EP1041173B1 - Light metal cylinder block, method for making it and apparatus for carrying out the process - Google Patents
Light metal cylinder block, method for making it and apparatus for carrying out the process Download PDFInfo
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- EP1041173B1 EP1041173B1 EP00105126A EP00105126A EP1041173B1 EP 1041173 B1 EP1041173 B1 EP 1041173B1 EP 00105126 A EP00105126 A EP 00105126A EP 00105126 A EP00105126 A EP 00105126A EP 1041173 B1 EP1041173 B1 EP 1041173B1
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- laser beam
- powder
- alloyed
- aluminum
- cylinder block
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02F—CYLINDERS, PISTONS OR CASINGS, FOR COMBUSTION ENGINES; ARRANGEMENTS OF SEALINGS IN COMBUSTION ENGINES
- F02F7/00—Casings, e.g. crankcases or frames
-
- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
-
- 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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
- C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
-
- 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
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
-
- 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
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/14—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying for coating elongate material
- C23C4/16—Wires; Tubes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02F—CYLINDERS, PISTONS OR CASINGS, FOR COMBUSTION ENGINES; ARRANGEMENTS OF SEALINGS IN COMBUSTION ENGINES
- F02F1/00—Cylinders; Cylinder heads
- F02F1/18—Other cylinders
- F02F1/20—Other cylinders characterised by constructional features providing for lubrication
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
- F05C—INDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
- F05C2201/00—Metals
- F05C2201/02—Light metals
- F05C2201/021—Aluminium
-
- 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
- Y10T29/00—Metal working
- Y10T29/49—Method of mechanical manufacture
- Y10T29/49229—Prime mover or fluid pump making
- Y10T29/4927—Cylinder, cylinder head or engine valve sleeve making
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Plasma & Fusion (AREA)
- Cylinder Crankcases Of Internal Combustion Engines (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Extrusion Of Metal (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Laser Beam Processing (AREA)
- Coating With Molten Metal (AREA)
Abstract
Description
Die Erfindung betrifft einen Leichtmetallzylinderblock mit mindestens einer verschleißfesten und tribologisch optimierten Zylinderlauffläche, umfassend eine Leichtmetallmatrixlegierung und ein hartmetallhaltiges Pulvermaterial, das als feindisperser, Primär-Silizium-Ausscheidungen enthaltene Oberflächenschicht auf der Leichtmetallmatrix vorliegt.The invention relates to a light metal cylinder block with at least a wear-resistant and tribologically optimized Cylinder tread, comprising a light metal matrix alloy and a carbide-containing powder material that is used as a finely dispersed, Primary silicon excretions contain surface layer is present on the light metal matrix.
Nach EP 0 837 152 A1 (Bayerische Motoren Werke AG) ist ein Verfahren zum Beschichten eines aus einer Aluminiumlegierung bestehenden Bauteils einer Brennkraftmaschine bekannt. Dabei wird ein Laserstrahl so gelenkt, daß er nicht direkt auf die Oberfläche des zu beschichtenden Bauteils gelangt, sondern zuvor auf einen Pulverstrahl trifft. Durch die Energie des Laserstrahls wird das Pulver vollständig vom festen in die flüssige Phase überführt, so daß es beim Auftreffen auf die Bauteiloberfläche in Form feiner Tröpfchen als Schichtmaterial darauf abgeschieden wird, die aufgrund der Erstarrungsbedingungen teilweise amorph erstarren.According to EP 0 837 152 A1 (Bayerische Motoren Werke AG) is a method for coating an existing aluminum alloy Known component of an internal combustion engine. In doing so, a Laser beam directed so that it is not directly on the surface of the component to be coated, but previously on one Powder jet hits. Because of the energy of the laser beam Powder completely transferred from the solid to the liquid phase, so that when it hits the component surface in shape fine droplets are deposited on it as layer material, which partially solidify amorphously due to the solidification conditions.
Bei dem bekannten Verfahren erfolgt daher kein Einlegieren des Pulvers in die Oberflächenschicht des Bauteils, sondern es wird eine Phasenumwandlung des Beschichtungsmaterials auf dem Weg zur Oberfläche durchgeführt, wobei das Aluminium-Siliziumpulver im Laserstrahl verflüssigt wird. Beim Erstarren auf der Oberfläche soll fein disperses Silizium, sogenanntes Primärsilizium, freigesetzt werden. In the known method, there is therefore no alloying of the Powder in the surface layer of the component, but it will a phase change of the coating material on the way to Surface performed, the aluminum-silicon powder in Laser beam is liquefied. When solidifying on the surface should release finely dispersed silicon, so-called primary silicon become.
Je nach Abkühlgeschwindigkeit sollen hierbei Siliziumkristalle in der Größenordnung von 1 bis 5 µm erzeugt werden. Die dazu erforderliche schnelle Abkühlung kann aber in der Praxis nicht erreicht werden, da die Energie des Laserstrahls auf das zu beschichtende Bauteil einwirkt. Die Substratoberfläche wird somit sehr heiß und kann daher die Wärme der auftreffenden Si-Schmelze nicht schnell genug abführen, so daß keine kristalline Phase und keine Primärkristalle sondern amorphe Phasen entstehen.Depending on the cooling rate, silicon crystals should be used be produced in the order of 1 to 5 microns. The one In practice, however, the rapid cooling required cannot be achieved because the energy of the laser beam is towards that coating component acts. The substrate surface is therefore very hot and can therefore heat the impacting Si melt not dissipate quickly enough so that no crystalline Phase and no primary crystals but amorphous phases.
