EP2935151A1 - Matériau céramique - Google Patents
Matériau céramiqueInfo
- Publication number
- EP2935151A1 EP2935151A1 EP13811508.4A EP13811508A EP2935151A1 EP 2935151 A1 EP2935151 A1 EP 2935151A1 EP 13811508 A EP13811508 A EP 13811508A EP 2935151 A1 EP2935151 A1 EP 2935151A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- ppm
- ceramic material
- ceramic
- material according
- impurities
- 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.)
- Withdrawn
Links
- 229910010293 ceramic material Inorganic materials 0.000 title claims description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 28
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims description 9
- 150000004706 metal oxides Chemical class 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 229910052566 spinel group Inorganic materials 0.000 claims description 4
- 229910003023 Mg-Al Inorganic materials 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 2
- 239000002994 raw material Substances 0.000 abstract description 21
- 238000000034 method Methods 0.000 description 19
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 11
- 229910001701 hydrotalcite Inorganic materials 0.000 description 11
- 229960001545 hydrotalcite Drugs 0.000 description 11
- 239000002245 particle Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
- 239000011324 bead Substances 0.000 description 5
- KLOIYEQEVSIOOO-UHFFFAOYSA-N carbocromen Chemical compound CC1=C(CCN(CC)CC)C(=O)OC2=CC(OCC(=O)OCC)=CC=C21 KLOIYEQEVSIOOO-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000004108 freeze drying Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- -1 however Substances 0.000 description 4
- 229910000000 metal hydroxide Inorganic materials 0.000 description 4
- 150000004692 metal hydroxides Chemical class 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000004815 dispersion polymer Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
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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
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- C04B2235/9653—Translucent or transparent ceramics other than alumina
Definitions
- the invention relates to ceramic materials;
- the invention relates to ceramic materials for the production of transparent ceramics.
- Transparent ceramics and their preparation are known from the prior art.
- DE 10 2004 004 259 B3 discloses a polycrystalline ceramic with a high mechanical load capacity, which has a true in-line transmission (RIT) of more than 75% of the theoretical maximum value for a 0.8 mm thick polished disk and at wavelengths between 600 and 650 nm, wherein the mean grain size D is in the range between 60 nm and 10 ⁇ .
- RIT true in-line transmission
- polycrystalline ceramic disks The transparency of polycrystalline ceramic disks is influenced by various factors. So of course, a material must be used that has only a very low light absorption. In addition, the transparency of polycrystalline ceramic discs depends essentially on the light scattering, which results from the crystal structure on the one hand and from the microstructure of the ceramic body on the other hand. Materials with cubic crystal systems are preferably used because birefringence does not occur. Furthermore, the processes for the production of transparent ceramics are optimized in such a way that the lowest possible porosity occurs, or the pore size is below the wavelength of the light, in order to minimize the light scattering at phase boundaries.
- the object of the invention is thus to provide alternative ceramic materials which are suitable for the production of transparent ceramics and which are less expensive than the high purity raw materials known in the art.
- This ceramic material is characterized in that it consists of metal oxides, which are obtained by calcination of hydrotalcites.
- the material can preferably be used to produce transparent ceramics.
- Hydrotalcites according to the invention are metal hydroxides prepared by a hydrotalcite process.
- a transparent ceramic according to the invention is understood to mean a ceramic which has an RIT of at least 40% at 300 nm, 600 nm and / or 1500 nm wavelength of the light. Theoretically, the transparency is independent of thickness, if a perfect material is present and from it a perfect ceramic was produced. As soon as the ceramic, however, pores o.ä. contains a scattering effect at the phase boundaries of the pores, which becomes stronger with increasing thickness of the ceramic. This effect leads to a decreasing transparency. Therefore, referred to in this document transparencies refer to ceramics with wall thicknesses between 50 ⁇ and 100 mm.
- the hydrotalcites, from which the ceramic material according to the invention is obtained by calcining are produced by means of a hydrotalcite process.
- Hydrotalcite processes are known in the art. Such a method is described for example in EP 0 807 086 B1.
