CN1171828C - 半透明陶瓷制品及其制备方法 - Google Patents
半透明陶瓷制品及其制备方法 Download PDFInfo
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- CN1171828C CN1171828C CNB01116980XA CN01116980A CN1171828C CN 1171828 C CN1171828 C CN 1171828C CN B01116980X A CNB01116980X A CN B01116980XA CN 01116980 A CN01116980 A CN 01116980A CN 1171828 C CN1171828 C CN 1171828C
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- 239000000919 ceramic Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 5
- 239000004902 Softening Agent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims 1
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229910003443 lutetium oxide Inorganic materials 0.000 abstract 3
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 abstract 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract 1
- 239000004014 plasticizer Substances 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- -1 magnesium aluminate Chemical class 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 241000588731 Hafnia Species 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003966 growth inhibitor Substances 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/10—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 aluminium oxide
- C04B35/111—Fine ceramics
- C04B35/115—Translucent or transparent products
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
- Y10S264/91—Sintering to produce translucent inorganic article
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Vessels And Coating Films For Discharge Lamps (AREA)
Abstract
本发明公开了一种包含α-氧化铝和至多0.050重量%氧化镁和在0.001至0.100重量%之间的氧化镥的烧结半透明陶瓷制品。在一个优选的实施方案中氧化镥为0.050重量%，而在第二个优选实施方案中一半氧化镥被氧化钇代替。制备半透明陶瓷制品的方法包括下述几个步骤：制备水性浆液以形成上述的组合物之一；加入硝酸将pH调至4.6；以2.5%(固体重量)的量加入水性粘合剂和增塑剂；将浆液喷雾干燥；经湿袋等压制成制品；将所述制品于大约1325℃在空气中预烧制大约2小时；和于1800℃在氢气中将所述经空气烧制的制品烧结大约3小时。
Description
本申请系申请日为1996年6月14日、申请号为96106188.X、发明名称为“半透明多晶氧化铝及其制备方法”的发明专利申请的分案申请。
技术领域
本发明涉及半透明陶瓷制品，更具体地说涉及可在较低的烧结温度下制造的高密度多晶氧化铝(PCA)。本发明还涉及该陶瓷制品的制备方法。
背景技术
PCA半透明坯体是已知的。Coble在美国专利第3026210号中披露：当密度超过98％时，使用0.0625至0.5％(重量)MgO通过防止在氧化铝晶粒内部残留气孔帮助消除残余孔隙并在烧结的后期控制晶粒生长。
Charles等人在美国专利第4285732中提出向氧化铝-氧化镁陶瓷中加入少量氧化锆和/或氧化铪以控制第二相、通常是尖晶石即铝酸镁MgAl2O4的形成，这在当氧化镁含量增加在该溶解度以上时可能发生。在该烧结坯体中的晶粒尺寸据认为是20至50微米。
发明内容
因此，本发明的目的是改进半透明陶瓷的制造方法。
本发明的另一个目的是生产具有小的晶粒尺寸并具有最适宜的密度的半透明陶瓷。
在本发明的一个方案中，这些目的通过提供包含相当大量的α-氧化铝和至多0.050％(重量)氧化镁和至多0.035％(重量)氧化镥或其前体的组合物作为晶粒生长抑制剂来实现。
在本发明的另一个方案中，提供一种经烧结的半透明的陶瓷坯体，它包含相当大量的α-氧化铝和至多0.050％(重量)氧化镁和在0.001至0.100％(重量)之间的氧化镥。
制备这样的半透明陶瓷制品的方法包括下述几个步骤：形成水性浆液以产生上述的组合物；向该组合物中加入硝酸将pH调节至4.6；然后向该浆液中加入2.5％(固体重量)的水性粘合剂和增塑剂，然后将该浆液喷雾干燥；通过湿袋等压(wet-bag isopress)制成制品，并将该制品于大约1325℃在空气中预烧制大约2小时，然后于1800℃在氢气中烧制大约3小时。
为了更好地理解本发明以及本发明的其它目的、优点和效果，披露下列内容。
具体实施方式
实施例1