Gemäß dem Ausführungsbeispiel des BMW-Patents werden bei einer
aufgetragenen Schichtdicke von 3 mm zur Erzielung einer glatten,
ebenen Oberfläche des Schichtmaterials etwa 50 % abgetragen
(Spalte 6, Zeilen 10 bis 15). Dies bedeutet einen hohen Abtragsverlust,
zu dem noch eine ungenutzte Randzone durch eine hohe
Welligkeit des tröpfchenförmig aufgetragenen Materials als nachteilig
hinzugerechnet werden muß.According to the embodiment of the BMW patent, a
applied layer thickness of 3 mm to achieve a smooth,
flat surface of the layer material removed about 50%
(
Aus der EP-A-0 221 276 ist es ferner bekannt, eine Aluminiumlegierung durch Umschmelzen ihrer Randschichten mit Laserenergie verschleißbeständiger auszubilden. Dabei wird auf die Oberfläche eine Schicht aus einem Binder, pulverförmigen Silizium, Kupfer und Titancarbid aufgebracht und anschließend mit dem Laser in die Oberfläche eingeschmolzen. Die Zugaben an TIC betragen in den Ausführungsbeispielen zwischen 5 bis 30 % und bewirken eine beträchtliche Zunahme in der Oberflächenhärte.From EP-A-0 221 276 it is also known an aluminum alloy by remelting their peripheral layers with laser energy train more wear resistant. Doing so will surface a layer of a binder, powdered silicon, copper and titanium carbide and then lasered in melted the surface. The additions to TIC are in the embodiments between 5 to 30% and cause a considerable increase in surface hardness.
Unter tribologischen Aspekten ist jedoch durch die extrem hohe Abkühlgeschwindigkeit beim Laserumschmelzen zwar eine hohe Kornfeinheit, jedoch keine ausreichende Ausbildung des Primärsiliziums bei diesem Verfahren erreichbar. Daher ist das Laserumschmelzen für die Herstellung von Zylinderlaufflächen von Hubkolbenmaschinen aus AlSi-Legierungen mit tragenden Plateaus aus Primärsilizium und zurückgesetzten, Schmierstoffen enthaltenden Bereichen ungeeignet. From a tribological point of view, however, the extremely high Cooling rate during laser remelting is a high grain size, however, insufficient formation of the primary silicon achievable with this procedure. Hence the laser remelting for the production of cylinder liners from Reciprocating piston machines made of AlSi alloys with load-bearing plateaus made of primary silicon and reset, containing lubricants Areas unsuitable.
In der EP 0 411 322 A1 wird ein Verfahren zum Herstellung verschleißfester Oberflächen an Bauteilen aus einer AlSi-Legierung beschrieben, das von der zuvor erwähnten EP 0 221 276 ausgeht, wobei jedoch der Schicht vor dem Lasereinschmelzen ein Impfmittel (Keimbildner) für primäre Siliziumkristalle zugegeben wird. Als Impfmittel bzw. Keimbildner werden folgende Substanzen genannt: Siliziumnitrid, Siliziumcarbid, Titancarbid, Titannitrid, Borcarbid und Titanborid.EP 0 411 322 A1 describes a method for producing more wear-resistant Surfaces on components made of an AlSi alloy described, which is based on the aforementioned EP 0 221 276, however, the layer prior to laser melting a vaccine (Nucleating agent) added for primary silicon crystals becomes. The following substances are used as inoculants or nucleating agents called: silicon nitride, silicon carbide, titanium carbide, titanium nitride, Boron carbide and titanium boride.
In einem bevorzugten Ausführungsbeispiel wird die Beschichtung in Form der Siebdrucktechnik als Abziehfolie hergestellt und auf die Oberfläche des betreffenden Bauteiles aufgebracht. Die Dicke der Schicht kann vorzugsweise 200 µm und die Einschmelztiefe 400 bis 600 µm betragen. Es wird ein linienförmig fokussierter Laserstrahl in inerter Atmosphäre verwendet, um das Einschmelzen mit einer Einschmelztiefe von 400 µm zu verwirklichen. Der Siliziumanteil in der legierten Zone betrug im Beispiel 25 % bei einem Nickelanteil von 8 % (Härte über 250 HV).In a preferred embodiment, the coating produced in the form of screen printing technology as a peel-off film applied the surface of the component in question. The fat the layer can preferably be 200 μm and the melting depth 400 up to 600 µm. It becomes a line-focused laser beam used in an inert atmosphere to melt down with a melting depth of 400 µm. The silicon content in the alloyed zone was 25% in the example a nickel content of 8% (hardness above 250 HV).
Wie schon zuvor beschrieben ist es bei den letztgenannten Verfahren des Umschmelzens bzw. Einschmelzens erforderlich, eine Kühlung während des Auftragens einer Schicht auf die Matrixlegierung durchzuführen, um die gewünschten feindispersen Ausscheidungen des Primärsiliziums zu erreichen. Wegen der zugesetzten Impfmittel können Reaktionen mit der Aluminiumoberfläche erfolgen. Außerdem sind die Beschichtungsmaßnahmen bei gekrümmten Oberflächen nicht immer anwendbar.As already described, it is the latter method remelting or melting required, one Cooling while applying a layer on the matrix alloy to perform the desired finely dispersed excretions of the primary silicon. Because of the added Vaccines can cause reactions with the aluminum surface respectively. In addition, the coating measures for curved Surfaces not always applicable.