- a hydrotalcite process in the context of this invention is understood as meaning a process which comprises at least the following steps:
- the metal oxides which are obtained by calcination from the metal hydroxides between 100 and 500 ppm, preferably between 100 and 200 ppm impurities, in particular of Fe, Mn, Cr, V, Zn, Sn, Ti, Si, Zr, Ca, Na, K, Li, Y, Ni, Co, Cu.
- impurities in particular of Fe, Mn, Cr, V, Zn, Sn, Ti, Si, Zr, Ca, Na, K, Li, Y, Ni, Co, Cu.
- the higher level of contamination is possible because the impurities are very finely divided and very homogeneous, possibly at the atomic level, present in the material. In any case, they do not form a separate phase, for example a grain boundary phase, which would lead to a reduction in transparency in the sintered ceramic. It is believed that the impurities are incorporated in the lattice of metal oxides. This means the incorporation of the metal cations in the lattice of the spinel, for example, cation lattice, interstitial sites, or the like.
- transparent ceramics can be produced with the raw material according to the invention which have a deviation in the RIT value of ⁇ 10% between 300 nm and 700 nm, in particular at 300 nm and 700 nm, and thus obtain a high white value.
- metal hydroxides whose metal oxides have a cubic crystal system.
- oxides like the Al 2 O 3 or MgO particularly preferably spinels, in particular Mg-Al spinels are produced.
- transparent ceramics of ZrO 2 oxides of mixtures of Y and Al and materials of the mixtures of Al, N, O or even non-cubic aluminum oxide can preferably be produced by this process.
- the use of the material according to the invention completely dispenses with the use of sintering aids.
- Sintering aids allow the use of lower sintering temperatures with less grain growth.
- the sintering aids must be at least partially expelled again by means of volatile compounds such as LiF, since they would otherwise be present as a separate phase in the ceramic, which in turn would have negative effects on the transparency.
- volatile compounds such as LiF
- Diammonium hydrogen citrate stirred is ground with a stirred ball mill (500 m Al 2 O 3 grinding beads) until an energy input of 1.60 kWh / kg is reached.
- the following particle size distribution is then available: d90: 375 nm, d50: 224 nm, d10: 138 nm (measured with a Nanoflex measuring instrument from Microtrac).
- the specific surface area (BET) is 25.5 m 2 / g.
- the thus prepared slurry is mixed with 6% of a short-chain polyethylene glycol and granulated by means of a freeze-spray process. After this
- the samples are ground and polished to a thickness of 2 mm for a transmission measurement:
- the treatment is carried out analogously to Example 1 until an energy input of 1.05 kWh / kg is reached.
- the following particle size distribution is then present: d90: 345 nm, d50: 195 nm, d10: 124 nm (measured with a Nanoflex measuring instrument from Microtrac), BET 23.5 m 2 / g.
- the thus prepared slurry is mixed with 6% of a short-chain polyethylene glycol and granulated by means of a freeze-spray process. After this
- Freeze-drying is a moldable granulate from which test pieces are formed having a net basis of 2.07 g / cm 3 . These are pre-sintered at 1400 ° C for 2 h at 3.512 g / cm 3 and then post-densified at 1650 ° C for 6 h at 200 MPa hot isostatic.
- the samples are ground and polished to a thickness of 2 mm for a transmission measurement:
- Example 3 A MgOAl 2 O 3 raw material with 156 ppm impurities, which was produced by the hydrotalcite process and has the following composition (ICP analysis), is used:
- 600 g of the raw material are added to 600 g of deionized water at 4.7%
- Diammonium hydrogen citrate stirred is ground with a stirred ball mill (500 m Al 2 O 3 grinding beads) until an energy input of 1.5 kWh / kg is reached.
- the specific surface area (BET) is then 51.3 m 2 / g.
- the thus prepared slip is admixed with 5% of an aqueous polymer dispersion and 4% of a fatty acid preparation and granulated by means of a freeze spray method. After freeze-drying, there is a moldable granule from which test pieces having a net basis of 2.18 g / cm 3 are formed. These are pre-sintered at 1550 ° C for 2 h to 3.413 g / cm 3 and then post-densified at 1650 ° C for 6 h at 200 MPa hot isostatic.
