EP0776985B1 - Verfahren zur Aufbringung einer metallischen Haftschicht für keramische Wärmedämmschichten auf metallische Bauteile - Google Patents
Verfahren zur Aufbringung einer metallischen Haftschicht für keramische Wärmedämmschichten auf metallische Bauteile Download PDFInfo
- Publication number
- EP0776985B1 EP0776985B1 EP96810768A EP96810768A EP0776985B1 EP 0776985 B1 EP0776985 B1 EP 0776985B1 EP 96810768 A EP96810768 A EP 96810768A EP 96810768 A EP96810768 A EP 96810768A EP 0776985 B1 EP0776985 B1 EP 0776985B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- metallic
- layer
- binder
- adhesive powder
- powder
- 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.)
- Expired - Lifetime
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Classifications
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12014—All metal or with adjacent metals having metal particles
- Y10T428/12028—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, etc.]
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12014—All metal or with adjacent metals having metal particles
- Y10T428/12028—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, etc.]
- Y10T428/12049—Nonmetal component
- Y10T428/12056—Entirely inorganic
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12014—All metal or with adjacent metals having metal particles
- Y10T428/12028—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, etc.]
- Y10T428/12063—Nonparticulate metal component
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12014—All metal or with adjacent metals having metal particles
- Y10T428/12028—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, etc.]
- Y10T428/12063—Nonparticulate metal component
- Y10T428/12097—Nonparticulate component encloses particles
Definitions
- the invention relates to the field of materials technology. It relates to a method for applying a metallic Adhesive layer for thermally sprayed ceramic thermal insulation layers to be subsequently applied to this adhesive layer (TBC) on metallic components as well as a metallic adhesive layer produced by this process.
- TBC adhesive layer
- metal and ceramic can be different because of the different Thermal expansion coefficients not with each other connect.
- the coated metallic Protect components from harmful thermal stresses their complete existence is important for a sufficient Component life.
- Components coated in this way are especially in the field of combustion technology used, for example for combustion chamber parts or gas turbine blades.
- the disadvantage of the metallic adhesive layers produced so far for ceramic thermal insulation layers is that they have insufficient roughness and therefore too little Offer form fit (undercuts) so that the layer thickness of the TBC layers is limited.
- Layer thicknesses are known from about 0.2 to 0.4 mm, with layer thicknesses of about 0.3 mm are most common. If you are fatter, so the risk of flaking increases rapidly. Are you thinner the thermal insulation effect quickly subsides. Recent developments go there, coarser adhesive layers (approx. 0.6 mm) to inject, but the necessary positive locking is missing.
- a roughness typical of known metallic adhesive layers is around 30 ⁇ m. Rougher the layers cannot be sprayed because of the dimension of the powder particles to be melted depending on the coating process (different spray temperatures and spray speeds) is limited to approx. 10 to 50 ⁇ m and the Flatten the liquid powder particles when they hit the substrate (cf. B. Heine: "Thermally sprayed layers", metal, 49th year, 1/1995, p.51-57).
- the invention tries to avoid all these disadvantages. you is based on the task of a metallic adhesive layer and a method of applying this adhesive layer for ceramic Thermal insulation layers on a metallic base body too develop with which it is compared to the known state of the art Technology is possible, then ceramic thermal insulation layers thermally spraying and attaching thicker. The layers should adhere stably and insensitively to be against impact.
- the advantages of the invention include in that with these Process adhesive layers are generated that are opposite to the State of the art are very rough.
- the soldered or sintered Metal powder particles are very stable and positive anchoring for the TBC layer to be sprayed on so that comparatively thick, stable adherence ceramic thermal insulation layers can be generated.
- both powders are first mixed intensively be and then this mixture on the metallic Surface of the base material is applied. This will achieved a more uniform distribution of the powder particles and also shortens the process time.
- solder material Material such as the base material and boron-free or low-boron solders used. This reduces possible brittle phase formation.
- the method according to the invention can be used locally for repair purposes as well as used for coating new parts become.