Aus der EP 0 622 476 A1 ist ein Metallsubstrat mit laserinduzierter MMC-Beschichtung bekannt. Die MMC-Schicht weist eine Schichtdicke zwischen 200 µm und 3 mm auf und enthält homogen verteilte SIC-Partikel, wobei bevorzugt bis zu 40 Gewichtsprozent SiC als homogen verteilte SIC-Partikel in der MMC-Schicht enthalten sind. Zur Herstellung wird das Pulvergemisch, enthalten. SiC-Pulver und vorlegiertes AlSi-Pulver in einem Laserstrahl erhitzt, wobei der für die Herstellung einer homogenen Legierung aus dem Pulvergemisch erforderliche Wärmegehalt durch das auf die Substrat auftreffende Pulver herbeigeführt wird. Produkte mit Hartmetallstoffen wie SiC weisen eine sehr hohe Härte auf, die für das Verschleißverhalten der Kolbenringe ungünstig sind. Außerdem ist die Bearbeitung sehr aufwendig, da die oberste Schicht der Keramikpartikel abgetragen werden muß, um eine funktionsfähige, splitterfreie Lauffläche zu erreichen.EP 0 622 476 A1 describes a metal substrate with a laser-induced one MMC coating known. The MMC layer has one Layer thickness between 200 µm and 3 mm and contains homogeneous distributed SIC particles, preferably up to 40 percent by weight SiC as homogeneously distributed SIC particles in the MMC layer are included. The powder mixture is included for production. SiC powder and pre-alloyed AlSi powder in one laser beam heated, the for the preparation of a homogeneous Alloy from the powder mixture required heat content the powder impinging on the substrate is brought about. Products with hard metal materials such as SiC have a very high Hardness that is unfavorable for the wear behavior of the piston rings are. In addition, the processing is very complex because the top layer of the ceramic particles has to be removed, to achieve a functional, splinter-free tread.
Aufgabe der vorliegenden Erfindung ist es daher, einen Leichtmetallzylinderblock
mit mindestens einer verschleißfesten tribologisch
beanspruchbaren Lauffläche zu entwickeln, bei der die
Oberflächenschicht aus 5 bis 20 % feindispersem Primärsilizium
besteht, das im Übergang zur Matrixlegierung eine geringe Randzonenbreite
aufweist und das in der Übergangszone frei von Fehlstellen
und Oxideinschlüssen ist.
Das zur Herstellung des Leichtmetallzylinderblocks eingesetzte
Verfahren soll mit weniger Verfahrensschritten auskommen, wobei
auf eine chemische Nachbearbeitung vollständig verzichtet werden
soll.The object of the present invention is therefore to develop a light metal cylinder block with at least one wear-resistant tribologically loadable running surface, in which the surface layer consists of 5 to 20% finely dispersed primary silicon, which has a small edge zone width in the transition to the matrix alloy and which is free of defects in the transition zone and is oxide inclusions.
The process used to manufacture the light metal cylinder block should manage with fewer process steps, and chemical post-processing should be completely dispensed with.
Die Aufgabe wird durch die in den Patentansprüchen angegebenen Merkmale gelöst. Im folgenden werden mehrere Ausführungsbeispiele angegeben, wobei es sich um bevorzugte Anwendungsfälle des erfindungsgemäßen Laserlegierens handelt.The object is achieved by those specified in the claims Features solved. The following are several embodiments indicated, which are preferred use cases of laser alloying according to the invention.
Zunächst wird eine Vorrichtung zur Innenraumbeschichtung eines Leichtmetallmotorblockes aus Aluminium oder einer Magnesiumlegierung beschrieben, wobei eine Sonde in den Zylinder eines Motorblocks eingesenkt wird und gleichzeitig reines Siliziumpulver zugeführt werden kann. Die Sonde weist eine Pulverzuführung und eine Laserstrahleinrichtung auf.First, a device for coating the interior of a Light metal engine block made of aluminum or a magnesium alloy described, with a probe in the cylinder of a Engine blocks are sunk and at the same time pure silicon powder can be supplied. The probe has a powder feed and a laser beam device.
Durch einen an der Sonde angeordneten Drehantrieb werden eine Pulverausbringungsdüse und ein Energiestrahl auf den Innenraum bzw. die Lauffläche des Leichtmetallmotorblockes gelenkt. By means of a rotary drive arranged on the probe, a Powder application nozzle and an energy beam on the interior or steered the tread of the light metal engine block.
Mit dieser Vorrichtung soll das Einlegieren von Hartstoffteilchen in Form von Silizium über einen über die Lauffläche spiralig rotierenden Laserstrahl mit parallel zugeführten Siliziumteilchen erfolgen. Damit die Laserenergie sich über eine breite Spur auf die Matrixoberfläche verteilt, hat der Laserstrahl einen linienförmigen Fokus mit einer Spurbreite von vorzugsweise 2 bis 4 mm. Im Vergleich zu einer durch punktförmigen Laser erzeugten Oberfläche bildet sich beim Fokus kein wellenförmiges Profil, sondern ein flaches Band mit feindispersen Primärsiliziumteilchen aus. Das Band wird als Auflegierungszone bezeichnet, wobei es nur eine schmale Übergangszone (der Randzone) zwischen auflegierter Zone und dem Matrixmetall aufweist (siehe Figur 1).The purpose of this device is to alloy hard particles in the form of silicon over a spiral over the tread rotating laser beam with silicon particles fed in parallel respectively. So that the laser energy is spread over a wide range The laser beam has a track on the matrix surface a linear focus with a track width of preferably 2 to 4 mm. Compared to one with point laser generated surface does not form a wavy at the focus Profile, but a flat band with finely dispersed primary silicon particles out. The band is called the Alloy Zone, being just a narrow transition zone (the peripheral zone) between has alloyed zone and the matrix metal (see Figure 1).