- the samples are ground and polished to a transmission measurement of 2 mm thickness: The following RIT values were determined as a function of the wavelength: 300 nm: 70%, 600 nm: 75%, 700 nm: 77%, 1500 nm: 79%.
- the compacts produced with a net comparable green density of 1 89 g / cm 3 are at 1430 ° C for 2 h to 3.524 g / cm 3 pre-sintered and then hot isostatic pressed at 1650 ° C, for 6 hours at 200 MPa.
- the samples are ground and polished to a thickness of 2 mm for a transmission measurement: no RIT values can be measured.
- the samples are ground and polished to a thickness of 2 mm for a transmission measurement: no RIT values can be measured.
- the samples are
- Freeze-drying is a moldable granulate, are formed from the sample with a net green density of 1, 91 g / cm 3 . These are pre-sintered at 1530 ° C for 2 h at 3.057 g / cm 3 and then post-densified at 1650 ° C for 4 h at 200 MPa hot isostatic.
- the samples are ground and polished to a thickness of 2 mm for a transmission measurement:
- the slip is granulated as described in Example 5.
- the comparatively produced compacts having a net green density of 1.87 g / cm 3 are pre-sintered at 1410 ° C. for 2 h to 3.452 g / cm 3 and then hot isostatically compressed at 1650 ° C. for 6 h at 200 MPa.
- the samples are ground and polished to a thickness of 2 mm for a transmission measurement: no RIT values can be measured.
- the samples are ground and polished to a thickness of 2 mm for a transmission measurement: no RIT values can be measured.
- the samples are
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- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
L'invention concerne la production de céramiques transparentes. Elle concerne en particulier l'utilisation de matières premières contenant des impuretés pour la production de céramiques transparentes.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102012223802 | 2012-12-19 | ||
| PCT/EP2013/077304 WO2014096142A1 (fr) | 2012-12-19 | 2013-12-19 | Matériau céramique |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP2935151A1 true EP2935151A1 (fr) | 2015-10-28 |
Family
ID=49876628
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP13811508.4A Withdrawn EP2935151A1 (fr) | 2012-12-19 | 2013-12-19 | Matériau céramique |
Country Status (10)
| Country | Link |
|---|---|
| US (2) | US20150299044A1 (fr) |
| EP (1) | EP2935151A1 (fr) |
| JP (1) | JP2016500362A (fr) |
| KR (1) | KR20150097714A (fr) |
| CN (1) | CN105263885A (fr) |
| AU (1) | AU2013360718A1 (fr) |
| DE (1) | DE102013226579A1 (fr) |
| IL (1) | IL239343A0 (fr) |
| RU (1) | RU2015129336A (fr) |
| WO (1) | WO2014096142A1 (fr) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013068576A1 (fr) * | 2011-11-10 | 2013-05-16 | Ceramtec-Etec Gmbh | Procédé pour produire des objets en céramique transparente par granulation en lit fluidisé |
| WO2015144717A1 (fr) | 2014-03-28 | 2015-10-01 | Ceramtec Gmbh | Platine et/ou corps de refroidissement translucide, muni d'une led |
| JP6845645B2 (ja) * | 2016-09-26 | 2021-03-24 | タテホ化学工業株式会社 | 酸化マグネシウム含有スピネル粉末及びその製造方法 |
| US20230357086A1 (en) * | 2019-05-14 | 2023-11-09 | Calix Ltd | A System and Method for the Production of High Strength Materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4396595A (en) * | 1982-02-08 | 1983-08-02 | North American Philips Electric Corp. | Method of enhancing the optical transmissivity of polycrystalline alumina bodies, and article produced by such method |
