WO2005001155A1 - SINTERKÖRPER AUS ZnO - Google Patents
SINTERKÖRPER AUS ZnO Download PDFInfo
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- WO2005001155A1 WO2005001155A1 PCT/EP2004/006992 EP2004006992W WO2005001155A1 WO 2005001155 A1 WO2005001155 A1 WO 2005001155A1 EP 2004006992 W EP2004006992 W EP 2004006992W WO 2005001155 A1 WO2005001155 A1 WO 2005001155A1
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- Prior art keywords
- zinc oxide
- sintered body
- weight
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C04B2235/3287—Germanium oxides, germanates or oxide forming salts thereof, e.g. copper germanate
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- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
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- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
- C04B2235/445—Fluoride containing anions, e.g. fluosilicate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Definitions
- the present invention relates to an electrically conductive doped sintered body made of zinc oxide (ZnO), a process for its production and its use, in particular as a sputtering target for the production of electrically highly conductive transparent layers, so-called TCO layers (transparent conductive oxide layers).
- ZnO zinc oxide
- TCO layers transparent conductive oxide layers
- Such layers have transparency in the visible light range and z.
- B. as transparent electrodes for EL (electroluminescence) display devices and liquid crystal display devices and plasma luminescence devices, used as electrode films for solar cells and all types of light-receiving elements. They are also widely used in layer systems for heat-reflecting films for automobiles and buildings, as antistatic films for photomasks or as transparent heating elements for various anti-fogging devices, including freezer showcases. In addition, they are useful as substrates for electrochromic devices such as light control glass.
- DE-T-689 19 299 discloses a zinc oxide sintered body which contains 0.1 to 20% by weight of an oxide of an at least positive trivalent element, based on the amount of zinc oxide, and a sintered density of at least 5 g / cm 3 and has a specific resistance of less than 1 ⁇ ⁇ cm. If this sintered body is used as a sputtering target for the production of TCO layers, then the so obtained However, layers of an unsatisfactory concentration of charge carriers for various applications.
- the object of the present invention is therefore to provide a sintered body based on zinc oxide, from which TCO layers can be deposited by sputtering, which do not have the disadvantages of the layers known in the prior art.
- layers with improved electrical properties compared to the prior art are sought.
- the object is achieved according to the invention by a zinc oxide sintered body containing a) 0.1 to 20% by weight of an oxide of an at least trivalent positively charged metal, and b) 0.1 to 20% by weight of a - different from a) Oxides of at least trivalent positively charged metal, and / or c) at least 0.05% by weight of a monovalent negatively charged element, each based on the weight of zinc oxide.
- the zinc oxide sintered body according to the invention has a sintered density of at least 5 g / cm 3 .
- the ZnO sintered body according to the invention is therefore doped with the constituents a) and b), a) and c) or a), b) and c). These components / doping elements will be explained in more detail below. Components a) and b)
- An at least trivalent positively charged metal is a metal cation, the valence of which is three or higher.
- the oxides of the at least trivalent positively charged metals are oxides of the elements from groups IIIA to VIIA and IIIB to VIIIB of the Periodic Table of the Elements (PSE) and oxides of the lanthanides.
- Examples are the oxides of B, Al, Ga, In, Tl (group purple of the PSE), Si, Ge, Sn, Pb (group IVa of the PSE), As, Sb, Bi (group Va of the PSE), Se, Te (Group Via des PSE), Sc, Y, La, (group Illb des PSE), Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu (lanthanoids), Ti , Zr, Hf (group IVb of the PSE), V, Nb, Ta (group Vb of the PSE), Cr, Mo, W (group VIb of the PSE), Mn, Re (group Vllb of the PSE), and the oxides of Fe , Ru, Os, Co, Rh, Ir, Ni, Pd, Pt (Group VHIb of the PSE).
- a component of components a) and b) is preferably selected from the group of the oxides of Al, Ga, In, Sn, Si, Ge, Zr and Ti, components a) and b) being different. Both components a) and b) are particularly preferably selected from this group, components a) and b) differing.
- the preferred amount of constituents a) and b) is, independently of one another, 0.1 to 5.0% by weight, based on the weight of zinc oxide. Both constituents a) and b) are particularly preferably present in an amount of 0.1 to 5.0% by weight, based on the weight of zinc oxide.
- Component c) is a monovalent negatively charged element. It is an anion of an element from group VIIA of the PSE. Examples are F, Cl, Br or I, with fluorine being particularly preferred.
- the component c) is fed to the sintered body in the form of a chemical compound which contains the anion and at least one cation, in particular a metal cation.
- the cation of the compound is preferably an element of constituents a) or b) and preferably Zn 2+ or Al 3+ .
- a particularly preferred compound is AIF3.
- the compound of component c) may have other components, for example an oxygen fraction.