Da das Pulver im Zeitpunkt kurz vor dem Auftreffen auf die Metallmatrixlegierung eine Kornstruktur besitzt und erst im Kontakt mit der Metallmatrixlegierung im Bereich des Laserstrahls innerhalb einer Kontaktzeit von 0,1 bis 0,5 sec aufgeschmolzen und einlegiert wird, läßt sich bei dem linienförmigen Fokus ein geringer Randzonenanteil von ca. 10 % erreichen. Die Laserspur wird in der Zylinderbohrung spiralisch abgesenkt, wobei im Bedarfsfalle auf eine Überlappung verzichtet werden kann, so daß die Nutzanteile praktisch gegeneinanderstoßen. Somit entsteht eine glatte, vollständig homogene Oberflächenschicht, die nur noch durch eine Feinbearbeitung zur Beseitigung einer leichten Welligkeit fertig bearbeitet werden muß.Because the powder just before it hits the metal matrix alloy has a grain structure and only in contact with the metal matrix alloy in the area of the laser beam melted within a contact time of 0.1 to 0.5 sec and is alloyed, can be in the linear focus achieve a low edge zone share of approx. 10%. The laser track is lowered spirally in the cylinder bore, if necessary an overlap can be dispensed with, so that the useful parts practically collide. Thus arises a smooth, completely homogeneous surface layer that only still by finishing to remove a slight Ripple must be finished.
Als Beispiel für die erfindungsgemäße Bearbeitung bei der Herstellung eines Leichtmetallzylinderblocks mit mindestens einer verschleißfesten, tribologisch optimierten Zylinderlauffläche wird von folgenden Bearbeitungsschritten ausgegangen:As an example of the processing according to the invention during manufacture a light alloy cylinder block with at least one wear-resistant, tribologically optimized cylinder running surface the following processing steps are assumed:
Zunächst wird eine Auflegierungszone enthaltend Primärsilizium mit einer mittleren Schichtdicke von 300 bis 750 µm in der Matrixlegierung erzeugt. Die exakten Werte der Schichtdicke hängen von verschiedenen Einflußgrößen, wie Verfahrensparameter, Genauigkeit der Vorrichtungspositionierung und Maßtoleranz des Gußteils ab. Es wird daher im folgenden bei allen Dickenangaben von einer "mittleren" Schichtdicke gesprochen, wobei der Toleranzbereich sehr eng gehalten werden kann, da die Vorrichtung am Bauteil zentriert werden kann.First, an alloy zone containing primary silicon with an average layer thickness of 300 to 750 µm in the matrix alloy generated. The exact values of the layer thickness depend of various influencing factors, such as process parameters, accuracy the device positioning and dimensional tolerance of the casting from. It is therefore in the following for all thicknesses of spoken of an "average" layer thickness, the tolerance range can be kept very close since the device on Component can be centered.
Die Ausgangsschichtdicke von 300 bis 750 µm wird dann in einem
weiteren Bearbeitungsschritt auf die gewünschte Endschichtdicke
durch eine Feinbearbeitung mit einem Abtrag bis zu 150 µm, wie
z.B. durch Honen etc., gebracht. Die nach dem erfindungsgemäßen
Verfahren erreichte Endschichtdicke liegt im Bereich von 150 bis
650 µm. Dabei handelt es sich um eine reine Diffusionsschicht,
die durch eine besondere in den Ansprüchen 1 und 2 definierte
Gefügestruktur gekennzeichnet ist.The initial layer thickness of 300 to 750 microns is then in one
further processing step to the desired final layer thickness
by fine machining with a removal of up to 150 µm, such as
e.g. by honing etc. The according to the invention
The final layer thickness achieved in the process is in the range from 150 to
650 µm. It is a pure diffusion layer,
that defined by a special one in
Mit der Steuerung der Pulverzufuhr, dem Vorschub des Laserstrahls und der zugeführten Laserenergie lassen sich die Ausscheidungsgrößen der Hartphasen einstellen. Bei Ausscheidungsgrößen kleiner 10 µm verringert sich die Zerstörungstiefe in der mechanischen Endbearbeitung der Hartphasen, so daß die bisher erforderlichen Bearbeitungszugaben für die Entfernung der zerstörten Hartphasen sich deutlich reduzieren lassen. (Die Zerstörungstiefe wird durch die in der obersten Schicht enthaltenden, nicht fest eingebundenen Hartphasen bestimmt.)With the control of the powder supply, the feed of the laser beam and the supplied laser energy can be the excretion variables adjust the hard phases. For excrement sizes less than 10 µm reduces the depth of destruction in the mechanical finishing of the hard phases, so that the previously required processing allowances for the removal of the destroyed Hard phases can be significantly reduced. (The depth of destruction is contained in the top layer, hard phases not firmly integrated.)
Durch das Einlegieren mit dem Laserstrahl wird die Oberfläche gehärtet, wobei Härtewerte der Oberflächenschicht von mindestens 160 HV erreicht werden. Infolge der guten Härtung lassen sich die Laseroberflächen direkt honen. Bisher erforderliche zusätzliche mechanische oder chemische Bearbeitungsschritte zur Freistellung der Hartphasen sind ebenfalls nicht mehr erforderlich. Damit ist das bisher erforderliche Ausbohren der Zylinderbeschichtungen nicht mehr erforderlich, da die Oberflächenwelligkeit je nach Überlappung der streifenförmigen Auflegierungszone vernachlässigbar da sehr gering ist. The surface is created by alloying with the laser beam hardened, with hardness values of the surface layer of at least 160 HV can be reached. As a result of the good hardening, honing the laser surfaces directly. Additional required so far mechanical or chemical processing steps for exemption the hard phases are also no longer required. This is the previously required drilling of the cylinder coatings no longer required because of the surface ripple depending on the overlap of the striped alloy zone negligible because it is very low.
