EP0779376B1 - Plasma carburizing of metallic workpieces - Google Patents
Plasma carburizing of metallic workpieces Download PDFInfo
- Publication number
- EP0779376B1 EP0779376B1 EP96118592A EP96118592A EP0779376B1 EP 0779376 B1 EP0779376 B1 EP 0779376B1 EP 96118592 A EP96118592 A EP 96118592A EP 96118592 A EP96118592 A EP 96118592A EP 0779376 B1 EP0779376 B1 EP 0779376B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- propane
- methane
- carbon
- plasma
- carburizing
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
- C23C8/38—Treatment of ferrous surfaces
Definitions
- the invention relates to a method for plasma carburizing metallic workpieces in a furnace, the furnace atmosphere containing a carbon carrier which under the process conditions of plasma carburizing with the release of pure Carbon is split.
- thermochemical treatment processes for case hardening metallic Workpieces have become conventional in recent years
- Gas carburizing is increasingly the carburizing process in vacuum plants enforced, because only with these processes a carburization free of edge oxidation is feasible.
- These carburizing processes in vacuum plants are concerned low pressure and plasma carburizing. Because with these carburizing processes one can work without oxygen-containing reaction gases there is no C level control; the decisive parameter for the carbon transition in these processes, the carbon mass flow density is is defined as the amount of carbon per unit of time and area in the Material passes over.
- This carbon required for the carburization is extracted from an in carbon carrier in the furnace atmosphere - usually one Hydrocarbon - provided under the given process conditions is split with the release of pure carbon.
- propane C 3 H 8
- propane pyrolysis the carbon carrier, which is split in the course of the so-called propane pyrolysis according to the following reaction equations: C 3 H 8 ⁇ CH 4 + C 2 H 4 C 2 H 4 ⁇ 2C + 2H 2 CH 4 ⁇ C + 2H 2
- methane (CH 4 ) is usually used as the carbon carrier, which is obtained by methane pyrolysis according to the equation CH 4 ⁇ C + 2H 2 is split.
- propane instead of methane.
- methane or propane as a carbon carrier is in each case with various advantages and disadvantages.
- propane due to its larger number of carbon atoms - 3 carbon atoms in the Propane versus 1 carbon atom in methane - a more effective carbon carrier as methane.
- propane has the disadvantage that propane is already split thermally in the temperature range above 600 ° C, whereby A carburization already takes place in the furnace, which leads to the furnace becoming sooty.
- methane only has one carbon atom, but it is the methane molecule so stable that it is not already at the necessary carburizing temperature is split. Rather, the splitting takes place only in the plasma and therefore really only on the workpiece surface. Since the carbon mass flow density at Cleavage of methane is very low, large batches can only be Carburize evenly with methane.
- the object of the invention is to provide a process for the plasma carburization of metallic workpieces which ensures carburization with a high carbon mass flow density without there being a risk of sooting the furnace at the same time.
- the furnace atmosphere consists of a mixture of methane and propane serving as carbon support, wherein the methane-propane mixture to .- contains about 60% by volume of propane, and that the gas pressure of the furnace atmosphere is below 10 mbar.
- the inventive method is characterized in that the increase the carbon mass flow density while avoiding soot formation is achieved in that an existing only of methane and propane Gas mixture with a propane content of up to 60 vol.% At a gas pressure in the furnace atmosphere of less than 10 mbar is used. At a gas pressure of Thermal splitting of the methane is almost impossible below 10 mbar. The Adding further gases such as hydrogen to the methane-propane mixture is to avoid soot formation among the Process parameters according to the invention are not necessary.
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Plasmaaufkohlung metallischer Werkstücke in einem Ofen, wobei die Ofenatmosphäre einen Kohlenstoff-Träger enthält, der unter den Prozeßbedingungen der Plasmaaufkohlung unter Abgabe von reinem Kohlenstoff gespalten wird.The invention relates to a method for plasma carburizing metallic workpieces in a furnace, the furnace atmosphere containing a carbon carrier which under the process conditions of plasma carburizing with the release of pure Carbon is split.