- An example of such compounds is AlO x F y .
- the component c) is either added to the components a) and b) or replaces the component b). It preferably replaces component b).
- Component c) is preferably present in an amount of at least 0.1% by weight, based on the weight of zinc oxide.
- the ZnO sintered bodies according to the invention are preferably doped with two constituents, ie they contain either constituents a) and b) or constituents a) and c).
- the invention also relates to the use of a zinc oxide sintered body according to the invention as a sputtering target for the production of electrically conductive, transparent layers.
- the layers obtainable in this way have improved electrical properties compared to the layers known in the prior art.
- Both the medium-frequency sputtering technique and the direct current sputtering technique can be used to produce the layers.
- the ZnO sintered body of the present invention is used, the discharge process is stable in each of the sputtering methods, and transparent electrically conductive layers are obtained which have a very low resistance and have excellent transparency.
- the ZnO sintered body according to the invention can be produced by conventional processes known to the person skilled in the art, for example by the process described in DE-T-689 19 299.
- the doping elements a) and b) can be dispersed both mechanically and chemically, for example by co-precipitating corresponding starting compounds.
- two variants can be traced for the production of the ZnO sintered body according to the invention: According to a first variant, component c) is already present in a ZnO green body before sintering, while component c) in the second variant is only present in the ZnO during sintering -Green body is introduced.
- a green body containing component c) can be produced, for example, using chemical precipitation procedures. For example, a suspension of ZnO grains and a soluble aluminum salt is formed. By adding hydrofluoric acid Aluminum fluoride precipitated, which attaches to the ZnO grains. These ZnO grains provided with aluminum fluoride are then dried and pressed into a ceramic molded part, a so-called green body.
- the green body is placed in a closable sintering vessel.
- the sintered vessel also has its own material and a portion of component c).
- the sintering takes place under pressure and temperature conditions at which the additional component c) changes into the gas phase and prevents the component c) from evaporating, i.e. prevents the component c) already introduced into the green body from escaping from the sintered body.
- the production method according to the second variant is preferred over the first variant and is also the subject of the present invention.
- ZnO is sintered in the presence of the constituents / doping elements a), b) or / and c) at a temperature and a pressure, ie heated to a certain temperature for a certain duration.
- the sintering temperature and the pressure are selected such that a certain proportion of at least one of the components a), b) or / and c) is in gaseous form, the doping element c) preferably being volatile at this temperature and the gas phase being enriched with the doping element c) is.
- the gas space surrounding the sintered body is preferably separated from the surrounding furnace atmosphere by a closable sintered vessel, so that the concentration of the doping elements in the gas phase in the sintered vessel is higher than in the surrounding furnace space.
- This method is preferably used for doping with component c).
- the starting point is a green body that contains only the components a) or a) and b) in addition to ZnO, but not the component c).
- the green body is placed in a closable sintered vessel, in which, in addition to the green body, there is also material of its own type and a portion of component c).
- the sintering is preferably carried out under pressure and temperature conditions in which the additional component c) present in the gas phase diffuses into the green body during the sintering.
- the additional component c) thus serves as a diffusion source for doping the sintered body with the component c), while during the sintering in the first method variant it merely serves as an outlet for the component c already previously introduced into the green body ) prevented.
- the production of a ZnO sintered body according to the invention by means of the method according to the second variant is described below.
- the starting point is a green body that contains only Al 3+ , for example in the form of Al2O3, but no fluorine ions, in addition to ZnO.
- the green body is embedded in a powder made of burnt ZnO, which is located in a closable crucible made of AI2O3.
- the ZnO powder is enriched with AIF3, the AIF3 being present in an amount of approximately 5% by weight based on the amount of the powdered ZnO. In addition to the AIF3, there is also a small amount of AI2O3 in the crucible.
- Sintering takes place over a period of five hours at normal pressure and at a sintering temperature of 1300 ° C to 1400 ° C.
- the fluorine present in the gas phase in the form of AIF3 or HF diffuses into the green body during sintering.
- Al 3+ and F- are installed in the ZnO grid.
- the result of the sintering process is a ZnO sintered body according to the invention which contains Al 3+ and F- in the ZnO lattice.
