EP0464265B1 - Method for nitriding titanium - Google Patents
Method for nitriding titanium Download PDFInfo
- Publication number
- EP0464265B1 EP0464265B1 EP90125660A EP90125660A EP0464265B1 EP 0464265 B1 EP0464265 B1 EP 0464265B1 EP 90125660 A EP90125660 A EP 90125660A EP 90125660 A EP90125660 A EP 90125660A EP 0464265 B1 EP0464265 B1 EP 0464265B1
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- EP
- European Patent Office
- Prior art keywords
- titanium
- ammonia
- mpa
- temperatures
- pressure
- 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.)
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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
- C23C8/08—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 only one element being applied
- C23C8/24—Nitriding
Definitions
- the invention relates to a method for applying nitride layers to parts made of titanium and titanium alloys by thermochemical treatment of the parts with ammonia or ammonia-containing gas mixtures under pressure and at temperatures above 500 ° C.
- titanium As a construction material, titanium has several advantages over steel, which result from its low specific weight, its corrosion resistance and its high strength. This is offset by the relatively low hardness, which makes surface treatment necessary if the wear resistance is to be increased.
- This surface treatment usually consists of the production of layers of titanium carbide or titanium nitride. In previously known methods for nitriding parts made of titanium and titanium alloys, high-energy gases or electromagnetic fields are used. These processes are very complex and can only be used for simple geometry of the parts to be treated.
- JP-A-2-025 559 Patent Abstracts of Japan, vol. 14, Ni. 176, 4119 describes the nitriding of titanium and titanium alloys in an ammonia atmosphere at normal pressure.
- EP-A 0 105 835 describes a method for producing nitride layers on components made of titanium and titanium alloys by exposing the components in an autoclave to pressures of at least 10 MPa and temperatures of at least 200 ° C. in an ammonia atmosphere.
- the ammonia must be of great purity.
- the nitration is preferably carried out at 90 to 130 MPa and temperatures from 930 ° to 1000 ° C. This process has the disadvantage that it is very expensive due to the use of autoclaves and very pure ammonia and 20 ⁇ m thick layers only in periods of three and more hours can be reached.
- This object is achieved in that the treatment is carried out at temperatures from 700 to 950 ° C. and pressures from 0.5 to 7 MPa, the ammonia partial pressure being kept at least at 0.2 MPa.
- components made of titanium and titanium alloys of any geometry and size can be provided with sufficiently thick nitride layers of 20 ⁇ m and more in appropriate chamber furnaces.
- no high-purity gases are required for this, but the normal commercial quality of ammonia is sufficient.
- nitrogen is also possible to add nitrogen to the ammonia, with only an ammonia partial pressure of at least 0.2 MPa being required for the nitriding process.
- the layer thickness of the titanium nitride that forms depends on the temperature and the treatment time in large pressure ranges.
- the surface is shiny gold and causes a significant increase in hardness.
- the layer thickness is almost independent of the pressure.
- the figure shows the formation of a titanium nitride layer on parts made of pure titanium depending on the pressure and the temperature of the ammonia-containing atmosphere.
- a TiN layer of, for example, 30 ⁇ m builds up if the samples are kept at 880 ° C for one hour.
- titanium alloys such as TiAl6V4 are nitrided.
- An autoclave is not required for these coatings, but the treatment can be carried out in a commercially available chamber furnace.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
- Chemically Coating (AREA)
- Physical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Road Paving Structures (AREA)
- Revetment (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zum Aufbringen von Nitridschichten auf Teile aus Titan und Titanlegierungen durch thermochemische Behandlung der Teile mit Ammoniak oder ammoniakhaltigen Gasgemischen unter Druck und bei Temperaturen oberhalb 500° C.The invention relates to a method for applying nitride layers to parts made of titanium and titanium alloys by thermochemical treatment of the parts with ammonia or ammonia-containing gas mixtures under pressure and at temperatures above 500 ° C.
