EP0209179B1 - Process for manufacturing a mechanically alloyed composite powder - Google Patents
Process for manufacturing a mechanically alloyed composite powder Download PDFInfo
- Publication number
- EP0209179B1 EP0209179B1 EP86201163A EP86201163A EP0209179B1 EP 0209179 B1 EP0209179 B1 EP 0209179B1 EP 86201163 A EP86201163 A EP 86201163A EP 86201163 A EP86201163 A EP 86201163A EP 0209179 B1 EP0209179 B1 EP 0209179B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- grinding
- drum
- axis
- rotation
- 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
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/14—Mills in which the charge to be ground is turned over by movements of the container other than by rotating, e.g. by swinging, vibrating, tilting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
Definitions
- the invention relates to a method for producing a mechanically alloyed composite powder by grinding at least one metallic powder with at least one non-metallic powder or of metallic powders, the components of which are incomplete or not soluble in one another in the liquid state, in a drum mill with high energy input into the Regrind, possibly under control of the atmospheric and / or temperature conditions.
- the process of mechanical alloying allows the production of composite powders which consist of a dispersion of the finest metallic or non-metallic particles with a small particle spacing in a metallic matrix.
- the method is used for the production of such alloys, the components of which are not sufficiently soluble in one another in the molten state and / or which are subject to undesirable oozing out during solidification.
- metallic powders and one or more components such as. B. ground high-melting oxide powder or another metal powder in a drum mill with high energy input. The powder particles are rolled out and / or crushed into thin foils by the grinding media and at the same time the thin foils are welded together again and again.
- the solution to this problem consists in the use of a centrifugal mill with a cylindrical grinding drum which rotates about its own axis and at the same time rotates on a rotating circle with a constant rotation ratio around a fixed axis of rotation parallel to the axis of the grinding drum and with a drive mechanism for rotating the grinding drum the drum axis and for rotation on the rotation circle of the axis of the grinding drum is provided.
- the center of rotation lies within the cross section of the grinding vessel.
- the grinding vessel itself does not make any rotational movement about its own axis.
- centrifugal mill known from DE-OS 26 31 826, which has no critical speed, uses up to 30 times the acceleration due to gravity for grinding, in contrast to the mills described above in relation to the prior art. This leads to a much higher energy density in the mill and thus to a much smaller design.
- the centrifugal mill has so far been used for grinding mineral raw materials and other products to high fineness and specific surfaces due to their high efficiency and for fine grinding coal in coal / water or coal / oil suspensions.
- the very good mixing effect due to the high effective centrifugal forces has a positive effect here. Since there are no complicated sprockets and pinions, wear is correspondingly lower.
- the degree of filling is expediently 30 to 90% with a throughput of 0.01 to 1.5 t / h.
- the high plastic deformation is of predominant importance for the mechanically alloyed composite powders produced in the centrifugal mill, which results in the high hardness of the powder particles.
- the composite powders can be compacted by extrusion and, if necessary, then heat-treated.
Landscapes
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Crushing And Grinding (AREA)
Description
Die Erfindung betrifft ein Verfahren zur Herstellung eines mechanisch legierten Verbundpulvers durch Vermahlen von wenigstens einem metallischen Pulver mit wenigstens einem nichtmetallischen Pulver oder von metallischen Pulvern, deren Komponenten im flüssigen Zustand unvollkommen bzw. gar nicht ineinander löslich sind, in einer Trommelmühle mit hoher Energieeinbringung in das Mahlgut, ggf. unter Steuerung der atmosphärischen und/oder Temperatur-Bedingungen.The invention relates to a method for producing a mechanically alloyed composite powder by grinding at least one metallic powder with at least one non-metallic powder or of metallic powders, the components of which are incomplete or not soluble in one another in the liquid state, in a drum mill with high energy input into the Regrind, possibly under control of the atmospheric and / or temperature conditions.