Im folgenden wird die erfindungsgemäß erzielbare Oberflächenstruktur auf einer Motorblock-Lauffläche anhand eines Vergleichsbeispieles näher erläutert. Es zeigen:
- Fig. 1
- Prinzipbild einer erfindungsgemäß ausgebildeten Beschichtungseinrichtung im Teilquerschnitt;
- Fig. 2
- Prinzipbild einer erfindungsgemäß erzeugten Oberflächenschicht;
- Fig. 3
- Vergleichsbeispiel mit einer anderen Oberflächenstruktur;
- Fig. 4
- Querschnitt an einem Gußteil im Bereich der laserlegierten Zone.
- Fig. 1
- Block diagram of a coating device designed according to the invention in partial cross section;
- Fig. 2
- Block diagram of a surface layer produced according to the invention;
- Fig. 3
- Comparative example with a different surface structure;
- Fig. 4
- Cross-section on a casting in the area of the laser-alloyed zone.
Nach Figur 1 besteht die erfindungsgemäß ausgebildete Beschichtungseinrichtung
aus einer Pulverzuführung 1, die an ihrem Ende
1a eine auf die Lauffläche 5 gerichtete Düse 1b aufweist.According to Figure 1, the coating device designed according to the invention
from a powder feeder 1 at its end
1a has a
Die Energiezufuhr erfolgt über eine Laserstrahleinrichtung 2,
einem Fokussiersystem 3 und einem Umlenkspiegel 4, die dafür
sorgt, daß der Laserstrahl 6 erst auf der Laufflächenoberfläche
7 zusammen mit dem Pulver auftrifft.The energy is supplied via a
Nach den bekannten optischen Gesetzen wird der Laserstrahl 6
linienförmig, vorzugsweise als X, I oder 8 fokussiert und dann
beispielsweise durch Kippen des Spiegels auf der Laufflächenoberfläche
7 abgebildet. Durch die Form der Abbildung kann der
Energieeintrag gesteuert werden, so daß das Ausscheidungsgefüge
in seiner Ausprägung an den Rändern beeinflußbar ist.According to the known optical laws, the
Durch Drehung des Spiegels 4 wandert der Laserstrahl 6 über die
Laufflächenoberfläche 7, so daß sich ein streifenförmiges Band
ergibt. Wenn dabei gleichzeitig eine Vorschubbewegung in Richtung
der Zylinderachse 8 erfolgt, ergibt sich durch Überlagerung
der beiden Bewegungen eine spiralförmige Beschichtung der Laufflächenoberfläche
7. Die rotierende und die translatorische
Bewegung in Richtung der Zylinderachse 8 sollten dabei so aufeinander
abgestimmt werden, daß die Windungen der Spirale dicht
aneinanderliegen, so daß sich eine geschlossene Auflegierungszone
ergibt.By rotating the mirror 4, the
In Figur 2 ist die erfindungsgemäß mit einem Linienfokus erzeugte
Auflegierungszone 10, bestehend aus einer ausscheidungsreichen
Zone 11 und zwei seitlich angeordneten ausscheidungsarmen
Zonen 12, 13, dargestellt. Figur 2 zeigt den Zustand der
Auflegierungszone unmittelbar nach der Laserbeschichtung, wobei
zu erkennen ist, daß der Anteil der ausscheidungsarmen Zone LAL,
bezogen auf die nutzbare Länge LNL der ausscheidungsreichen Zone,
relativ gering ist. Die entsprechenden Bereiche in Figur 3 sind
mit LAK bezeichnet, die zu den Randzonen 15, 16, 17 gehören.FIG. 2 shows the
In Figur 3 sind als Vergleichsbeispiel drei mit herkömmlichem
Kreisfokus hergestellte Auflegierungszonen dargestellt, wobei
die Beschichtungsbreite bei dem Verfahren mit Linienfokus und
bei dem Verfahren mit Kreisfokus annähernd übereinstimmen. Man
erkennt, daß die nutzbare Länge LNK des ausscheidungsreichen
Gefüges bei dem Verfahren mit Kreisfokus wesentlich geringer ist
als die nutzbare Länge beim Linienfokus LNL. Ferner ist die nutzbare
Tiefe der gehärteten Oberflächenschicht beim Kreisfokus
wesentlich geringer als beim Linienfokus, da beim Kreisfokus ein
ausscheidungsarmes Gefüge bis in tiefere Zonen des Zylinderblockgefüges
reicht. Dies ist im Querschnitt nach Figur 3 durch
die breiten Randzonen 15, 16, 17 veranschaulicht.In FIG. 3, three alloy zones produced with a conventional circular focus are shown as a comparative example, the coating width approximately matching in the method with line focus and in the method with circular focus. It can be seen that the usable length L NK of the structure rich in excretions in the method with circular focus is considerably less than the usable length in the line focus L NL . In addition, the usable depth of the hardened surface layer in the circular focus is considerably less than in the line focus, since in the circular focus a structure with little elimination extends into deeper zones of the cylinder block structure. This is illustrated in the cross section according to FIG. 3 by the
Da bei gleicher Eindringtiefe die nutzbare Tiefe im vergleichsbeispiel nach Figur 3 geringer ist als im erfindungsgemäßen Beispiel nach Figur 2 ist die Qualität der Beschichtung nach dem Vergleichsbeispiel ungünstiger. Ferner ist der erforderliche Abtrag ΔHWK im Vergleichsbeispiel bei gleicher Bearbeitungstiefe wie im Erfindungsbeispiel wesentlich höher (ΔHWL), da der Kreisfokus eine wellige Oberflächenschicht erzeugt, die im Bereich der Lauffläche einen geringeren nutzbaren Materialanteil MK aufweist als ein entsprechender Laufflächenabschnitt gemäß Figur 2 (LNL).Since the usable depth in the comparative example according to FIG. 3 is less than the same depth of penetration in the example according to the invention according to FIG. 2, the quality of the coating according to the comparative example is less favorable. Furthermore, the required removal ΔH WK in the comparative example with the same machining depth as in the inventive example is significantly higher (ΔH WL ), since the circular focus creates a wavy surface layer which has a lower usable material proportion M K in the area of the tread than a corresponding tread section according to FIG. 2 ( L NL ).