- the metallic adhesive layer produced according to the invention exists depending on the process variant used from a Surface of the solder layer wetting the metallic component with spherically or sputteringly formed soldered in it Adhesive powder particles or additionally from a thin sprayed, in particular protective gas plasma sprayed layer same type of material as the adhesive powder particles or an inert gas plasma sprayed onto the surface of the metallic component Protective layer with on its surface sintered adhesive powder particles.
- This metallic adhesive layer guarantees stable adhesion of the thermally sprayed ceramic thermal insulation layers, allows larger ones Layer thicknesses and leads to good emergency running properties.
- the height of the adhesive powder particles is approximately as large as the layer thickness of the thermal ceramic thermal barrier coating to be sprayed on. This will the layer is almost insensitive to impact because strikes essentially be collected in a metallic way.
- a guide vane of a gas turbine as an example of a metallic component 1 to be coated. It consists of the metallic base material (substrate) 2, in this case the alloy IN 939 with the following chemical composition: Bal. Ni; 22.5% Cr; 19.0% Co; 2.0% W; 1.0% Nb; 1.4% Ta; 3.7% Ti; 1.9% Al; 0.1 Zr; 0.01 B; 0.15 C.
- the blade is provided with a corrosion and oxidation layer on the gas-carrying surfaces (MCrAlY, e.g. SV201473: Bal. Ni; 25% Cr; 5% Al; 2.5% Si; 0.5% Y; 1 % Ta).
- this blade is coated on the leading edge, the pressure side of the blade and on the channel walls with an approximately 0.3 mm thick thermal insulation layer made of ytrium-stabilized zirconium oxide with the following composition: Bal. ZrO 2 incl 2.5% HfO 2 ; 7-9% Y 2 O 3 ; ⁇ 3% others.
- the gas turbine guide vane comes after an operating time of 25,000 hours for reconditioning. It is determined that due to thermal overload and erosion at the leading edge of the sheet and on the channel wall Thermal insulation layer is no longer present (see hatched Areas in Fig. 1). Since the shovel did no further damage will not be completely re-coated for cost reasons, but a partial repair of the thermal insulation layer sought. Because of that on the above Systematically make a particularly strong attack by the TBC the TBC layer should not only be of the same thickness, but run as thick as possible.
- the blade 1 becomes coarse in the steam jet Dirt (combustion residues) cleaned. After that deposits still adhering by means of soft sandblasting, (e.g. fine aluminum powder, 2 bar jet pressure, 20 cm distance) away. The still intact ceramic thermal insulation layer is allowed not be removed.
- soft sandblasting e.g. fine aluminum powder, 2 bar jet pressure, 20 cm distance
- the blade parts not to be coated are covered, for example with a sheet metal template, and the too coating surfaces are blasted (e.g. fine silicon carbide, Jet pressure 4 bar, distance 40 mm), so that any TBC residues and possible oxides are removed.
- a sheet metal template e.g. fine silicon carbide, Jet pressure 4 bar, distance 40 mm
- Adhesive powder 4 of the NiAl95 / 5 type is then used a pond size in the range of 100 to 200 microns over the sprinkled 3 moistened areas with the binder until about all 0.5 mm such adhesive powder particles 4 come to rest. After that the much finer solder powder 5 (particle diameter approx. 10-30 ⁇ m).
- solder material the alloy NB 150 (Bal.Ni; 15% Cr; 3.5% B; 0.1% C) with a melting point of 1055 ° C and a soldering range of 1065 used up to 1200 ° C.
- Weight is advantageous equal quantities of adhesive powder 4 and solder powder 5. But of course you can also use other proportions to get voted.
- the packing density of the particles not of crucial importance because they are dense Packs are suitable, but less dense packs are also already sufficient.
- Fig. 2 schematically shows a cross section of the different ones Layers after application.
- the surface coated in this way can now be brought into the soldering furnace horizontally, vertically or overhead.