| JPH0672045B2 (ja) * | 1988-07-05 | 1994-09-14 | 住友電気工業株式会社 | 透光性スピネル焼結体及びその製造方法 |
| DE19503522A1 (de) * | 1995-02-03 | 1996-08-08 | Rwe Dea Ag | Herstellung gemischter schichtförmig aufgebauter Metallhydroxide sowie deren Metalloxide |
| CN1049881C (zh) * | 1995-12-15 | 2000-03-01 | 国家建筑材料工业局人工晶体研究所 | 一种透明多晶尖晶石的制备方法 |
| JP3783445B2 (ja) * | 1999-01-29 | 2006-06-07 | 住友化学株式会社 | 透光性アルミナ焼結体の製造方法およびその用途 |
| CA2308933C (fr) * | 1999-05-19 | 2008-07-22 | Ngk Spark Plug Co., Ltd. | Ceramique polycristalline translucide et methode de fabrication |
| JP3440299B2 (ja) * | 2000-11-15 | 2003-08-25 | 独立行政法人物質・材料研究機構 | 透明スピネル焼結体の製造法 |
| DE102004004259B3 (de) | 2004-01-23 | 2005-11-24 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Transparente polykristalline Sinterkeramik kubischer Kristallstruktur |
| US8133051B2 (en) * | 2004-08-27 | 2012-03-13 | Tosoh Corporation | Orthodontic bracket and process for producing the same |
| JP2006273679A (ja) * | 2005-03-30 | 2006-10-12 | Sumitomo Electric Ind Ltd | スピネル焼結体、光透過窓および光透過レンズ |
| JP4830911B2 (ja) * | 2007-03-02 | 2011-12-07 | 住友電気工業株式会社 | スピネル焼結体、その製造方法、透明基板と液晶プロジェクター |
| FR2917404B1 (fr) * | 2007-06-15 | 2009-09-04 | Saint Gobain Ct Recherches | Produit fritte de structure cubique. |
| JP2009126749A (ja) * | 2007-11-26 | 2009-06-11 | Sumitomo Electric Ind Ltd | 透明多結晶スピネル基板とその製造方法および前記基板を用いた光学製品 |
| US8268286B2 (en) * | 2008-11-06 | 2012-09-18 | General Electric Company | High strength, fine grained spinel for window applications, methods of manufacture thereof and articles comprising the same |
| EP2808313B1 (fr) * | 2008-11-18 | 2018-05-02 | Tosoh Corporation | Corps fritté d'alumine colorée à haute ténacité et translucidité élevée, son procédé de production et ses utilisations |
| JP5435397B2 (ja) * | 2009-04-02 | 2014-03-05 | 住友電気工業株式会社 | スピネル製光透過用窓材及びその製造方法 |
| DE102009046036B4 (de) * | 2009-10-27 | 2014-02-13 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Herstellung von redispergierbaren hochreinen Nanospinellpulvern und redispergierbares hochreines Nanospinellpulver |
-
2013
- 2013-12-19 KR KR1020157019331A patent/KR20150097714A/ko not_active Withdrawn
- 2013-12-19 AU AU2013360718A patent/AU2013360718A1/en not_active Abandoned
- 2013-12-19 CN CN201380067388.0A patent/CN105263885A/zh active Pending
- 2013-12-19 WO PCT/EP2013/077304 patent/WO2014096142A1/fr not_active Ceased
- 2013-12-19 EP EP13811508.4A patent/EP2935151A1/fr not_active Withdrawn
- 2013-12-19 US US14/652,180 patent/US20150299044A1/en not_active Abandoned
- 2013-12-19 DE DE102013226579.4A patent/DE102013226579A1/de not_active Withdrawn
- 2013-12-19 RU RU2015129336A patent/RU2015129336A/ru not_active Application Discontinuation
- 2013-12-19 JP JP2015548548A patent/JP2016500362A/ja not_active Ceased
-
2015
- 2015-06-11 IL IL239343A patent/IL239343A0/en unknown
-
2017
- 2017-12-04 US US15/830,265 patent/US20180093923A1/en not_active Abandoned
Non-Patent Citations (2)
| Title |
|---|
| None * |
| See also references of WO2014096142A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20150097714A (ko) | 2015-08-26 |
| RU2015129336A (ru) | 2017-01-25 |
| IL239343A0 (en) | 2015-07-30 |
| CN105263885A (zh) | 2016-01-20 |
| US20180093923A1 (en) | 2018-04-05 |
| DE102013226579A1 (de) | 2014-06-26 |
| WO2014096142A1 (fr) | 2014-06-26 |
| AU2013360718A1 (en) | 2015-07-09 |
| JP2016500362A (ja) | 2016-01-12 |
| US20150299044A1 (en) | 2015-10-22 |
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