Das Verfahren des mechanischen Legierens erlaubt die Herstellung von Verbundpulvern, die aus einer Dispersion feinster metallischer oder nichtmetallischer Teilchen mit niedrigem Teilchenabstand in einer metallischen Grundmasse bestehen. Das Verfahren wird zur Herstellung solcher Legierungen benutzt, deren Komponenten im schmelzflüssigen Zustand nicht hinreichend ineinander löslich sind und/oder die bei der Erstarrung einem unerwünschten Ausseigern unterliegen. Beim mechanischen Legieren werden metallische Pulver und ein oder mehrere Bestandteile, wie z. B. hochschmelzendes Oxidpulver oder ein anderes Metallpulver in einer Trommelmühle mit hoher Energieeinbringung vermahlen. Dabei werden die Pulverteilchen von den Mahlkörpern zu dünnen Folien ausgewalzt und/oder zerkleinert und gleichzeitig die dünnen Folien immer wieder miteinander verschweißt. Wegen der hohen energetischen Bedingungen stellt sich sehr schnell ein Gleichgewicht zwischen Verschweißen der Pulverteilchen und Zerkleinern ein, so daß im allgemeinen ein Verbundpulver gleichmäßiger Korngröße und sehr homogener Dispersion erzielt wird. Während der Vermahlung entstehen Verbundpulverteilchen identischer Zusammensetzung mit einem meist schichtenförmigen Aufbau, wobei die Dicke der einzelnen Schichten mit zunehmender Vermahlungsdauer immer mehr ab- und die Anzahl der Schichten je Pulverteilchen immer mehr zunimmt. Durch mechanisches Legieren lassen sich nicht nur duktile Metalle miteinander legieren, sondern auch spröde und/ oder nicht-metallische Komponenten in einer feinen Verteilung in eine metallische Matrix einbringen. Die Vermahlung erfolgt in konventionellen Kugelmühlen oder in Attritoren, ggf. unter Steuerung der atmosphärischen und/oder der Temperatur-Bedingungen. Um die gewünschte Homogenisierung des legierten Verbundpulvers zu erzielen, wird bei Einsatz einer Kugelmühle eine vergleichsweise sehr viel längere Behandlungsdauer als bei Einsatz eines Attritors benötigt. Beiden Mahlaggregaten ist jedoch gemein, daß es praktisch unmöglich ist, die mechanisch-technologischen Eigenschaften der mechanisch legierten Verbundpulverteilchen zu reproduzieren. Darüber hinaus unterliegen die Bauteile der genannten Mahlaggregate einem nicht unbeachtlichen Verschleiß.The process of mechanical alloying allows the production of composite powders which consist of a dispersion of the finest metallic or non-metallic particles with a small particle spacing in a metallic matrix. The method is used for the production of such alloys, the components of which are not sufficiently soluble in one another in the molten state and / or which are subject to undesirable oozing out during solidification. In mechanical alloying, metallic powders and one or more components, such as. B. ground high-melting oxide powder or another metal powder in a drum mill with high energy input. The powder particles are rolled out and / or crushed into thin foils by the grinding media and at the same time the thin foils are welded together again and again. Because of the high energetic conditions, an equilibrium between welding of the powder particles and comminution is established very quickly, so that in general a composite powder of uniform grain size and very homogeneous dispersion is achieved. Compound powder particles of identical composition with a mostly layered structure are formed during the grinding, the thickness of the individual layers decreasing more and more with increasing grinding time and the number of layers per powder particle increasing more and more. Mechanical alloying not only allows ductile metals to be alloyed with one another, but also brittle and / or non-metallic components can be introduced into a metallic matrix in a fine distribution. The grinding takes place in conventional ball mills or in attritors, possibly under control of the atmospheric and / or temperature conditions. In order to achieve the desired homogenization of the alloyed composite powder, a comparatively much longer treatment time is required when using a ball mill than when using an attritor. However, both grinding units have in common that it is practically impossible to reproduce the mechanical-technological properties of the mechanically alloyed composite powder particles. In addition, the components of the grinding units mentioned are subject to considerable wear.
Es ist die Aufgabe der vorliegenden Erfindung, einen Weg zu zeigen, der die Herstellung mechanisch legierter Verbundpulver in reproduzierbarer Art und Weise ermöglicht, mit dem eine kürzere Behandlungsdauer der Pulver bis zum Erreichen der gleichmäßigen Zusammensetzung des Verbundpulvers erreicht werden kann und durch den sich eine deutliche Senkung des Verschleisses der Bauteile der Mühle und der Mahlkörper erzielen läßt.It is the object of the present invention to show a way which enables the production of mechanically alloyed composite powders in a reproducible manner, with which a shorter treatment time of the powders can be achieved until the uniform composition of the composite powder is achieved, and by which a clear difference can be seen Reduce the wear of the components of the mill and the grinding media can be achieved.
Die Lösung dieser Aufgabe besteht in der Verwendung einer Zentrifugalmühle mit zylinderförmiger Mahltrommel, die um ihre eigene Achse rotiert und gleichzeitig auf einem Rotationskreis mit konstantem Drehverhältnis um eine feststehende und zu der Achse der Mahltrommel parallele Rotationsachse rotiert und mit einem Antriebsmechanismus für die Rotation der Mahltrommel um die Trommelachse und für die Rotation auf dem Rotationskreis der Achse der Mahltrommel versehen ist.The solution to this problem consists in the use of a centrifugal mill with a cylindrical grinding drum which rotates about its own axis and at the same time rotates on a rotating circle with a constant rotation ratio around a fixed axis of rotation parallel to the axis of the grinding drum and with a drive mechanism for rotating the grinding drum the drum axis and for rotation on the rotation circle of the axis of the grinding drum is provided.
