CN1041058A - 高温超导体的生产方法以及由其组成的成型体 - Google Patents
高温超导体的生产方法以及由其组成的成型体 Download PDFInfo
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- 239000002887 superconductor Substances 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 19
- 239000010949 copper Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 239000011575 calcium Substances 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005266 casting Methods 0.000 claims abstract description 12
- 229910052802 copper Inorganic materials 0.000 claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000013517 stratification Methods 0.000 description 17
- 238000010586 diagram Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 3
- 229960004643 cupric oxide Drugs 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- GDFCXHYUALKPOU-UHFFFAOYSA-N [Cu][Ca][Sr][Bi] Chemical compound [Cu][Ca][Sr][Bi] GDFCXHYUALKPOU-UHFFFAOYSA-N 0.000 description 1
- OSOKRZIXBNTTJX-UHFFFAOYSA-N [O].[Ca].[Cu].[Sr].[Bi] Chemical compound [O].[Ca].[Cu].[Sr].[Bi] OSOKRZIXBNTTJX-UHFFFAOYSA-N 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- 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
- C04B35/45—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 copper oxide or solid solutions thereof with other oxides
- C04B35/4521—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 copper oxide or solid solutions thereof with other oxides containing bismuth oxide
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- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/653—Processes involving a melting step
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N60/00—Superconducting devices
- H10N60/01—Manufacture or treatment
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- 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
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- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S505/00—Superconductor technology: apparatus, material, process
- Y10S505/725—Process of making or treating high tc, above 30 k, superconducting shaped material, article, or device
- Y10S505/739—Molding, coating, shaping, or casting of superconducting material
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- 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
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- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S505/00—Superconductor technology: apparatus, material, process
- Y10S505/775—High tc, above 30 k, superconducting material
- Y10S505/776—Containing transition metal oxide with rare earth or alkaline earth
- Y10S505/782—Bismuth-, e.g. BiCaSrCuO
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Abstract
一种高温超导体的生产方法,该超导体的组成为Bi2(Sr,Ca)3Cu2O8+x,其中Sr对Ca之比为(5-2)∶1,X为0-2,该方法包括用力拌合具有化学计量比的铋、锶、钙和铜的氧化物和/或碳酸盐的化合物,在870-1100℃下加热所得到的混合物直到得到均匀的熔融体,将该熔融体浇注到模具中,并使其固化,使从模中取出的浇铸体在780-850℃下退火6-30小时,最后在氧气气氛中于600-830℃的温度下处理经退火后的浇铸体至少6小时。
Description
本发明涉及一种高温超导体的生成方法,及其用该超导体生产的成型体。该超导体的组成为Bi2(Sr,Ca)3Cu2O8+x,其中Sr对Ca的比例为(5~2)∶1,x为0~2。
