 BAR", NANOSTRUCTURED MATERIALS,US,PERGAMON PRESS, TARRYWOOD, NY, vol. 4, no. 5, 1 September 1994 (1994-09-01), pages 577 - 582, XP000460804, ISSN: 0965-9773 * |
DATABASE CHEMABS [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; FEDOSEEV, D. V. ET AL: "Diamond-like films deposition from the mixtures of cyclohexane with argon in low temperature plasma", XP002151878, retrieved from STN Database accession no. 126:11820 CA * |
DATABASE CHEMABS [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; FEDOSEEV, D. V. ET AL: "Effect of ion flux on the growth of diamond-like films in a low-temperature plasma", XP002151876, retrieved from STN Database accession no. 128:161101 CA * |
DATABASE CHEMABS [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; FEDOSEEV, D. V. ET AL: "Growth and properties of diamond-like films deposited from cyclohexane-argon mixtures in low-temperature plasma", XP002151877, retrieved from STN Database accession no. 126:134622 CA * |
DATABASE CHEMABS [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; MARUYAMA, KATSUHISA ET AL: "Synthesis of cubic diamond by hydrogen plasma jet", XP002151879, retrieved from STN Database accession no. 116:111974 CA * |
DATABASE WPI Section Ch Week 199301, Derwent World Patents Index; Class M11, AN 1993-005087, XP002151880 * |
DATABASE WPI Section Ch Week 199315, Derwent World Patents Index; Class E36, AN 1993-121190, XP002151881 * |
DATABASE WPI Section Ch Week 199425, Derwent World Patents Index; Class E36, AN 1994-208076, XP002151882 * |
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KOGAI SHIGEN KENKYUSHO IHO (1991), 21(1), 23-30, 1991 * |
YOSHIKAWA M ET AL: "RAMAN SCATTERING FROM NANOMETER-SIZED DIAMOND", APPLIED PHYSICS LETTERS,US,AMERICAN INSTITUTE OF PHYSICS. NEW YORK, vol. 67, no. 5, 31 July 1995 (1995-07-31), pages 694 - 696, XP000520546, ISSN: 0003-6951 * |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014076910A (ja) * | 2012-10-09 | 2014-05-01 | Sumitomo Electric Ind Ltd | ダイヤモンド多結晶体およびその製造方法、ならびに工具 |
Also Published As
Publication number | Publication date |
---|---|
EP1194373A1 (de) | 2002-04-10 |
AU5964400A (en) | 2001-01-09 |
CN1368936A (zh) | 2002-09-11 |
DE10081682D2 (de) | 2002-07-25 |
JP2003502266A (ja) | 2003-01-21 |
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