通过将500g 0.1μm 65％α-氧化铝以40％固体分散于已加入经定量分析的Mg(NO3)2和Lu(NO3)3的水溶液的水中，制备一批含有0.05％(重量)MgO、0.035％(重量)Lu2O3和2.5％(重量)有机粘合剂和增塑剂例如2.0％(重量)聚乙二醇和0.5％(重量)聚乙烯基醇的氧化铝粉。该硝酸镥购自Johnson Matthey Electronics，其纯度按金属计为99.9％。加入硝酸将pH调至4.6。以2.5％(固体重量)的量加入水性粘合剂例如聚乙烯基醇和增塑剂例如聚乙二醇。搅拌该浆液，然后喷雾干燥，并将得到的粉末通过湿袋等压制成制品。将该制品于1325℃在空气中预烧制2小时，然后在氢气中于1800℃烧结3小时。该氢气烧制以两个步骤完成，即于2psi在干燥的氢气中第一次烧制1小时，和于2psi的露点为23℃的氢气中第二次烧制2小时。
实施例2
方法同实施例1，只是一半的Lu2O3(0.0175％(重量))用Y2O3代替。将得自实施例1和2的样品(2)与含有MgO和Y2O3的先有技术组合物的对照样品一起同时烧结。对照组的在线光透射率为5.2％，总光透射率为96％，平均晶粒尺寸为11微米。实施例1的制品相应的值分别为4.5％、96％和7.8，而实施例2的制品的值分别为4.9％、95％和9.2。
在所有的情况下，制得的烧结制品均是适宜用在高压钠灯中的放电管。
因此，本文中所述的组合物制造出的半透明陶瓷制品比先有技术组合物的具有更小的合乎需要的晶粒尺寸。
尽管已描述了目前被认为是本发明的优选的实施方案，但在不背离由所附权利要求书所限定的本发明的范围的条件下可进行的各种改变和修饰对本领域的技术人员来说将是显而易见的。
Claims (5)
1.含有α-氧化铝和至多0.050％重量氧化镁和在0.001至0.100％重量之间的氧化镥的一种经烧结的半透明的陶瓷制品。
2.权利要求1的制品，其中所述的氧化镥的含量为所述氧化铝重量的0.035％重量。
3.权利要求2的制品，其中50％重量的所述氧化镥被氧化钇代替。
4.制备半透明陶瓷制品的方法，包括下述几个步骤：形成水性浆液以产生权利要求3的组合物；加入硝酸将pH调节至4.6；以2.5％固体重量的量加入水性粘合剂和增塑剂；将该浆液喷雾干燥；通过湿袋等压制成制品；将所述制品于1325℃在空气中预烧制2小时；和将所述经空气烧制的制品于1800℃在氢气中烧结3小时。
5.权利要求4的方法，其中所述的在氢气中烧结包括：在2psi的干燥的氢气气氛中第一次烧制1小时；和在2psi的压力下在露点为23℃的氢气中第二次烧制2小时。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US08/491,064 US5587346A (en) | 1995-06-16 | 1995-06-16 | Translucent polycrystalline alumina |
| US491064 | 1995-06-16 | ||
| US491,064 | 1995-06-16 |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96106188A Division CN1080247C (zh) | 1995-06-16 | 1996-06-14 | α－氧化铝组合物 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1326908A CN1326908A (zh) | 2001-12-19 |
| CN1171828C true CN1171828C (zh) | 2004-10-20 |
Family
ID=23950639
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96106188A Expired - Fee Related CN1080247C (zh) | 1995-06-16 | 1996-06-14 | α－氧化铝组合物 |
| CNB01116980XA Expired - Fee Related CN1171828C (zh) | 1995-06-16 | 2001-05-18 | 半透明陶瓷制品及其制备方法 |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96106188A Expired - Fee Related CN1080247C (zh) | 1995-06-16 | 1996-06-14 | α－氧化铝组合物 |
Country Status (6)
| Country | Link |
|---|---|
| US (2) | US5587346A (zh) |
| EP (1) | EP0748780B1 (zh) |
| JP (1) | JPH092865A (zh) |
| CN (2) | CN1080247C (zh) |
| DE (1) | DE69604021T2 (zh) |
| HU (1) | HU219678B (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100242601B1 (ko) * | 1994-10-21 | 2000-04-01 | 이쿠노 도모히사 | 태양 전지 시계용 문자판 및 그것의 제조 방법 |
| DE19602525A1 (de) * | 1996-01-25 | 1997-08-07 | Starck H C Gmbh Co Kg | Sphärische Keramikformkörper, Verfahren zu ihrer Herstellung sowie deren Verwendung |
| US5631201A (en) * | 1996-07-29 | 1997-05-20 | Osram Sylvania Inc. | Translucent polycrystalline alumina and method of making same |
| US5993725A (en) * | 1998-10-02 | 1999-11-30 | Osram Sylvania Inc. | Method of forming complex-shaped hollow ceramic bodies |
| JP2001322867A (ja) * | 2000-05-09 | 2001-11-20 | Matsushita Electric Ind Co Ltd | 透光性焼結体と、これを用いた発光管及び放電灯 |