作为授予诺贝尔奖的Bednorz和Miiller的发现结果,已知不仅在低于24K的温度下某些金属合金为超导体,而且除氧化铜以外还含有碱土氧化物和稀土氧化物的陶瓷化合物也具有超导性能,即使在较高温度下也是如此。由于它们的较高的所谓临界温度,这些化合物被称之为高温超导体。
至今,已知铋-锶-钙-铜-氧体系中有三种化合物显示出超导性能,详见如下:
Bi2(Sr,Ca)2CuO6+x(1-层化合物);
临界温度:约40K;
Bi2(Sr,Ca)3Cu2O8+x(2-层化合物);
临界温度:85K;
Bi2(Sr,Ca)4Cu3O10+x(3-层化合物);
临界温度:约105K;
同时,这两种第一命名化合物可以通过烧结粉末状氧化物或碳酸盐来生产,在该方法中,如果使用适量的原料,并在刚好低于粉末混合物的熔点下进行烧结,在相混合物中只能获得大比例的2-层化合物。为了防止部分粉末混合物在这种环境下熔化,首先使粉末混合物在低温下烧结,以便使其经几次中间研磨之后总是在稍微升高的温度下再烧结。
最后,建议熔融具有过量氧化铜的铋、锶、钙和铜的氧化物的混合物,而从这种熔体中拉出单晶,特别是2-层化合物的单晶体(参见H.G.von Schnering et al.in:“Angewandte Chemie”,100(1988),604~607)。
这种第一命名的方法缺点在于技术上非常复杂。另外,二种方法都不能生产出X射线用的相纯产品。
因此,本发明的目的在于提供一种组成为Bi2(Sr,Ca)3Cu2O8+x(2-层化合物)的高温超导体的生产方法,用这种方法可以获得基本相纯的产品,而具有很小的技术复杂性。根据本发明,这一目的可通过下列方法实现,该方法包括用力拌和具有化学计量比的铋、锶、钙和铜的氧化物和/或碳酸盐,在870~1100℃最好是950~1000℃下加热该混合物,直到获得均相熔融体,将所得到的熔融体浇注到模型中,并使其在膜型中固化,再将从模型中取出的浇铸体在780~850℃下退火6~30小时,最好7~12小时,然后在氧气气氛中于600~830℃下处理退火后的浇铸体至少6小时。
本发明的方法还可以进一步选择性地改进,
a)使用铜制模型,
b)在810~830℃下进行退火,
c)在氧气氛中的处理进行8~24小时,
d)在800~820℃下进行氧气氛中的处理,
e)在退火之前,用机械方法使浇铸体转换成具有理想尺寸的型体,
f)型体的最大厚度达6mm。
最后,根据本发明的方法可以生产出型体。在这些情况下,它们的形状和尺寸可以通过用于生产浇注体的模型的形状和尺寸来决定。
在本发明的方法中,优先使用铜模,是因为在它们表面产生的氧化铜是其体系中固有的,而由此会引起很小的干扰或根本没有。
在本发明的方法中,在纯氧气中的退火只造成轻微的但却是可检测到的结构变化。为形成纯的2-层化合物,在氧气中的退火是不可缺少的。
通常,铋-锶-钙-铜的氧指数不是精确地符合从参加的元素在每种情况下均为最稳定价时计算得到的数值。某些铜和/或铋也可以是更高价的。所述的三种化合物在它们的结构中具有可以被氧占据的点阵位,但并不一定被氧占据。取决于温度和氧分压的高低,氧可能进入上述化合物中或再次离开这些化合物。氧指数a+x的规格是这样选择的:即与最稳定价(Cu:2+,Bi:3+,Sr:2+,Ca:2+)的数值相一致。其中X表示对铜和铋的较高价部分的氧当量。
实施例1(对比实例)
将467g的Sr O、126g的Ca O和358g的Cu O的混合物在一个辊筒混合机中均匀化之后,将其在一个烧结刚至坩埚中于920℃下加热12小时。然后向得到的混合物之中加入1049g的Bi2O3。将该四组分混合物的一半首先在800℃下退火12小时。中间研磨之后,在870℃下加热6小时。所得到的产品产生出X-射线图1a(参见附图)。
将这四组分混合物的另一半在800℃、820℃、850℃、860℃和870℃的每一温度下退火12小时,在每一温度下处理之后进行中间研磨。所得的产品产生出X-射线图1b(参见附图)。
这两个X-射线图的比较表示出,一方面,通过较长的热处理,减少1-层化合物,而有利于2-层化合物,而另一方面,即使在退火72小时之后,还没有存在相纯的2-层化合物。将具有X-射线图1b的产物在氧气气氛中于815℃加热8小时。其临界温度为68K。
实施例2(对比实例)
将467g的Sr O、126g的Ca O、358g的Cu O和1049g的Bi2O3的混合物在辊筒混合机中均匀化。将300g的这种混合物倒入一个烧结刚至坩埚中,然后在一个箱式炉中于1000℃下加热1小时。将得到的均匀的熔体浇铸到一个铜模(尺寸:30×30×60mm)中,使其固化。使其冷却后,研磨得到的浇铸体。所得粉末产生出X-射线图2(参见附图);该图中没有2-层化合物的反射,而只有1-层化合物和至少另外一相的反射。
将具有X-射线图2的粉末在空气中于815℃下退火三次,每次8小时,每次退火之间进行研磨,最后使其在氧气氛下于815℃下再次退火8小时。所得到的粉末产生出X-射线图3(参见附图),即,该粉末是由1-层化合物和2-层化合物组成的相混合物。
实施例3(根据本发明)
将根据实施例2生成的浇铸体用切割轮(钻石涂层的铜轮)切成3mm厚的板。将这些板的空气中于815℃下退火8小时,经退火后,所得到的X-射线图表示,除少量残余的1-层化合物外,存在2-层化合物。这些板在氧气氛中于815℃下进行的后续8小时退火期间,1-层化合物的线消失到最大可能的程度(参见附图曲线4)。
该板的临界温度为85K。
实施例4(根据本发明)
重复实施例3,不同的是使3mm厚的板在空气中于790℃下退火30小时,然后在氧气气氛下于与上同样温度下退火12小时。
从它们的X-射线图和临界温度来看,这些板与根据实施例3所获得的板一致。
Claims (11)
1、一种高温超导体的生产方法,该超导体的组成为Bi2(Sr,Ca)3Cu2O8+X,其中Sr对Ca之比为(5~2)∶1,X为0~2,该方法包括用力伴合具有化学计量比的铋、锶、钙和铜的氧化物和/或碳酸盐的化合物,在870~1100℃下加热所得到的混合物直到得到均匀的熔融体,将该熔融体浇注到模具中,并使其固化,使从模中取出的浇铸体在780~850℃下退火6~30小时,最后在氧气气氛中于600~830℃的温度下处理经退火后的浇铸体至少6小时。
2、一种如权利要求1所述的方法,其中将所说的混合物加热到950~1000℃。
3、一种如权利要求1所述的方法,其中使用铜制的模子。
4、一种如权利要求1所述的方法,其中将所说的从膜中取出的浇铸体退火7~12小时。
5、一种如权利要求1所述的方法,其中的退火是在810~830℃下进行。
6、一种如权利要求1所述的方法,其中在氧气气氛中的处理进行8~24小时。
7、一种如权利要求1所述的方法,其中氧气气氛中的处理在800~820℃下进行。
8、一种如权利要求1所述的方法,其中浇铸体在退火之前,用机械方法将其加工成具有所需尺寸的型体。
9、一种如权利要求8所述的方法,其中所说的型体最大厚度达6mm。
10、根据权利要求1所述方法生产的型体。
11、根据权利要求1所述方法生产的型体,其中它们的形状和尺寸由生产浇铸体时所用的模具的形状和尺寸所决定。