- the solder 5 and the adhesive powder 4 remain in their applied position until the solder has melted and has wetted and soldered the substrate surface and the surface of the adhesive powder particles.
- the soldering is carried out in a high vacuum oven at 5x10 -6 mbar, 1080 ° C and a holding time of 15 min.
- Fig. 3 shows schematically a cross section of the different Layers after the soldering process.
- Lot 5 has the one to be repaired
- the surface is completely wetted and the adhesive powder particles 4 are soldered.
- the surface looks metallic matt silvery shiny.
- the diffusion zone is because of the short Soldering time and the relatively low soldering temperature only very much small.
- the shovel is again covered with a template and with a 0.5 mm thick ceramic thermal barrier coating 6, here made of calcium-stabilized zirconium oxide (MetaCeram 28085), the zirconium oxide using a known flame spraying process is applied, provided.
- a ceramic thermal barrier coating 6 here made of calcium-stabilized zirconium oxide (MetaCeram 28085)
- Fig. 4 shows schematically the layer structure according to the flame spraying process.
- the attachment of the zirconium oxide can be done with a Compare push button technology.
- the zirconium oxide has one strong positive locking and many undercuts on the contrary to the usual adhesive geometries, which at best only have a small form fit. This is the anchor the zirconium oxide (TBC) layer on the component is very stable.
- TBC zirconium oxide
- Adhesive layers is therefore next to plasma spraying and detonation flame spraying as described above flame spraying is also suitable. The latter has the advantage that portable coating devices are used for this can.
- Another advantage of the invention is the high resistance to thermal shock of layers.
- coated metallic component 1 was then thermocycled in a hot gas stream (heating with about 50 Degrees / min gas temperature, 2 min hold at 1000 ° C, cooling with 100 degrees / s gas temperature to 500 ° C). Even after 70 cycles the shift has not yet occurred.
- Another advantage is the excellent emergency running properties the thermal on the adhesive layer according to the invention sprayed TBC layers.
- the ceramic layer 6 bursts, ie in in this case the zirconium oxide, only above the adhesive powder 4 from.
- the TBC layer 6 falls between the adhesive powder particles 4 due to the large positive connection, so that the ceramic thermal barrier coating 6 at least in the thickness of Adhesive powder particles 4 (approx. 200 ⁇ m) are retained.
- Fig. 6 shows a perspective Representation of a thermal insulation board for hot gas, which in New condition with the thickest possible thermal spray Thermal insulation layer should be provided.
- the thermal insulation board consists of the alloy MAR M 247, the following chemical Composition: Bal. Ni; 8.2-8.6% Cr; 9.7-10.3% Co; 0.6-0.8% Mo; 9.8-10.2% W; 2.9-3.1% Ta; 5.4-5.6% Al; 0.8-1.2% Ti; 1.0-1.6% Hf; 0.14-0.16% C).
- the metallic component 1 to be coated is included relatively coarse silicon carbide (particle diameter ⁇ 200 ⁇ m) blasted oxide-free and rough (10 to 30 ⁇ m). After that the surface to be coated, for example with a brush Spread thinly with organic binder 3. Under a trickle for coarse spherical adhesive powder 4 (SV 20 14 73 with the following chemical composition: Bal. Ni; 25% Cr; 5% Al; 2.5% Si; 0.5% Y; 1% Ta) with a grain diameter of 150 the plate 1 to be coated is moved back and forth up to 300 ⁇ m, even distribution down to the adhesive layer of the highly corrosion-resistant adhesive powder 4 has taken place. in the The individual powder particles should be 0.3 to 0.6 mm Distance from each other.
- Amdry Alloy DF 5 which is additional to the high Cr content, a high Al content with somewhat reduced B content selected.
- the exact composition is the following: Bal. Ni; 13% Cr; 3% Ta; 4% Al; 2.7% B; 0.02% Y. Lot 5 is also made using a suitable Spray device applied evenly to the surface to be soldered. It is also possible to mix adhesive powder 4 and solder 5 and then the mixture in one process step on the sprinkle the coated surface with the cement binder 3.