Der nutzbare Materialanteil ist im Erfindungsbeispiel LNL, während MK als Summe der Einzelwerte LNK1, LNK2, LNK3 gebildet wird.In the example of the invention, the usable material fraction is L NL , while M K is formed as the sum of the individual values L NK1 , L NK2 , L NK3 .
Der erfindungsgemäße Leichtmetallzylinderblock hat daher eine verschleißfestere Zylinderlauffläche, die durch gleichmäßige Verteilung der feinen Si-Primärausscheidungen tribologisch optimiert ist und durch linienförmige Fokussierung und überlappende Beschichtung mit deutlich reduziertem Fertigungsaufwand herstellbar ist.The light alloy cylinder block according to the invention therefore has a more wear-resistant cylinder running surface thanks to uniform Distribution of the fine primary Si precipitates optimized tribologically is and by linear focus and overlapping Coating can be produced with significantly reduced production costs is.
Es wird anhand des Gefügebildes in Figur 4 verdeutlicht. Es handelt sich um ein Schliffbild mit der Vergrößerung 200 : 1, wobei im rechten Bildteil A eine Gußlegierung vom Typ AlSi9Cu3 und im linken Bildteil B eine tribologisch optimierte Oberflächenschicht mit feindispersen Primär-Silizium-Ausscheidungen zu erkennen ist. Der Primärsiliziumanteil beträgt im vorliegenden Beispiel 10 %, der Primärphasendurchmesser 4,4 µm und der Abstand der Si-Primärphasen 13 µm.It is illustrated using the microstructure in FIG. 4. It is a micrograph with a magnification of 200: 1, in the right part of the picture A a casting alloy of the type AlSi9Cu3 and in the left part B a tribologically optimized surface layer with finely dispersed primary silicon precipitates is recognizable. The primary silicon content here Example 10%, the primary phase diameter 4.4 µm and the distance the Si primary phases 13 µm.
Für die Belastungsfähigkeit des neuen Werkstoffs ist besonders von Bedeutung die Anbindung der Auflegierungszone B an das Matrixgefüge A. Am Schliffbild 4 ist erkennbar, daß in der Übergangszone C keine Oxide oder andere Fehlstellen vorliegen. Dieses beruht darauf, daß die Auflegierungszone quasi "insitu" aus dem Matrixgefüge gebildet wurde und somit ein einheitlicher Werkstoff mit unterschiedlichen Zusammensetzungen im Bereich A, B entstanden ist. What is special about the resilience of the new material of importance is the connection of the alloy zone B to the matrix structure A. On micrograph 4 you can see that in the transition zone C there are no oxides or other defects. This is based on the fact that the alloy zone is quasi "in situ" the matrix structure was formed and thus a uniform one Material with different compositions in area A, B was created.
- 11
- Pulverzuführungpowder feed
- 1a1a
- Ende der PulverzuführungEnd of powder feed
- 1b1b
- Düsejet
- 22
- Laserstrahleinrichtunglaser-beam device
- 33
- Fokussiersystemfocusing
- 44
- Umlenkspiegeldeflecting
- 55
- Laufflächetread
- 66
- Laserstrahllaser beam
- 77
- LaufflächenoberflächeTread surface
- 88th
- Zylinderachsecylinder axis
- 99
- --
- 1010
- Auflegierungszonealloyed
- 1111
- Ausscheidungsreiche ZoneEliminating zone
- 12,1312.13
- Ausscheidungsarme ZoneElimination-poor zone
- 1414
- --
- 15,16,1715,16,17
- Randzonenperipheral zones
- MK M K
- Materialanteilmaterial ratio
- LNK L NK
- Nutzbare Länge des ausscheidungsreichen GefügesUsable length of the structure rich in excretions
- LNL L NL
- Nutzbare Länge der ausscheidungsreichen ZoneUsable length of the elimination zone
- LAL L AL
- Anteil der ausscheidungsarmen ZoneProportion of the low-excretion zone
- LAK L AK
- Bereiche, die zu den Randzonen gehörenAreas that belong to the marginal zones
- ΔHWK ΔH WK
- Abtrag VergleichsbeispielRemoval of comparative example
- ΔHWL ΔH WL
- Abtrag ErfindungsbeispielRemoval example of invention
- AA
- Matrixgefügematrix structure
- BB
- Auflegierungszonealloyed
- CC
- ÜbergangszoneTransition zone
Claims (16)
- An aluminum cylinder block having at least one wear-resistant cylinder running face, which has a minimum hardness of 160 HV and is tribologically optimized, whereinthe aluminum cylinder block is made of an aluminum matrix alloy (matrix microstructure A) and, in the post-processed state, has a surface layer (matrix microstructure B), 150 µm to 650 pm thick, which is formed as an alloyed-on zone from the matrix microstructure (matrix microstructure A) of the aluminum matrix alloy by alloying in finely dispersed primary silicon precipitates in situ, by guiding a laser beam in a linearly focused way in a strip width of at least 2 mm, measured transversely to the advance direction, over the aluminum matrix surface, and the silicon powder not until in the incidence point of the laser beam being heated in a contact time of 0.1 to 0.5 seconds to melting temperature and, at the same time, being alloyed into the aluminum matrix,the primary silicon is made of uniformly distributed, round-shaped grains having an average grain diameter between 1 µm and 10 µm, andthe surface layer contains 10 % to 14 % AlSi eutectic, 5 % to 20 % primary silicon, and the remainder pure Al phase.