Unter den thermochemischen Behandlungsverfahren zur Einsatzhärtung metallischer Werkstücke haben sich in den letzten Jahren neben der konventionellen Gasaufkohlung immer mehr die Aufkohlungsprozesse in Vakuumanlagen durchgesetzt, da nur mit diesen Verfahren eine randoxidationsfreie Aufkohlung realisierbar ist. Bei diesen Aufkohlungsprozessen in Vakuumanlagen handelt es sich um die Niederdruck- und die Plasmaaufkohlung. Da bei diesen Aufkohlungsverfahren ohne sauerstoffhaltige Reaktionsgase gearbeitet wird, kann keine C-Pegelregelung erfolgen; die entscheidende Kenngröße für den Kohlenstoffübergang ist bei diesen Verfahren die Kohlenstoff-Massenstromdichte, die als Kohlenstoffmenge definiert ist, die pro Zeit- und Flächeneinheit in den Werkstoff übergeht. Dieser zur Aufkohlung benötigte Kohlenstoff wird von einem in der Ofenatmosphäre befindlichen Kohlenstoff-Träger - meist einem Kohlenwasserstoff - zur Verfügung gestellt, der bei den gegebenen Prozeßbedingungen unter Abgabe von reinem Kohlenstoff gespalten wird.Among the thermochemical treatment processes for case hardening metallic Workpieces have become conventional in recent years Gas carburizing is increasingly the carburizing process in vacuum plants enforced, because only with these processes a carburization free of edge oxidation is feasible. These carburizing processes in vacuum plants are concerned low pressure and plasma carburizing. Because with these carburizing processes one can work without oxygen-containing reaction gases there is no C level control; the decisive parameter for the carbon transition in these processes, the carbon mass flow density is is defined as the amount of carbon per unit of time and area in the Material passes over. This carbon required for the carburization is extracted from an in carbon carrier in the furnace atmosphere - usually one Hydrocarbon - provided under the given process conditions is split with the release of pure carbon.
Bei den bekannten Niederdruck-Aufkohlungsverfahren wird als Kohlenstoff-Träger
in der Regel Propan (C3H8) verwendet, welches im Laufe der sogenannten
Propanpyrolyse nach folgenden Reaktionsgleichungen gespalten wird:
Bei der Plasmaaufkohlung wird als Kohlenstoff-Träger meist Methan (CH4)
verwendet, welches im Wege der Methanpyrolyse nach der Gleichung
Die Verwendung von Methan oder Propan als Kohlenstoff-Träger ist jeweils mit verschiedenen Vor- und Nachteilen verbunden. So ist beispielsweise Propan aufgrund seiner größeren Anzahl von Kohlenstoffatomen - 3 C-Atome beim Propan gegenüber 1 C-Atom beim Methan - ein wirksamerer Kohlenstoff-Träger als Methan. Andererseits weist Propan jedoch den Nachteil auf, daß Propan bereits im Temperaturbereich über 600°C thermisch gespalten wird, wodurch bereits im Ofen eine Aufkohlung stattfindet, die zum Verrußen des Ofens führt. Methan hingegen weist zwar nur ein C-Atom auf, jedoch ist das Methan-Molekül so stabil, daß es nicht bereits bei der notwendigen Aufkohlungstemperatur gespalten wird. Die Spaltung erfolgt vielmehr erst im Plasma und somit wirklich nur an der Werkstückoberfläche. Da die Kohlenstoff-Massenstromdichte bei der Spaltung von Methan nur sehr gering ist, lassen sich großflächige Chargen nur sehr schwer gleichmäßig mit Methan aufkohlen.The use of methane or propane as a carbon carrier is in each case with various advantages and disadvantages. For example, propane due to its larger number of carbon atoms - 3 carbon atoms in the Propane versus 1 carbon atom in methane - a more effective carbon carrier as methane. On the other hand, propane has the disadvantage that propane is already split thermally in the temperature range above 600 ° C, whereby A carburization already takes place in the furnace, which leads to the furnace becoming sooty. In contrast, methane only has one carbon atom, but it is the methane molecule so stable that it is not already at the necessary carburizing temperature is split. Rather, the splitting takes place only in the plasma and therefore really only on the workpiece surface. Since the carbon mass flow density at Cleavage of methane is very low, large batches can only be Carburize evenly with methane.
