DE4021286C1 - - Google Patents
Info
- Publication number
- DE4021286C1 DE4021286C1 DE4021286A DE4021286A DE4021286C1 DE 4021286 C1 DE4021286 C1 DE 4021286C1 DE 4021286 A DE4021286 A DE 4021286A DE 4021286 A DE4021286 A DE 4021286A DE 4021286 C1 DE4021286 C1 DE 4021286C1
- Authority
- DE
- Germany
- Prior art keywords
- mpa
- titanium
- ammonia
- temperatures
- treatment
- 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
Links
Classifications
-
- 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
Landscapes
- 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 application of nitride layers on parts made of titanium and Titanium alloys by thermochemical treatment of the Parts with ammonia or gas mixtures containing ammonia 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 Titanlegierungen wird mit hochenergetischen Gasen oder elektromagnetischen Feldern gearbeitet. Diese Verfahren sind sehr aufwendig und nur für einfache Geometrie der zu behandelnden Teile anwendbar.Titanium is a construction material compared to steel some advantages arising from the minor specific weight, its corrosion resistance and its high strength. That suits them relatively low hardness compared to the one Surface treatment is necessary if the Wear resistance should be increased. These Surface treatment usually consists of Generation of layers of titanium carbide or Titanium nitride. In previously known methods for Nitriding parts made of titanium and titanium alloys is using high energy gases or electromagnetic fields worked. These Procedures are very complex and only for simple ones Geometry of the parts to be treated applicable.
In der DE-PS 17 96 212 wird die Oberflächenhärtung von Titan durch Ausbildung von Nitridschichten in einer Ammoniakatmosphäre bei höheren Temperaturen unter Normaldruck erwähnt. In DE-PS 17 96 212 the surface hardening of Titanium through the formation of nitride layers in one Ammonia atmosphere at higher temperatures below Normal pressure mentioned.
Obwohl dabei relativ dicke und harte Schichten entstehen sollen, findet dieses Verfahren in der Praxis keine Anwendung, da durch Wasserstoffdiffusion eine Versprödung des Bauteilkerns stattfindet.Although relatively thick and hard layers this process takes place in the Practice no application because of hydrogen diffusion embrittlement of the component core takes place.
In der EP-OS 01 05 835 wird ein Verfahren zur Herstellung von Nitridschichten auf Bauteilen aus Titan und Titanlegierungen beschrieben, indem man die Bauteile in einem Autoklaven Drucken von 10 bis 500 MPa und Temperaturen von 200 bis 1200°C in beispielsweise 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 Ammoniak von hoher Reinheit sehr teuer ist und 20 µm-starke Schichten erst in Zeiträumen von drei und mehr Stunden erreichbar sind.EP-OS 01 05 835 describes a method for Manufacture of nitride layers on components Titanium and titanium alloys are described using the Components in an autoclave print from 10 to 500 MPa and temperatures from 200 to 1200 ° C in for example exposed to an ammonia atmosphere. The ammonia must be of great purity. The nitriding is preferably carried out at 90 to 130 MPa and temperatures from 930 ° to 1000 ° C. This The disadvantage of the method is that it can Use of autoclaves and high ammonia Purity is very expensive and 20 µm thick layers only in periods of three or more hours are reachable.
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 relativ kurzen Zeiträumen ermöglicht.It was therefore an object of the present invention Process for applying nitride layers to parts made of titanium and titanium alloys by thermochemical Treat the parts with ammonia or ammonia-containing gas mixtures under pressure and at To develop temperatures above 500 ° C is inexpensive and nitride layer thicknesses of 20 microns and enables more in relatively short periods of time.
Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß die Behandlung bei Temperaturen von 500 bis 1000°C und Drucken von 0,2 bis 10 MPa durchgeführt wird, wobei der Ammoniakpartialdruck mindestens bei 0,2 MPa gehalten wird. This object is achieved in that treatment at temperatures from 500 to 1000 ° C and printing from 0.2 to 10 MPa is carried out, the ammonia partial pressure being at least 0.2 MPa is held.
Besonders vorteilhaft haben sich Temperaturen von 700 bis 950°C und Drucke von 0,5 bis 7 MPa erwiesen, wobei ein Ammoniakpartialdruck von mindestens 0,2 MPa erforderlich ist.Temperatures of 700 to 950 ° C and pressures from 0.5 to 7 MPa, with an ammonia partial pressure of at least 0.2 MPa is required.