Das Rotationszentrum liegt innerhalb des Mahlgefäßquerschnittes. Das Mahlgefäß selbst führt keine Rotationsbewegung um die eigene Achse aus.The center of rotation lies within the cross section of the grinding vessel. The grinding vessel itself does not make any rotational movement about its own axis.
Eine solche keine kritische Drehzahl besitzende aus der DE-OS 26 31 826 bekannte Zentrifugalmühle nutzt im Gegensatz zu den vorstehend zum Stand der Technik beschriebenen Mühlen das bis zu 30-fache der Erdbeschleunigung für die Mahlung aus. Dies führt zu einer wesentlich höheren Energiedichte in der Mühle und damit zu einer wesentlich kleineren Bauweise. Die Zentrifugalmühle ist bisher eingesetzt worden für die Vermahlung von mineralischen Rohstoffen und sonstigen Produkten auf hohe Feinheit und spezifische Oberflächen aufgrund des hohen Wirkungsgrades sowie zur Feinmahlung von Kohle in Kohle/Wasser- bzw. Kohle/Öl-Suspensionen. Hier wirkt sich der sehr gute Mischeffekt aufgrund der hohen wirksamen Zentrifugalkräfte positiv aus. Da komplizierte Zahnkränze und Ritzel fehlen, ist der Verschleiß entsprechend geringer. Verglichen mit einem Attritor wird eine Energieeinsparung bis zu 30 % erreicht und gleichzeitig die Behandlungsdauer gegenüber Kugelmühlen um 95 % gegenüber Rührwerksattritoren um über 50 % erniedrigt. Da die Mahltrommel ihre Orientierung im Raum beibehält, ist es relativ einfach, eine direkte oder indirekte Kühlung zu realisieren.Such a centrifugal mill known from DE-OS 26 31 826, which has no critical speed, uses up to 30 times the acceleration due to gravity for grinding, in contrast to the mills described above in relation to the prior art. This leads to a much higher energy density in the mill and thus to a much smaller design. The centrifugal mill has so far been used for grinding mineral raw materials and other products to high fineness and specific surfaces due to their high efficiency and for fine grinding coal in coal / water or coal / oil suspensions. The very good mixing effect due to the high effective centrifugal forces has a positive effect here. Since there are no complicated sprockets and pinions, wear is correspondingly lower. Compared to an attritor, energy savings of up to 30% are achieved and at the same time the treatment time compared to ball mills is reduced by 95% compared to agitator attritors by more than 50%. Since the grinding drum remains oriented in the room, it is relatively easy to implement direct or indirect cooling.
Zweckmäßigerweise beträgt der Füllungsgrad 30 bis 90 % bei einer Durchsatzleistung von 0,01 bis 1,5 t/h.The degree of filling is expediently 30 to 90% with a throughput of 0.01 to 1.5 t / h.
Die Erfindung ist im folgenden anhand eines Ausführungsbeispiels näher erläutert :
- Als Ausgangspulver wurden folgende handelsübliche Pulver eingesetzt :
- The following commercially available powders were used as the starting powder:
Als Mahlkörper wurden Stahlkugeln mit einem Gewicht von 2,5 kg und einem Durchmesser von 10 mm verwendet, die Mahlgutmenge betrug 2,0 kg. Das Volumen des Mahlgefäßes betrug 8 I. Als Frequenz des Mahlgefäßes wurden 450 U/min gewählt. Die im Deckel des Mahlgefäßes gemessene Temperatur stieg innerhalb 15 min auf 110 bis 130 °C an und blieb danach konstant. Anschließend wurde noch 15 min weitergemahlen. Nach dem Mahlen hat das Pulver gemäß der Siebanalyse eine Korngröße von 88 % unter 0,5 mm. Die Härte der Pulverpartikel betrug zwischen 782 und 888 HV. Die Schichten der einzelnen Komponenten waren so dünn, daß sie lichtmikroskopisch nicht mehr aufzulösen waren.Steel balls with a weight of 2.5 kg and a diameter of 10 mm were used as grinding media, the amount of ground material was 2.0 kg. The volume of the grinding vessel was 8 I. The frequency of the grinding vessel was chosen to be 450 rpm. The temperature measured in the lid of the grinding vessel rose to 110 to 130 ° C. in the course of 15 minutes and then remained constant. The grinding was then continued for a further 15 minutes. After grinding, the powder has a grain size of 88% below 0.5 mm according to the sieve analysis. The hardness of the powder particles was between 782 and 888 HV. The layers of the individual components were so thin that they could no longer be resolved by light microscopy.
Für die in der Zentrifugalmühle erzeugten mechanisch legierten Verbundpulver ist die hohe plastische Verformung von vorherrschender Bedeutung, wodurch die hohe Härte der Pulverteilchen entsteht. Die Verbundpulver können durch Strangpressen verdichtet und ggf. anschließend wärmebehandelt werden.The high plastic deformation is of predominant importance for the mechanically alloyed composite powders produced in the centrifugal mill, which results in the high hardness of the powder particles. The composite powders can be compacted by extrusion and, if necessary, then heat-treated.