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Application Number | Priority Date | Filing Date | Title |
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DEP3830092.3 | 1988-09-03 | ||
DE3830092A DE3830092A1 (de) | 1988-09-03 | 1988-09-03 | Verfahren zur herstellung eines hochtemperatursupraleiters sowie daraus bestehende formkoerper |
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CN1041058A true CN1041058A (zh) | 1990-04-04 |
CN1034247C CN1034247C (zh) | 1997-03-12 |
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US (2) | US5047391A (zh) |
EP (1) | EP0362492B1 (zh) |
JP (1) | JP2645470B2 (zh) |
KR (1) | KR100194844B1 (zh) |
CN (1) | CN1034247C (zh) |
AT (1) | ATE93503T1 (zh) |
CA (1) | CA1321870C (zh) |
DE (2) | DE3830092A1 (zh) |
ES (1) | ES2043976T3 (zh) |
NO (1) | NO300062B1 (zh) |
Cited By (1)
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CN100375794C (zh) * | 2005-12-28 | 2008-03-19 | 西北有色金属研究院 | 一种铋系Bi-2223高温超导带材的制备方法 |
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NZ228132A (en) * | 1988-04-08 | 1992-04-28 | Nz Government | Metal oxide material comprising various mixtures of bi, tl, pb, sr, ca, cu, y and ag |
DE3830092A1 (de) * | 1988-09-03 | 1990-03-15 | Hoechst Ag | Verfahren zur herstellung eines hochtemperatursupraleiters sowie daraus bestehende formkoerper |
DE3913397A1 (de) * | 1989-04-24 | 1989-10-19 | Asea Brown Boveri | Verfahren zur herstellung eines hochtemperatur-supraleiters |
US5244876A (en) * | 1990-02-13 | 1993-09-14 | Hoechst Aktiengesellschaft | Method for joining parts of ceramic high-temperature superconductor material |
US5151407A (en) * | 1990-02-28 | 1992-09-29 | The United States Of America As Represented By The Secretary Of The Navy | Method of producing Bi-Sr-Ca-Cu-O superconducting materials in cast form |
DE4011725A1 (de) * | 1990-04-11 | 1991-10-17 | Hoechst Ag | Verfahren zur herstellung eines hochtemperatursupraleiters |
DE4019368A1 (de) * | 1990-06-18 | 1991-12-19 | Hoechst Ag | Verfahren zur herstellung rohrfoermiger formteile aus hochtemperatur-supraleiter-material sowie eine anlage zu seiner durchfuehrung |
US5215961A (en) * | 1990-06-25 | 1993-06-01 | The United States Of America As Represented By The Secretary Of The Navy | Machinable oxide ceramic |
DE4026017A1 (de) * | 1990-08-17 | 1992-02-20 | Hoechst Ag | Verfahren zur herstellung von formkoerpern aus vorstufen von hochtemperatursupraleitern |
DE4026014A1 (de) * | 1990-08-17 | 1992-02-20 | Hoechst Ag | Verfahren zur herstellung von formkoerpern aus vorstufen oxidischer hochtemperatursupraleiter |
DE4026015A1 (de) * | 1990-08-17 | 1992-02-20 | Hoechst Ag | Verfahren zur herstellung von formkoerpern aus vorstufen oxidischer hochtemperatursupraleiter |
DE4109499A1 (de) * | 1990-10-13 | 1992-04-16 | Hoechst Ag | Supraleitende verbindung und verfahren zu ihrer herstellung |
JP2900951B2 (ja) * | 1990-11-30 | 1999-06-02 | 富士通株式会社 | セラミック製中空管の製造方法 |
US5759961A (en) * | 1991-01-31 | 1998-06-02 | The Babcock & Wilcox Company | Superconductor fiber elongation with a heated injected gas |