- the soldering is carried out in a high vacuum oven at 1100 ° C and 15 min Hold time.
- Thermal insulation layer 6 is a protective gas plasma spraying thin layer 7 (approx. 50 ⁇ m) SV 20 14 73 applied. That makes in addition to the rough anchoring option (as in the embodiment 1) additionally a fine interlocking what the adhesive strength of thick TBC layers in thermal shock further increases.
- Fig. 7 shows schematically the formation of these layers.
- the component coated in this way proved itself in a thermal shock test in a sand bed (1000 ° C to room temperature) as resistant to thermal shock.
- the solder layer After a long period of operation, the solder layer is between corroded somewhat away from the large adhesive powder grains, but the The load-bearing part of the solder neck cannot be attacked by corrosion reduce significantly.
- a cooled guide vane made of the material CM 247 LC DS (chemical composition: Ba. Ni; 8.1% Cr; 9.2% Co; 0.5% Mo; 9.5% W; 3.2% Ta; 0.7% Ti; 5.6% Al; 0.01% Zr; 0.01% B; 0.07% C; 1.4% Hf) exists, in new condition with a 0.7 to 0.8 mm thick TBC layer be provided.
- CM 247 LC DS chemical composition: Ba. Ni; 8.1% Cr; 9.2% Co; 0.5% Mo; 9.5% W; 3.2% Ta; 0.7% Ti; 5.6% Al; 0.01% Zr; 0.01% B; 0.07% C; 1.4% Hf
- the blade is sprayed in the entire channel area using inert gas plasma with the powder ProXon 21031 (alloy on Nickel base) about 0.2 mm thick coated (sprayed low in oxygen).
- This powder exhibits because of its high aluminum content and chromium content an excellent oxidation and Corrosion resistance.
- Oxidation and corrosion protection layer 8 a thin Layer Binder 3 applied.
- the coating takes place then in a high vacuum furnace under solution annealing conditions for CM 247 LS DS (several hours at 1220 to 1250 ° C).
- the oxidation and corrosion protection layer 8 am Base material 1.
- Layer 8 further densifies and coarse adhesive powder particles 4 are formed by stable sintering 9 on the layer 8, which is now a Protective and adhesive layer is bound.
- a cooled one is also intended Guide vane made of CM 247 LC DS with a thermal barrier coating be provided.
- Lot 5 for attaching the coarse adhesive powder particles 4 from ProXon 21031 will be the same Powder CM 247 with an addition of 6% Cr; 3% Si; 2% Al and 0.5% B used. The order is made as above described, i.e. on the thin cement binder layer 3 the approximately 150 to 200 ⁇ m large adhesive powder 4 scattered and on it in abundance the solder powder 5. Then subjected the blade to a heat treatment in which the Base material 2 solution annealed and the solder 5 partially melted becomes.
- thermal shock tests showed that the thermal insulation layer thus attached superior to a conventionally produced layer is. Even if for different reasons a piece of the TBC layer bursts off, remains between the adhesive powder particles maintain this layer and thus guarantee good emergency running properties. In contrast, bursts with conventionally coated If the TBC layer is scooped off, it remains on the substrate only minimal residues, which is by no means an insulating Feature. In addition, in this example shown that it is cheap, boron-free or almost boron-free Solder to be used as the brittle phase formation with W-borides is hardly possible.