- The aluminum cylinder block according to Claim 1, characterized in that the Si primary phases are distributed in an interval of 1 to 5 primary phase diameters in the surface.
- The aluminum cylinder block according to one of the preceding claims, characterized in that the primary silicon is alloyed into the matrix alloy in a strip-shaped alloyed-on zone, the strips running in a spiral over the cylinder running face.
- The aluminum cylinder block according to Claim 3, characterized in that the strip thickness is 2 to 4 mm.
- The aluminum cylinder block according to one of the preceding claims, characterized in that, for multiple alloyed-on zones positioned next one another, overlap of the strips is provided and the width of the overlap is 5 % to 10 %.
- The aluminum cylinder block according to one of the preceding claims, characterized in that the finely dispersed surface layer into which the primary silicon precipitates are alloyed consists of an alloyed-on zone (11), which is rich in precipitates, and an edge zone (12, 13), which is poor in precipitates.
- A method of producing an aluminum cylinder block having at least one wear-resistant and tribologically optimized cylinder running face,in which the aluminum block is cast from an aluminum matrix alloy in a gravity, low-pressure, or pressure diecasting method, andin which surface processing is subsequently performed in the form of laser and powder beams occurring parallelly to one another forming a surface layer by alloying Si powder into the aluminum matrix in such a way that a finely dispersed alloyed-on zone containing primary silicon precipitates results,the laser beam being guided in a linearly focused way in a strip width of at least 2 mm, measured transversely to the advance direction, over the aluminum matrix and the Si powder not until in the incidence point of the laser beam being heated in a contact time of 0.1 to 0.5 seconds to the melting temperature and at the same time being alloyed into the aluminum matrix, andthe advance speed of the laser beam and powder beam being controlled in such a way that the primary silicon is present in the surface layer over an average layer thickness of 300 µm to 750 µm.
- The method according to Claim 7, characterized in that in the incidence point the aluminum matrix alloy is completely melted to a depth of at least 350 µm and is converted into the plasma state at the aluminum matrix surface.
- The method according to one of Claims 7 or 8, characterized in that, in the instant shortly before the incidence on the metal matrix alloy, the silicon powder has a grain structure and the powder is melted and alloyed in not until upon contact with the metal matrix alloy in the region of the laser beam within a contact time of 0.1 to 0.5 seconds.
- The method according to one of Claims 7 through 9, characterized in that for a focused incidence area of the laser beam of 1 mm2 to 10 mm2 and a laser light output of 3 to 4 kW, the advance speed of the laser beam and powder beam is 0.8 m to 4.0 m per minute.
- The method according to one of Claims 7 through 10, characterized in that the laser beam rotates with its focus in a spiral on the inner running face of a hollow cylinder and a strip-shaped alloyed-on zone containing primary silicon is formed at the same time by adding a Si powder.
- The method according to one of Claims 7 through 11, characterized in that the average processing depth in the alloyed-on zone is 750 µm.
- The method according to one of Claims 7 through 12, characterized in that the hard phases of the alloyed-on zone are exposed by mechanical processing, the abrasion of the uppermost layer being less than 30 % of the total layer thickness.
- The method according to one of Claims 7 through 13, characterized in that the alloyed-on zone is honed directly without intermediate processing.
- A device for performing the method of a running face coating of hollow cylinders, having a powder feed device (1), having a laser beam device (2), and having a focusing system (3), which has a deflection mirror (4), characterized in thatthe powder feed (1) and laser beam device (2) are guided parallel to one another in the radial and axial directions of the hollow cylinder,the focusing system (3) has a linear beam. outlet having a beam width of 2.0 mm to 2.5 mm, andthe powder feed is provided with a dosing device, via which the volume flow of the powder is adjustable as a function of the advance speed of the laser beam.