CH682358A5 (en) * | 1991-02-22 | 1993-08-31 | Asea Brown Boveri | Ceramic high temp. superconductor prodn. - by pouring starting material into mould, heating, cooling, thermally treating in oxygen@ and cooling, for shield magnetic fields in switching elements |
DE69227274T2 (de) * | 1991-03-29 | 1999-06-24 | Hitachi, Ltd., Tokio/Tokyo | Supraleitender Gegenstand und Verfahren zur Herstellung diesen supraleitenden Gegenstand |
DE4118988A1 (de) * | 1991-06-08 | 1992-12-10 | Hoechst Ag | Mit metallischen leitern kontaktierte massivkoerper aus keramischem hochtemperatur-supraleiter-material sowie verfahren zu ihrer herstellung |
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DE3711975A1 (de) * | 1987-04-09 | 1988-10-27 | Siemens Ag | Verfahren zur herstellung eines keramischen supraleiter-materials mit hoher sprungtemperatur |
DE3803530C2 (de) * | 1988-02-05 | 1997-11-27 | Hoechst Ag | Oxidischer Supraleiter und Verfahren zu seiner Herstellung |
US5126321A (en) * | 1988-08-09 | 1992-06-30 | The United States Of America As Represented By The Department Of Energy | Preparation of Bi-Sr-Ca-Cu-O superconductors from oxide-glass precursors |
DE3830092A1 (de) * | 1988-09-03 | 1990-03-15 | Hoechst Ag | Verfahren zur herstellung eines hochtemperatursupraleiters sowie daraus bestehende formkoerper |
-
1988
- 1988-09-03 DE DE3830092A patent/DE3830092A1/de active Granted
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1989
- 1989-07-10 AT AT89112543T patent/ATE93503T1/de not_active IP Right Cessation
- 1989-07-10 DE DE89112543T patent/DE58905375D1/de not_active Expired - Fee Related
- 1989-07-10 EP EP89112543A patent/EP0362492B1/de not_active Expired - Lifetime
- 1989-07-10 ES ES89112543T patent/ES2043976T3/es not_active Expired - Lifetime
- 1989-07-21 CA CA000606320A patent/CA1321870C/en not_active Expired - Fee Related
- 1989-08-18 US US07/395,609 patent/US5047391A/en not_active Expired - Fee Related
- 1989-08-31 NO NO893494A patent/NO300062B1/no unknown
- 1989-09-01 CN CN89106736A patent/CN1034247C/zh not_active Expired - Fee Related
- 1989-09-01 KR KR1019890012617A patent/KR100194844B1/ko not_active IP Right Cessation
- 1989-09-04 JP JP1227654A patent/JP2645470B2/ja not_active Expired - Lifetime
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100375794C (zh) * | 2005-12-28 | 2008-03-19 | 西北有色金属研究院 | 一种铋系Bi-2223高温超导带材的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
DE58905375D1 (de) | 1993-09-30 |
CA1321870C (en) | 1993-09-07 |
EP0362492A3 (en) | 1990-07-11 |
NO893494D0 (no) | 1989-08-31 |
ES2043976T3 (es) | 1994-01-01 |
NO300062B1 (no) | 1997-04-01 |
US5409888A (en) | 1995-04-25 |
JPH02107558A (ja) | 1990-04-19 |
US5047391A (en) | 1991-09-10 |
KR100194844B1 (ko) | 1999-06-15 |
JP2645470B2 (ja) | 1997-08-25 |
EP0362492A2 (de) | 1990-04-11 |
EP0362492B1 (de) | 1993-08-25 |
ATE93503T1 (de) | 1993-09-15 |
DE3830092C2 (zh) | 1993-06-09 |
CN1034247C (zh) | 1997-03-12 |
DE3830092A1 (de) | 1990-03-15 |
NO893494L (no) | 1990-03-05 |
KR900005636A (ko) | 1990-04-14 |
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