- the Base material 2 is MAR M 247, NB 150 was used as lot 5 and the adhesive powder particles 4 are made of NiA195 / 5.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Coating By Spraying Or Casting (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Insulated Metal Substrates For Printed Circuits (AREA)
- Ceramic Products (AREA)
- Laminated Bodies (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19545025 | 1995-12-02 | ||
DE19545025A DE19545025A1 (de) | 1995-12-02 | 1995-12-02 | Verfahren zur Aufbringung einer metallischen Haftschicht für keramische Wärmedämmschichten auf metallische Bauteile |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0776985A1 EP0776985A1 (de) | 1997-06-04 |
EP0776985B1 true EP0776985B1 (de) | 2001-12-19 |
Family
ID=7779041
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP96810768A Expired - Lifetime EP0776985B1 (de) | 1995-12-02 | 1996-11-11 | Verfahren zur Aufbringung einer metallischen Haftschicht für keramische Wärmedämmschichten auf metallische Bauteile |
Country Status (11)
Country | Link |
---|---|
US (1) | US5894053A (uk) |
EP (1) | EP0776985B1 (uk) |
JP (1) | JP3983323B2 (uk) |
CN (1) | CN1161489C (uk) |
AT (1) | ATE211185T1 (uk) |
CA (1) | CA2188614C (uk) |
CZ (1) | CZ290920B6 (uk) |
DE (2) | DE19545025A1 (uk) |
PL (2) | PL182552B1 (uk) |
RU (1) | RU2209256C2 (uk) |
UA (1) | UA42001C2 (uk) |
Cited By (1)
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FR2827308B1 (fr) * | 2001-07-12 | 2004-05-14 | Snecma Moteurs | Procede de reparation globale d'une piece revetue d'une barriere thermique |
EP1275748A3 (de) | 2001-07-13 | 2004-01-07 | ALSTOM (Switzerland) Ltd | Hochtemperaturbeständiger Schutzüberzug mit eingebetteten lokalen Erhebungen sowie Verfahren zur Herstellung des Schutzüberzuges |
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-
1995
- 1995-12-02 DE DE19545025A patent/DE19545025A1/de not_active Withdrawn
-
1996
- 1996-10-23 CA CA002188614A patent/CA2188614C/en not_active Expired - Fee Related
- 1996-11-05 US US08/743,936 patent/US5894053A/en not_active Expired - Lifetime
- 1996-11-11 DE DE59608498T patent/DE59608498D1/de not_active Expired - Lifetime
- 1996-11-11 AT AT96810768T patent/ATE211185T1/de active
- 1996-11-11 EP EP96810768A patent/EP0776985B1/de not_active Expired - Lifetime
- 1996-11-26 CZ CZ19963468A patent/CZ290920B6/cs not_active IP Right Cessation
- 1996-11-29 RU RU96122818/02A patent/RU2209256C2/ru not_active IP Right Cessation
- 1996-11-29 UA UA96114470A patent/UA42001C2/uk unknown
- 1996-12-02 PL PL96344351A patent/PL182552B1/pl not_active IP Right Cessation
- 1996-12-02 CN CNB961239093A patent/CN1161489C/zh not_active Expired - Fee Related
- 1996-12-02 PL PL96317298A patent/PL181404B1/pl not_active IP Right Cessation
- 1996-12-02 JP JP33444496A patent/JP3983323B2/ja not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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RU2763953C1 (ru) * | 2021-03-11 | 2022-01-11 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" (Госкорпорация "Росатом") | Комбинированное защитное покрытие |
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DE59608498D1 (de) | 2002-01-31 |
CZ346896A3 (en) | 1997-08-13 |
DE19545025A1 (de) | 1997-06-05 |
PL182552B1 (pl) | 2002-01-31 |
CA2188614C (en) | 2005-10-04 |
ATE211185T1 (de) | 2002-01-15 |
CN1160088A (zh) | 1997-09-24 |
US5894053A (en) | 1999-04-13 |
JPH09176818A (ja) | 1997-07-08 |
CN1161489C (zh) | 2004-08-11 |
UA42001C2 (uk) | 2001-10-15 |
JP3983323B2 (ja) | 2007-09-26 |
CA2188614A1 (en) | 1997-06-03 |
CZ290920B6 (cs) | 2002-11-13 |
PL181404B1 (pl) | 2001-07-31 |
PL317298A1 (en) | 1997-06-09 |
EP0776985A1 (de) | 1997-06-04 |
RU2209256C2 (ru) | 2003-07-27 |
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