Claims (3)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3525056 | 1985-07-13 | ||
| DE19853525056 DE3525056A1 (en) | 1985-07-13 | 1985-07-13 | METHOD FOR PRODUCING A MECHANICALLY ALLOYED COMPOSITE POWDER |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0209179A1 EP0209179A1 (en) | 1987-01-21 |
| EP0209179B1 true EP0209179B1 (en) | 1988-12-21 |
Family
ID=6275698
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP86201163A Expired EP0209179B1 (en) | 1985-07-13 | 1986-07-02 | Process for manufacturing a mechanically alloyed composite powder |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US4706894A (en) |
| EP (1) | EP0209179B1 (en) |
| JP (1) | JPS6220802A (en) |
| DE (2) | DE3525056A1 (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3741119A1 (en) * | 1987-12-04 | 1989-06-15 | Krupp Gmbh | PRODUCTION OF SECONDARY POWDER PARTICLES WITH NANOCRISTALLINE STRUCTURE AND WITH SEALED SURFACES |
| JPH0720441B2 (en) * | 1988-02-10 | 1995-03-08 | ローマン商事株式会社 | Method for producing a plastic heel having a leather grain mark |
| DE3813224A1 (en) * | 1988-04-20 | 1988-08-25 | Krupp Gmbh | METHOD FOR ADJUSTING FINE CRYSTALLINE TO NANOCRISTALLINE STRUCTURES IN METAL-METAL METALOID POWDER |
| DE3925973A1 (en) * | 1989-08-05 | 1991-02-07 | Eckart Standard Bronzepulver | Producing aluminium-lead alloy powder - by intensively grinding together powder, of the two components |
| JP2560565B2 (en) * | 1991-04-23 | 1996-12-04 | 株式会社栗本鐵工所 | Method for producing hydrogen storage alloy |
| DE4343106C2 (en) * | 1992-12-23 | 1995-12-07 | Deutsche Forsch Luft Raumfahrt | Mechanical alloying of brittle and hard materials using planetary mills |
| DE4418598C2 (en) * | 1994-05-27 | 1998-05-20 | Fraunhofer Ges Forschung | Process for producing a highly disperse powder mixture, in particular for producing components from materials that are difficult to sinter with intermetallic phases |
| WO2002100548A2 (en) * | 2001-06-13 | 2002-12-19 | Inhale Therapeutic Systems, Inc. | Centrifuged rotating drum for treating cohesive powders |
| GB2511111B (en) * | 2013-02-25 | 2015-08-19 | Chinook End Stage Recycling Ltd | Improvements in Waste Processing |
| FR3055813B1 (en) | 2016-09-09 | 2020-06-26 | H.E.F | MULTIMATERIAL COMPOSITE GRAIN POWDER FOR ADDITIVE SYNTHESIS |
| LU101177B1 (en) | 2019-04-16 | 2020-10-16 | Delmee Maxime | Functionalized metal powders by small particles made by non-thermal plasma glow discharge for additive manufacturing applications |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2995780A (en) * | 1958-12-09 | 1961-08-15 | Int Nickel Co | Treatment of metal powder |
| DE1151665B (en) * | 1958-12-09 | 1963-07-18 | Mond Nickel Co Ltd | Process for increasing the grain size of carbonyl nickel powder, carbonyl iron powder or copper powder |
| US3723092A (en) * | 1968-03-01 | 1973-03-27 | Int Nickel Co | Composite metal powder and production thereof |
| US3529780A (en) * | 1968-05-08 | 1970-09-22 | Cecil H Wilkinson Jr | Planetary grinding mill |
| SU814453A1 (en) * | 1979-04-12 | 1981-03-23 | Государственный Научно-Исследовательскийи Проектно-Конструкторский Институтгидрометаллургии Цветных Металлов | Planetary mill |
-
1985
- 1985-07-13 DE DE19853525056 patent/DE3525056A1/en not_active Withdrawn
-
1986
- 1986-07-02 DE DE8686201163T patent/DE3661463D1/en not_active Expired
- 1986-07-02 EP EP86201163A patent/EP0209179B1/en not_active Expired
- 1986-07-10 US US06/884,250 patent/US4706894A/en not_active Expired - Fee Related
- 1986-07-11 JP JP61163527A patent/JPS6220802A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| DE3525056A1 (en) | 1987-01-22 |
| EP0209179A1 (en) | 1987-01-21 |
| DE3661463D1 (en) | 1989-01-26 |
| US4706894A (en) | 1987-11-17 |
| JPS6220802A (en) | 1987-01-29 |
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