| JP2006315955A (ja) * | 2000-07-10 | 2006-11-24 | Toshiba Ceramics Co Ltd | セラミックス部材 |
| DE10101169C2 (de) * | 2001-01-12 | 2002-11-07 | Georg Grathwohl | Verfahren zur Herstellung eines transparenten alpha-Aluminiumoxidkörpers mit sub-mum Gefüge |
| DE10239058A1 (de) * | 2001-08-27 | 2003-04-03 | Denso Corp | Verfahren zur Herstellung eines Heißleiterelements und Herstellungsgerät zur Herstellung von Rohmaterial für ein Heißleiterelement |
| US6878456B2 (en) | 2001-12-28 | 2005-04-12 | 3M Innovative Properties Co. | Polycrystalline translucent alumina-based ceramic material, uses, and methods |
| US6648638B2 (en) | 2001-12-28 | 2003-11-18 | 3M Innovative Properties Company | Orthodontic appliances including polycrystalline alumina-based ceramic material, kits, and methods |
| US20040120886A1 (en) * | 2002-12-20 | 2004-06-24 | General Electric Company | Chlorine treatment for producing alumina ceramics with low transition metal impurities |
| CN1316695C (zh) * | 2002-12-31 | 2007-05-16 | 中国建筑材料科学研究院 | 陶瓷聚光腔材料、陶瓷聚光腔及其制造方法 |
| DE102004024017A1 (de) * | 2004-05-13 | 2005-12-01 | Schott Ag | Verfahren zur Herstellung einer Leuchtvorrichtung umfassend eine Glaskeramik |
| JP4959113B2 (ja) * | 2004-02-25 | 2012-06-20 | 京セラ株式会社 | アルミナ質焼結体 |
| CN1317224C (zh) * | 2004-05-11 | 2007-05-23 | 山东轻工业学院 | 氧化铝系多相复合结构陶瓷材料及其生产方法 |
| ES2354885T3 (es) * | 2004-07-02 | 2011-03-18 | Konoshima Chemical Co., Ltd. | Producto de sinterización de óxido de lutecio tansmisor de luz y procedimiento para producir el mismo. |
| US20060199041A1 (en) * | 2005-03-03 | 2006-09-07 | Osram Sylvania Inc. | Method of making a ceramic arc discharge vessel and ceramic arc discharge vessel made by the method |
| US8021451B2 (en) * | 2005-07-25 | 2011-09-20 | Sumitomo Chemical Company, Limited | Fine α-alumina particle |
| US7678725B2 (en) * | 2007-05-14 | 2010-03-16 | General Electric Company | Translucent polycrystalline alumina ceramic |
| US20080283522A1 (en) * | 2007-05-14 | 2008-11-20 | Shuyl Qin | Translucent polycrystalline alumina ceramic |
| WO2009105581A1 (en) | 2008-02-21 | 2009-08-27 | Nitto Denko Corporation | Light emitting device with translucent ceramic plate |
| CN101407410B (zh) * | 2008-11-11 | 2012-01-04 | 中国铝业股份有限公司 | 一种密封环用氧化铝陶瓷造粒粉的制备方法 |
| CN101560102B (zh) * | 2009-05-26 | 2012-02-22 | 上海大学 | C掺杂α-Al2O3透明陶瓷热释光和光释光材料的制备方法 |
| CN102807368B (zh) * | 2012-09-03 | 2014-06-11 | 上海应用技术学院 | 一种Nd3+:Lu2O3半透明纳米陶瓷的制备方法 |
| CN105074870B (zh) * | 2013-12-25 | 2016-12-07 | 日本碍子株式会社 | 操作基板、半导体用复合基板、半导体电路基板及其制造方法 |
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| DE202016009069U1 (de) | 2015-06-29 | 2022-01-24 | Corning Incorporated | Fertigungslinie und gesinterter Artikel |