Die Verwendung von Methan, Propan oder Gemischen aus Methan und Stickstoff sowie Propan und Stickstoff als Kohlenstoff-Träger ist beispielsweise aus der DE-Publikation "Härterei-Technische Mitteilungen", Band 49, Nr. 2, März/April 1994, Seite 105 bekannt.The use of methane, propane or mixtures of methane and nitrogen as well as propane and nitrogen as a carbon carrier is for example from the DE publication "Härterei-Technische Mitteilungen", Volume 49, No. 2, March / April 1994, Page 105 known.
Aus den Chemical Abstracts, Vol. 102, No. 26, 1985, Abstract No. 224092 u ist schließlich ein durch Computer-Simulation getestetes Verfahren zum Aufkohlen von Eisenlegierungen mittels Glimm-Entladung bekannt, bei dem als Prozeßgas Methan, Propan und Methan-Propan-Gemisch mit Ar oder H2 mit Verdünnungszusätzen in einem Druckbereich zwischen 13,3 - 146,6 Pa bzw. 0,13 - 1,46 mbar (0,1 und 1,1 Torr) mit einer Konzentration der gasförmigen Verdünner von 80 - 95 %. Der Gegenwert von H und H-lonen verhindert hierdurch die Rußbildung.From Chemical Abstracts, Vol. 102, No. 26, 1985, abstract no. 224092 u is finally known a method for carburizing iron alloys by means of glow discharge which has been tested by computer simulation and in which the process gas is methane, propane and methane-propane mixture with Ar or H 2 with dilution additives in a pressure range between 13.3 - 146 , 6 Pa or 0.13 - 1.46 mbar (0.1 and 1.1 Torr) with a concentration of the gaseous thinners of 80 - 95%. The counter value of H and H ions thereby prevents soot formation.
In Anbetracht des voranstehend geschilderten Standes der Technik liegt der Erfindung die Aufgabe zugrunde, ein Verfahren zur Plasmaaufkohlung metallischer Werkstücke bereitzustellen, das eine Aufkohlung mit einer hohen Kohlenstoff-Massenstromdichte gewährleistet, ohne daß gleichzeitig die Gefahr der Verrußung des Ofens besteht.In view of the above-described prior art, the object of the invention is to provide a process for the plasma carburization of metallic workpieces which ensures carburization with a high carbon mass flow density without there being a risk of sooting the furnace at the same time.
Überraschenderweise hat sich herausgestellt, daß diese Aufgabe erfindungsgemäß dadurch gelöst wird, daß die Ofenatmosphäre aus einem Gemisch von Methan und Propan besteht, das als Kohlenstoff-Träger dient, wobei das Methan-Propan-Gemisch bis zu 60 Vol.-% Propan enthält, und daß der Gasdruck der Ofenatmosphäre unter 10 mbar beträgt.Surprisingly, it has been found that this object is achieved in that the furnace atmosphere consists of a mixture of methane and propane serving as carbon support, wherein the methane-propane mixture to .- contains about 60% by volume of propane, and that the gas pressure of the furnace atmosphere is below 10 mbar.