Titan hat als Konstruktionswerkstoff gegenüber Stahl einige Vorteile, die sich aus dem geringen spezifischen Gewicht, seiner Korrosionsbeständigkeit und seiner hohen Festigkeit ergeben. Dem steht die relativ geringe Härte gegenüber, die eine Oberflächenbehandlung notwendig macht, wenn die Verschleißfestigkeit erhöht werden soll. Diese Oberflächenbehandlung besteht in der Regel aus der Erzeugung von Schichten aus Titancarbid oder Titannitrid. Bei bisher bekannten Verfahren zur Nitrierung von Teilen aus Titan und Titan legierungen wird mit hochenergetischen Gasen oder elektromagnetischen Feldern gearbeitet. Diese Verfahren sind sehr aufwendig und nur für einfache Geometrie der zu behandelnden Teile anwendbar.As a construction material, titanium has several advantages over steel, which result from its low specific weight, its corrosion resistance and its high strength. This is offset by the relatively low hardness, which makes surface treatment necessary if the wear resistance is to be increased. This surface treatment usually consists of the production of layers of titanium carbide or titanium nitride. In previously known methods for nitriding parts made of titanium and titanium alloys, high-energy gases or electromagnetic fields are used. These processes are very complex and can only be used for simple geometry of the parts to be treated.
In der japanischen Patentanmeldung JP-A- 2-025 559 (Patent Abstracts of Japan, Bd.14, Ni. 176, 4119) wird das Nitrieren von Titan und Titanlegierungen in einer Ammoniakatmosphäre bei Normaldruck beschrieben.Japanese patent application JP-A-2-025 559 (Patent Abstracts of Japan, vol. 14, Ni. 176, 4119) describes the nitriding of titanium and titanium alloys in an ammonia atmosphere at normal pressure.
In der EP-A 0 105 835 wird ein Verfahren zur Herstellung von Nitridschichten auf Bauteilen aus Titan und Titanlegierungen beschrieben, indem man die Bauteile in einem Autoklaven Drucken von mindestens 10 MPa und Temperaturen von mindestens 200° C in einer Ammoniakatmosphäre aussetzt. Dabei muß der Ammoniak von großer Reinheit sein. Vorzugsweise erfolgt die Nitrierung bei 90 bis 130 MPa und Temperaturen von 930° bis 1000° C. Dieses Verfahren hat den Nachteil, daß es durch die Verwendung von Autoklaven und sehr reinem Ammoniak sehr teuer ist und 20 um-starke Schichten erst in Zeiträumen von drei und mehr Stunden erreichbar sind.EP-
Es war daher Aufgabe der vorliegenden Erfindung, ein Verfahren zum Aufbringen von Nitridschichten auf Teile aus Titan und Titanlegierungen durch thermochemische Behandlung der Teile mit Ammoniak oder ammoniakhaltigen Gasgemischen unter Druck und bei Temperaturen oberhalb 500° C zu entwickeln, das preisgünstig ist und Nitridschichtdicken von 20 µm und mehr in kurzen Zeiträumen von weniger als drei Stunden ermöglicht.It was therefore an object of the present invention to develop a process for applying nitride layers to parts made of titanium and titanium alloys by thermochemical treatment of the parts with ammonia or ammonia-containing gas mixtures under pressure and at temperatures above 500 ° C., which is inexpensive and nitride layer thicknesses of 20 μm and more in less than three hours.
Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß die Behandlung bei Temperaturen von 700 bis 950° C und Drucken von 0,5 bis 7 MPa durchgeführt wird, wobei der Ammoniakpartialdruck mindestens bei 0,2 MPa gehalten wird.This object is achieved in that the treatment is carried out at temperatures from 700 to 950 ° C. and pressures from 0.5 to 7 MPa, the ammonia partial pressure being kept at least at 0.2 MPa.
Mit diesem Druck verfahren können Bauteile aus Titan und Titanlegierungen beliebiger Geometrie und Größe in entsprechenden Kammeröfen mit ausreichend dicken Nitridschichten von 20 µm und mehr versehen werden. Überraschenderweise sind hierfür keine hochreinen Gase erforderlich, sondern es genügt die normale Handelsqualität von Ammoniak. Außerdem ist es möglich, dem Ammoniak Stickstoff beizumischen, wobei lediglich ein Ammoniakpartialdruck von mindestens 0,2 MPa für das Nitrierverfahren erforderlich ist.With this pressure process, components made of titanium and titanium alloys of any geometry and size can be provided with sufficiently thick nitride layers of 20 µm and more in appropriate chamber furnaces. Surprisingly, no high-purity gases are required for this, but the normal commercial quality of ammonia is sufficient. It is also possible to add nitrogen to the ammonia, with only an ammonia partial pressure of at least 0.2 MPa being required for the nitriding process.