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| US3026210A (en) * | 1961-01-03 | 1962-03-20 | Gen Electric | Transparent alumina and method of preparation |
| US3905845A (en) * | 1969-08-27 | 1975-09-16 | Ngk Insulators Ltd | Translucent alumina containing magnesia yttria and lanthium oxide |
| FR2475533A1 (fr) * | 1980-02-08 | 1981-08-14 | Euroceral | Procede de fabrication de pieces, notamment de tubes, en alumine translucide |
| US4285732A (en) * | 1980-03-11 | 1981-08-25 | General Electric Company | Alumina ceramic |
| NL8502457A (nl) * | 1985-09-09 | 1987-04-01 | Philips Nv | Gasdicht gesinterd translucent aluminiumoxyde. |
| FR2600055B1 (fr) * | 1986-06-16 | 1988-08-26 | Commissariat Energie Atomique | Aluminates mixtes de lanthanide-magnesium, lasers utilisant des monocristaux de ces aluminates |
| US5244849A (en) * | 1987-05-06 | 1993-09-14 | Coors Porcelain Company | Method for producing transparent polycrystalline body with high ultraviolet transmittance |
| US5001093A (en) * | 1987-05-06 | 1991-03-19 | Coors Porcelain Company | Transparent polycrystalline body with high ultraviolet transmittance |
| SU1511243A1 (ru) * | 1987-06-15 | 1989-09-30 | Харьковский Автомобильно-Дорожный Институт Им.Комсомола Украины | Шихта дл изготовлени керамики |
| EP0567095B1 (en) * | 1992-04-22 | 1996-07-03 | Sumitomo Chemical Company, Limited | Translucent polycrystalline alumina and process for producing the same |
| US5376606A (en) * | 1993-12-30 | 1994-12-27 | Korea Institute Of Science And Technology | Light-transmissive polycrystalline alumina ceramics |
-
1995
- 1995-06-16 US US08/491,064 patent/US5587346A/en not_active Expired - Fee Related
-
1996
- 1996-04-25 JP JP8127643A patent/JPH092865A/ja active Pending
- 1996-06-14 HU HU9601650A patent/HU219678B/hu not_active IP Right Cessation
- 1996-06-14 CN CN96106188A patent/CN1080247C/zh not_active Expired - Fee Related
- 1996-06-14 EP EP96109608A patent/EP0748780B1/en not_active Expired - Lifetime
- 1996-06-14 DE DE69604021T patent/DE69604021T2/de not_active Expired - Lifetime
- 1996-09-24 US US08/718,887 patent/US5627116A/en not_active Expired - Fee Related
-
2001
- 2001-05-18 CN CNB01116980XA patent/CN1171828C/zh not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| DE69604021T2 (de) | 1999-12-23 |
| HUP9601650A3 (en) | 1997-09-29 |
| EP0748780B1 (en) | 1999-09-01 |
| EP0748780A1 (en) | 1996-12-18 |
| HU9601650D0 (en) | 1996-08-28 |
| JPH092865A (ja) | 1997-01-07 |
| HU219678B (hu) | 2001-06-28 |
| CN1080247C (zh) | 2002-03-06 |
| DE69604021D1 (de) | 1999-10-07 |
| HUP9601650A2 (en) | 1997-02-28 |
| CN1326908A (zh) | 2001-12-19 |
| US5587346A (en) | 1996-12-24 |
| CN1141271A (zh) | 1997-01-29 |
| US5627116A (en) | 1997-05-06 |
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