Das Erreichen der hohen Kohlenstoff-Massenstromdichte einerseits und das Vermeiden der Verrußung des Ofens andererseits kommt dabei dadurch zustande, daß Propan aufgrund seiner drei C-Atome bei der thermischen und elektrischen Spaltung im Plasma viel mehr Kohlenstoff zur Verfügung stellen kann als Methan. Das Methan auf der anderen Seite spaltet sich bei den Aufkohlungstemperaturen zwischen 800°C und 1000°C fast gar nicht. Die Spaltung des Methans findet erst im Plasma, also wirklich nur an der Werkstückoberfläche statt, so daß diese frei werdenden Kohlenstoff-Atome nur zum Aufkohlen der Werkstücke, nicht jedoch zur Verrußung des Ofens beitragen können.The achievement of the high carbon mass flow density on the one hand and that Avoiding the soot on the other hand, that propane due to its three carbon atoms in thermal and electrical Cleavage in plasma can provide much more carbon than methane. The methane on the other hand splits at carburizing temperatures between 800 ° C and 1000 ° C almost not at all. The splitting of the methane takes place only in plasma, really only on the workpiece surface, so that it is free carbon atoms only for carburizing the workpieces, but not can contribute to sooting the furnace.
Das erfindungsgemäße Verfahren zeichnet sich dadurch aus, daß die Erhöhung der Kohlenstoff-Massenstromdichte bei gleichzeitigem Vermeiden von Rußbildung dadurch erreicht wird, daß ein nur aus Methan und Propan bestehendes Gasgemisch mit einem Propan-Anteil von bis zu 60 Vol.-% bei einem Gasdruck in der Ofenatmosphäre von unter 10 mbar verwendet wird. Bei einem Gasdruck von unter 10 mbar ist eine thermische Spaltung des Methans nahezu unmöglich. Die Zugabe von weiteren Gasen wie beispielsweise Wasserstoff, zu dem Methan-Propan-Gemisch ist zur Vermeidung der Rußbildung unter den erfindungsgemäßen Verfahrensparametern nicht notwendig. The inventive method is characterized in that the increase the carbon mass flow density while avoiding soot formation is achieved in that an existing only of methane and propane Gas mixture with a propane content of up to 60 vol.% At a gas pressure in the furnace atmosphere of less than 10 mbar is used. At a gas pressure of Thermal splitting of the methane is almost impossible below 10 mbar. The Adding further gases such as hydrogen to the methane-propane mixture is to avoid soot formation among the Process parameters according to the invention are not necessary.
Bei den Versuchen hat sich herausgestellt, daß insbesondere ein Propan-Anteil von 5 bis 50 Vol.-% besonders geeignet ist, um ohne Rußbildung eine hohe Kohlenstoff-Massenstromdichte bzw. Kohlenstoff-Übertragungsrate zu erhalten.The experiments have shown that in particular a propane fraction from 5 to 50 vol .-% is particularly suitable to a high without soot formation To obtain carbon mass flow density or carbon transfer rate.
In der Zeichnung ist für den Werkstoff 27 CrMo 4 der Härteverlauf nach dem Plasmaaufkohlungsverfahren mit einem Methan-Propan-Gemisch als Kohlenstoff-Träger dargestellt.In the drawing, the hardness curve for the material 27 CrMo 4 after Plasma carburizing process with a methane-propane mixture as a carbon carrier shown.
Die Prozeßparameter für den in der Abbildung dargestellten Plasmaaufkohlungsprozeß waren:
- zehnminütiges Aufkohlen bei einer Aufkohlungstemperatur von 940°C.
- Die anschließende Diffusionsphase betrug 51 Minuten,
- woran anschließend nach dem Absenken auf die Härtetemperatur von 860°C die Charge mittels Hochdruckgasabschreckung abgeschreckt wurde.
- Carburizing for ten minutes at a carburizing temperature of 940 ° C.
- The subsequent diffusion phase was 51 minutes,
- after which the charge was quenched by high-pressure gas quenching after lowering to the hardening temperature of 860 ° C.
Als Ergebnis dieses Prozesses wurde eine Einsatzhärtungstiefe (550 HV 1) von 0,7 mm auf der Zahnflanke erzielt.As a result of this process, a case hardening depth (550 HV 1) of 0.7 mm achieved on the tooth flank.