Die Schichtdicke des sich ausbildenden Titannitrids ist in großen Druckbereichen abhängig von der Temperatur und der Behandlungszeit. Die Oberfläche ist goldglänzend und bewirkt eine signifikante Härtesteigerung. Bei Drucken im Bereich oberhalb 6 MPa ist die Schichtdicke fast unabhängig vom Druck.The layer thickness of the titanium nitride that forms depends on the temperature and the treatment time in large pressure ranges. The surface is shiny gold and causes a significant increase in hardness. When printing in the range above 6 MPa, the layer thickness is almost independent of the pressure.
Die Abbildung zeigt die Ausbildung einer Titannitridschicht auf Teilen aus Reintitan in Abhängigkeit vom Druck und der Temperatur der ammoniakhaltigen Atmosphäre.The figure shows the formation of a titanium nitride layer on parts made of pure titanium depending on the pressure and the temperature of the ammonia-containing atmosphere.
Bereits bei Temperaturen von beispielsweise 500° C wurde bei 2 MPa (= 20 bar) Absolutdruck nach einer Stunde eine TiN-Schichtdicke von 10 µm gemessen. Bei 880° C wird in dieser Zeit eine reine TiN-Schicht von 20 µm aufgebaut.Even at temperatures of, for example, 500 ° C., a TiN layer thickness of 10 μm was measured at 2 MPa (= 20 bar) absolute pressure after one hour. During this time, a pure 20 µm TiN layer is built up at 880 ° C.
Bei einem Druck von 6 MPa (= 60 bar) baut sich eine TiN-Schicht von beispielsweise 30 µm auf, wenn die Proben für eine Stunde bei 880° C gehalten werden.At a pressure of 6 MPa (= 60 bar), a TiN layer of, for example, 30 µm builds up if the samples are kept at 880 ° C for one hour.
Bei weiter gesteigertem Druck bis zu 9 MPa (= 90 bar) nimmt der Einfluß des Druckes auf die TiN-Schichtdicke ab. Die Zunahme ist nicht mehr linear. Bei noch höheren Drücken ist aufgrund der sich rasch bildenden dichten TiN-Schicht nur noch die Diffusion des Stickstoff durch die Schicht der zeitbestimmende Faktor.With a further increased pressure up to 9 MPa (= 90 bar), the influence of the pressure on the TiN layer thickness decreases. The increase is no longer linear. At even higher pressures, only the diffusion of nitrogen through the layer is the time-determining factor due to the rapidly forming dense TiN layer.
Wie Reintitan können auch Titanlegierungen, wie z.B. TiAl6V4 nitriert werden.Like pure titanium, titanium alloys such as TiAl6V4 are nitrided.
Für diese Beschichtungen ist kein Autoklav erforderlich, sondern die Behandlung kann in einem handelsüblichen Kammerofen erfolgen.An autoclave is not required for these coatings, but the treatment can be carried out in a commercially available chamber furnace.
Claims (1)
- Method of applying nitride layers to parts composed of titanium and titanium alloys by thermochemical treatment of the parts with ammonia or ammonia-containing gas mixtures under pressure and at temperatures of more than 500°C,
characterised in that
the treatment is carried out at temperatures of 700 to 950°C and pressures of 0.5 to 7 MPa, the ammonia partial pressure being maintained at at least 0.2 MPa.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4021286 | 1990-07-04 | ||
| DE4021286A DE4021286C1 (en) | 1990-07-04 | 1990-07-04 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0464265A1 EP0464265A1 (en) | 1992-01-08 |
| EP0464265B1 true EP0464265B1 (en) | 1996-03-06 |
Family
ID=6409636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP90125660A Expired - Lifetime EP0464265B1 (en) | 1990-07-04 | 1990-12-28 | Method for nitriding titanium |
Country Status (14)
| Country | Link |
|---|---|
| EP (1) | EP0464265B1 (en) |
| JP (1) | JPH0649924B2 (en) |
| CN (1) | CN1020476C (en) |
| AT (1) | ATE135058T1 (en) |