- the sintered body can contain a proportion of Al 2 O 3 which is present in an amount of less than about 10% by weight, based on the mass of the zinc oxide.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
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Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE2003129338 DE10329338A1 (de) | 2003-06-30 | 2003-06-30 | Sinterkörper aus ZnO |
DE10329338.8 | 2003-06-30 |
Publications (1)
Publication Number | Publication Date |
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WO2005001155A1 true WO2005001155A1 (de) | 2005-01-06 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/EP2004/006992 WO2005001155A1 (de) | 2003-06-30 | 2004-06-28 | SINTERKÖRPER AUS ZnO |
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DE (1) | DE10329338A1 (de) |
WO (1) | WO2005001155A1 (de) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2194158A1 (de) * | 2007-09-27 | 2010-06-09 | Mitsubishi Materials Corporation | ZnO-AUFDAMPFUNGSMATERIAL, HERSTELLUNGSVERFAHREN DAFÜR UND ZnO-SCHICHT |
CN102534501A (zh) * | 2012-03-29 | 2012-07-04 | 山东理工大学 | 太阳电池用共掺杂氧化锌透明导电薄膜的制备方法 |
WO2019068807A1 (de) * | 2017-10-04 | 2019-04-11 | Ceramtec Gmbh | Teilstabilisierter zirkonoxid-werkstoff mit hoher sinteraktivität |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH06128743A (ja) * | 1992-09-04 | 1994-05-10 | Mitsubishi Materials Corp | 透明導電膜とその製造方法およびそれに用いるターゲット |
JPH06293956A (ja) * | 1993-04-06 | 1994-10-21 | Japan Energy Corp | 酸化亜鉛系透明導電膜及びその作製法並びにそれに使用するスパッタリングターゲット |
JPH11171539A (ja) * | 1997-12-08 | 1999-06-29 | Sumitomo Metal Mining Co Ltd | ZnO系焼結体およびその製法 |
US6146765A (en) * | 1994-08-17 | 2000-11-14 | Asahi Glass Company Ltd. | Transparent conductive film and method for its production, and sputtering target |
EP1063317A1 (de) * | 1998-03-05 | 2000-12-27 | Asahi Glass Company Ltd. | Sputtertarget, transparenter leitender film und verfahren zu dessen herstellung |
EP1211679A1 (de) * | 1999-08-12 | 2002-06-05 | Nikko Materials Company, Limited | Lichtdurchlassende schicht und sputtertarget zur herstellung dieser schicht |
WO2004075212A1 (de) * | 2003-02-19 | 2004-09-02 | GfE Gesellschaft für Elektrometallurgie mbH | Pvd-beschichtungsmaterial |
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2003
- 2003-06-30 DE DE2003129338 patent/DE10329338A1/de not_active Ceased
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2004
- 2004-06-28 WO PCT/EP2004/006992 patent/WO2005001155A1/de active Application Filing
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06128743A (ja) * | 1992-09-04 | 1994-05-10 | Mitsubishi Materials Corp | 透明導電膜とその製造方法およびそれに用いるターゲット |
JPH06293956A (ja) * | 1993-04-06 | 1994-10-21 | Japan Energy Corp | 酸化亜鉛系透明導電膜及びその作製法並びにそれに使用するスパッタリングターゲット |
US6146765A (en) * | 1994-08-17 | 2000-11-14 | Asahi Glass Company Ltd. | Transparent conductive film and method for its production, and sputtering target |
JPH11171539A (ja) * | 1997-12-08 | 1999-06-29 | Sumitomo Metal Mining Co Ltd | ZnO系焼結体およびその製法 |
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EP2194158A1 (de) * | 2007-09-27 | 2010-06-09 | Mitsubishi Materials Corporation | ZnO-AUFDAMPFUNGSMATERIAL, HERSTELLUNGSVERFAHREN DAFÜR UND ZnO-SCHICHT |
US20100243966A1 (en) | 2007-09-27 | 2010-09-30 | Mitsubishi Materials Corporation | ZnO VAPOR DEPOSITION MATERIAL, PROCESS FOR PRODUCING THE SAME, AND ZnO FILM |
EP2194158A4 (de) * | 2007-09-27 | 2011-07-27 | Mitsubishi Materials Corp | ZnO-AUFDAMPFUNGSMATERIAL, HERSTELLUNGSVERFAHREN DAFÜR UND ZnO-SCHICHT |
US8231812B2 (en) | 2007-09-27 | 2012-07-31 | Mitsubishi Materials Corporation | ZnO vapor deposition material, process for producing the same, and ZnO film |
EP2508497A1 (de) * | 2007-09-27 | 2012-10-10 | Mitsubishi Materials Corporation | ZnO-Aufdampfungsmaterial, Verfahren zu dessen Herstellung |
US8409477B2 (en) | 2007-09-27 | 2013-04-02 | Mitsubishi Materials Corporation | ZnO vapor deposition material, process for producing the same, and ZnO film |
CN102534501A (zh) * | 2012-03-29 | 2012-07-04 | 山东理工大学 | 太阳电池用共掺杂氧化锌透明导电薄膜的制备方法 |
WO2019068807A1 (de) * | 2017-10-04 | 2019-04-11 | Ceramtec Gmbh | Teilstabilisierter zirkonoxid-werkstoff mit hoher sinteraktivität |
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