- The device according to Claim 15, characterized in that the focusing system (3) has an X-shaped, I-shaped, or 8-shaped focus shape, which allows an elevated energy emission at the upper and lower edge zones in comparison to the middle focus region.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE19915038 | 1999-04-01 | ||
DE19915038A DE19915038A1 (en) | 1999-04-01 | 1999-04-01 | Light metal cylinder block, method for its production and device for carrying out the method |
Publications (2)
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EP1041173A1 EP1041173A1 (en) | 2000-10-04 |
EP1041173B1 true EP1041173B1 (en) | 2004-05-26 |
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EP00105126A Expired - Lifetime EP1041173B1 (en) | 1999-04-01 | 2000-03-10 | Light metal cylinder block, method for making it and apparatus for carrying out the process |
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US (3) | US6390050B2 (en) |
EP (1) | EP1041173B1 (en) |
JP (1) | JP3467744B2 (en) |
KR (1) | KR100388150B1 (en) |
AT (1) | ATE267891T1 (en) |
AU (1) | AU775660B2 (en) |
BR (1) | BR0006013B1 (en) |
CA (1) | CA2332944C (en) |
CZ (1) | CZ294043B6 (en) |
DE (2) | DE19915038A1 (en) |
ES (1) | ES2222122T3 (en) |
HU (1) | HU222858B1 (en) |
PL (1) | PL193699B1 (en) |
RU (1) | RU2212472C2 (en) |
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DE19630197C2 (en) * | 1996-07-26 | 1999-10-14 | Kolbenschmidt Ag | Process for producing wear-resistant surfaces on components made of aluminum materials and device for carrying it out; Pistons for internal combustion engines |
DE19643029A1 (en) | 1996-10-18 | 1998-04-23 | Bayerische Motoren Werke Ag | Method for coating an internal combustion engine component made of an aluminum alloy with silicon |
DE19711756A1 (en) * | 1997-03-21 | 1998-09-24 | Audi Ag | Coating light metal alloy workpiece |
JP3409631B2 (en) * | 1997-04-15 | 2003-05-26 | 日産自動車株式会社 | Method of overlaying with laser beam and overlaying structure |
DE19915038A1 (en) * | 1999-04-01 | 2000-10-26 | Vaw Ver Aluminium Werke Ag | Light metal cylinder block, method for its production and device for carrying out the method |
-
1999
- 1999-04-01 DE DE19915038A patent/DE19915038A1/en not_active Withdrawn
-
2000
- 2000-03-10 CA CA002332944A patent/CA2332944C/en not_active Expired - Fee Related
- 2000-03-10 AU AU32882/00A patent/AU775660B2/en not_active Ceased
- 2000-03-10 WO PCT/EP2000/002125 patent/WO2000060136A1/en active IP Right Grant
- 2000-03-10 EP EP00105126A patent/EP1041173B1/en not_active Expired - Lifetime
- 2000-03-10 AT AT00105126T patent/ATE267891T1/en not_active IP Right Cessation
- 2000-03-10 JP JP2000609624A patent/JP3467744B2/en not_active Expired - Fee Related
- 2000-03-10 BR BRPI0006013-5A patent/BR0006013B1/en not_active IP Right Cessation
- 2000-03-10 RU RU2000133330/02A patent/RU2212472C2/en not_active IP Right Cessation
- 2000-03-10 DE DE50006550T patent/DE50006550D1/en not_active Expired - Fee Related
- 2000-03-10 KR KR10-2000-7012800A patent/KR100388150B1/en not_active IP Right Cessation
- 2000-03-10 ES ES00105126T patent/ES2222122T3/en not_active Expired - Lifetime
- 2000-03-29 CZ CZ20001135A patent/CZ294043B6/en not_active IP Right Cessation
- 2000-03-30 PL PL339334A patent/PL193699B1/en unknown
- 2000-03-31 HU HU0001361A patent/HU222858B1/en not_active IP Right Cessation
- 2000-11-08 ZA ZA200006437A patent/ZA200006437B/en unknown
- 2000-11-30 US US09/727,366 patent/US6390050B2/en not_active Expired - Fee Related
-
2001
- 2001-11-14 US US09/992,797 patent/US6575130B2/en not_active Expired - Fee Related
-
2002
- 2002-06-12 US US10/171,028 patent/US6797916B2/en not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105201809A (en) * | 2014-06-20 | 2015-12-30 | 中联重科股份有限公司 | Concrete pump vehicle and detection device, system and method for detecting pumping efficiency of concrete pump |
CN105201809B (en) * | 2014-06-20 | 2017-06-09 | 中联重科股份有限公司 | Concrete mixer and detect detection means, system, the method for its pumping efficiency |
Also Published As
Publication number | Publication date |
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AU775660B2 (en) | 2004-08-12 |
CZ20001135A3 (en) | 2000-12-13 |
JP3467744B2 (en) | 2003-11-17 |
US6575130B2 (en) | 2003-06-10 |
KR20010043633A (en) | 2001-05-25 |
US6390050B2 (en) | 2002-05-21 |
US6797916B2 (en) | 2004-09-28 |
AU3288200A (en) | 2000-10-23 |
US20020153359A1 (en) | 2002-10-24 |
KR100388150B1 (en) | 2003-06-19 |
CZ294043B6 (en) | 2004-09-15 |
WO2000060136A1 (en) | 2000-10-12 |
RU2212472C2 (en) | 2003-09-20 |
PL339334A1 (en) | 2000-10-09 |
CA2332944C (en) | 2005-05-24 |
BR0006013B1 (en) | 2011-02-22 |
JP2002541322A (en) | 2002-12-03 |
US20010003227A1 (en) | 2001-06-14 |
DE50006550D1 (en) | 2004-07-01 |
HUP0001361A2 (en) | 2000-12-28 |
EP1041173A1 (en) | 2000-10-04 |
PL193699B1 (en) | 2007-03-30 |
ATE267891T1 (en) | 2004-06-15 |
ES2222122T3 (en) | 2005-02-01 |
CA2332944A1 (en) | 2000-10-12 |
HU222858B1 (en) | 2003-12-29 |
ZA200006437B (en) | 2001-05-21 |
BR0006013A (en) | 2001-03-06 |
US20020033160A1 (en) | 2002-03-21 |
HU0001361D0 (en) | 2000-06-28 |
HUP0001361A3 (en) | 2001-02-28 |
DE19915038A1 (en) | 2000-10-26 |
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