| AU (1) | AU627960B2 (en) |
| BR (1) | BR9101899A (en) |
| CZ (1) | CZ279472B6 (en) |
| DE (2) | DE4021286C1 (en) |
| ES (1) | ES2085320T3 (en) |
| NO (1) | NO905209L (en) |
| PL (1) | PL166281B1 (en) |
| PT (1) | PT98195A (en) |
| RU (1) | RU1836484C (en) |
| TW (1) | TW208721B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1169487A1 (en) * | 1999-04-15 | 2002-01-09 | Vacuumschmelze GmbH | Corrosion-free iron-nickel alloy for residual-current circuit-breakers and clockworks |
| JP4684383B2 (en) * | 2000-04-03 | 2011-05-18 | 株式会社アライドマテリアル | Refractory metal material having oxidation resistant layer and method for producing the same |
| JP2001295023A (en) * | 2000-04-06 | 2001-10-26 | Allied Material Corp | High melting point metallic material having surface hardened layer and its producing method |
| US9580790B2 (en) | 2006-12-22 | 2017-02-28 | Iap Research, Inc. | System and method for surface hardening of refractory metals |
| US10031113B2 (en) | 2007-02-28 | 2018-07-24 | Waters Technologies Corporation | Liquid-chromatography apparatus having diffusion-bonded titanium components |
| JP5977669B2 (en) * | 2012-12-28 | 2016-08-24 | 株式会社セブン・セブン | Method for manufacturing vacuum insulated double container |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0105835A1 (en) * | 1982-09-07 | 1984-04-18 | Vereinigte Drahtwerke AG | Method of producing a hard layer on articles of Ti or Ti-alloys |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2804410A (en) * | 1953-10-27 | 1957-08-27 | Nat Lead Co | Method for nitriding titanium surfaces |
-
1990
- 1990-07-04 DE DE4021286A patent/DE4021286C1/de not_active Expired - Lifetime
- 1990-10-26 TW TW079109059A patent/TW208721B/zh active
- 1990-11-29 AU AU67602/90A patent/AU627960B2/en not_active Ceased
- 1990-11-30 NO NO90905209A patent/NO905209L/en unknown
- 1990-12-20 CN CN90110418A patent/CN1020476C/en not_active Expired - Fee Related
- 1990-12-28 EP EP90125660A patent/EP0464265B1/en not_active Expired - Lifetime
- 1990-12-28 DE DE59010178T patent/DE59010178D1/en not_active Expired - Lifetime
- 1990-12-28 ES ES90125660T patent/ES2085320T3/en not_active Expired - Lifetime
- 1990-12-28 AT AT90125660T patent/ATE135058T1/en not_active IP Right Cessation
-
1991
- 1991-05-09 BR BR919101899A patent/BR9101899A/en not_active Application Discontinuation
- 1991-06-28 CZ CS911988A patent/CZ279472B6/en unknown
- 1991-07-02 JP JP3161349A patent/JPH0649924B2/en not_active Expired - Lifetime
- 1991-07-03 RU SU915001026A patent/RU1836484C/en active
- 1991-07-03 PL PL91290931A patent/PL166281B1/en unknown
- 1991-07-03 PT PT98195A patent/PT98195A/en not_active Application Discontinuation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0105835A1 (en) * | 1982-09-07 | 1984-04-18 | Vereinigte Drahtwerke AG | Method of producing a hard layer on articles of Ti or Ti-alloys |
Non-Patent Citations (1)
| Title |
|---|
| TRANSACTIONS OF THE ASM vol.46 (1954) p 540 ff * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1020476C (en) | 1993-05-05 |
| PL290931A1 (en) | 1992-10-05 |
| CS198891A3 (en) | 1992-02-19 |
| AU627960B2 (en) | 1992-09-03 |
| DE4021286C1 (en) | 1991-02-21 |
| DE59010178D1 (en) | 1996-04-11 |
| TW208721B (en) | 1993-07-01 |
| AU6760290A (en) | 1992-01-09 |
| JPH04232247A (en) | 1992-08-20 |
| CZ279472B6 (en) | 1995-05-17 |
| CN1057866A (en) | 1992-01-15 |
| JPH0649924B2 (en) | 1994-06-29 |
| PL166281B1 (en) | 1995-04-28 |
| NO905209D0 (en) | 1990-11-30 |
| EP0464265A1 (en) | 1992-01-08 |
| BR9101899A (en) | 1992-01-14 |
| PT98195A (en) | 1992-04-30 |
| ATE135058T1 (en) | 1996-03-15 |
| RU1836484C (en) | 1993-08-23 |
| NO905209L (en) | 1992-01-06 |
| ES2085320T3 (en) | 1996-06-01 |
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