Mit dem voranstehend dargestellten Verfahren ist es somit möglich, durch die Verwendung des Methan-Propan-Gemisches als Kohlenstoff-Träger die Kohlenstoff-Massenstromdichte bei der Plasmaaufkohlung deutlich zu erhöhen, ohne daß die Gefahr der Verrußung des Ofens besteht.With the method described above, it is thus possible to Using the methane-propane mixture as a carbon carrier, the carbon mass flow density increase significantly in plasma carburizing without that there is a risk of sooting the furnace.
Claims (2)
- Process for plasma carbonisation of metallic workpieces in a furnace, wherein the furnace atmosphere contains a carbon substrate which is cleaved under the process conditions of plasma carbonisation with release of pure carbon, characterised in that the furnace atmosphere consists of a mixture of methane and propane serving as carbon substrate, wherein the methane-propane mixture contains up to 60 volume % of propane, and in that the gas pressure of the furnace atmosphere is below 10 mbar.
- Process according to claim 1, characterised in that the propane portion in the methane-propane mixture is 5 to 50 volume %.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19547131A DE19547131A1 (en) | 1995-12-16 | 1995-12-16 | Process for plasma carburizing metallic workpieces |
| DE19547131 | 1995-12-16 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0779376A1 EP0779376A1 (en) | 1997-06-18 |
| EP0779376B1 true EP0779376B1 (en) | 2000-01-26 |
| EP0779376B2 EP0779376B2 (en) | 2002-12-18 |
Family
ID=7780384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP96118592A Expired - Lifetime EP0779376B2 (en) | 1995-12-16 | 1996-11-20 | Plasma carburizing of metallic workpieces |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US5851314A (en) |
| EP (1) | EP0779376B2 (en) |
| AT (1) | ATE189271T1 (en) |
| DE (2) | DE19547131A1 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19815233A1 (en) * | 1998-04-04 | 1999-10-07 | Ald Vacuum Techn Gmbh | Process for vacuum carburizing under treatment gas |
| US20050016831A1 (en) * | 2003-07-24 | 2005-01-27 | Paganessi Joseph E. | Generation of acetylene for on-site use in carburization and other processes |
| DE102004053935B4 (en) * | 2004-11-09 | 2015-04-09 | Schaeffler Technologies AG & Co. KG | Process for the heat treatment of a component made of a thermosetting heat-resistant steel and a component made of a thermosetting, heat-resistant steel |
| DE102006040814A1 (en) * | 2006-08-31 | 2008-03-06 | Schaeffler Kg | Method for producing a highly hardenable rolling bearing component |
| KR101622306B1 (en) * | 2009-10-29 | 2016-05-19 | 삼성전자주식회사 | Graphene sheet, substrate comprising graphene sheet and process for preparing these materials |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58113371A (en) * | 1981-12-28 | 1983-07-06 | Seiko Epson Corp | Plasma surface hardening method |
| US5139584A (en) † | 1989-07-13 | 1992-08-18 | Solo Fours Industriels Sa | Carburization process |
| US5383980A (en) * | 1992-01-20 | 1995-01-24 | Leybold Durferrit Gmbh | Process for hardening workpieces in a pulsed plasma discharge |
| DE4427902C1 (en) † | 1994-08-06 | 1995-03-30 | Leybold Durferrit Gmbh | Method for carburising components made from carburisable materials by means of a plasma discharge operated in a pulsed fashion |
-
1995
- 1995-12-16 DE DE19547131A patent/DE19547131A1/en not_active Withdrawn
-
1996
- 1996-11-20 AT AT96118592T patent/ATE189271T1/en not_active IP Right Cessation
- 1996-11-20 DE DE59604291T patent/DE59604291D1/en not_active Expired - Fee Related
- 1996-11-20 EP EP96118592A patent/EP0779376B2/en not_active Expired - Lifetime
- 1996-12-13 US US08/766,282 patent/US5851314A/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| ATE189271T1 (en) | 2000-02-15 |
| DE19547131A1 (en) | 1997-06-19 |
| EP0779376B2 (en) | 2002-12-18 |
| EP0779376A1 (en) | 1997-06-18 |
| US5851314A (en) | 1998-12-22 |
| DE59604291D1 (en) | 2000-03-02 |
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