Mit diesem Druckverfahren 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 printing process, components made of titanium and titanium alloys of any geometry and size in appropriate chamber furnaces with sufficient thickness Nitride layers of 20 µm and more can be provided. Surprisingly, there are no high-purity gases for this required, but the normal one is sufficient Commercial quality of ammonia. It is also possible add nitrogen to the ammonia, whereby only an ammonia partial pressure of at least 0.2 MPa for the nitriding process is required.
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 is dependent on the in large pressure ranges Temperature and treatment time. The surface is shiny gold and causes a significant Increase in hardness. For pressures 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 in Dependence on the pressure and temperature of the atmosphere containing ammonia.
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 was at 2 MPa (= 20 bar) absolute pressure after a Hour a TiN layer thickness of 10 microns measured. At During this time, 880 ° C becomes a pure TiN layer of 20 µm built up.
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.One builds up at a pressure of 6 MPa (= 60 bar) TiN layer of, for example, 30 microns when 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 Stickstoffs durch die Schicht der zeitbestimmende Faktor.With further increased pressure up to 9 MPa (= 90 bar) the influence of pressure on the TiN layer thickness increases from. The increase is no longer linear. At still higher pressures is due to the rapidly developing dense TiN layer only the diffusion of the Nitrogen through the layer of time-determining Factor.
Wie Reintitan können auch Titanlegierungen, wie z. B. TiAl6V4 nitriert werden.Like pure titanium, titanium alloys such as e.g. B. TiAl6V4 are nitrided.
Für diese Beschichtungen ist kein Autoklav erforderlich, sondern die Behandlung kann in einem handelsüblichen Kammerofen erfolgen.There is no autoclave for these coatings required, but treatment can be done in one commercially available chamber furnace.
Claims (2)
Priority Applications (16)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4021286A DE4021286C1 (en) | 1990-07-04 | 1990-07-04 | |
TW079109059A TW208721B (en) | 1990-07-04 | 1990-10-26 | |
AU67602/90A AU627960B2 (en) | 1990-07-04 | 1990-11-29 | Process for applying nitrite layers to titanium |
NO90905209A NO905209L (en) | 1990-07-04 | 1990-11-30 | PROCEDURE FOR APPLYING NITRID LAYERS ON TITAN. |
CN90110418A CN1020476C (en) | 1990-07-04 | 1990-12-20 | Process for applying nitride layers to titanium |
DE59010178T DE59010178D1 (en) | 1990-07-04 | 1990-12-28 | Process for applying nitride layers on titanium |
EP90125660A EP0464265B1 (en) | 1990-07-04 | 1990-12-28 | Method for nitriding titanium |
AT90125660T ATE135058T1 (en) | 1990-07-04 | 1990-12-28 | METHOD FOR APPLYING NITRIDE LAYERS ON TITANIUM |
ES90125660T ES2085320T3 (en) | 1990-07-04 | 1990-12-28 | PROCEDURE TO APPLY LAYERS OF NITRIDE ON TITANIUM. |
BR919101899A BR9101899A (en) | 1990-07-04 | 1991-05-09 | PROCESS FOR THE APPLICATION OF NITRET LAYERS ON TITANIUM |
CS911988A CZ279472B6 (en) | 1990-07-04 | 1991-06-28 | Process for applying nitride layers on titanium and alloys thereof |
JP3161349A JPH0649924B2 (en) | 1990-07-04 | 1991-07-02 | Method for applying a nitride layer to a member made of titanium and titanium alloy |
SU915001026A RU1836484C (en) | 1990-07-04 | 1991-07-03 | Method of application of nitride layers on parts made of titanium and titanium alloys |
PT98195A PT98195A (en) | 1990-07-04 | 1991-07-03 | PROCESS FOR THE APPLICATION OF NITRIDE LAYERS ON TITANIUM |
PL91290931A PL166281B1 (en) | 1990-07-04 | 1991-07-03 | Method of producing nitride coatings on titanium substrates |
US07/984,136 US5292555A (en) | 1990-07-04 | 1992-12-01 | Process for applying nitride layers to titanium |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4021286A DE4021286C1 (en) | 1990-07-04 | 1990-07-04 |
Publications (1)
Publication Number | Publication Date |
---|---|
DE4021286C1 true DE4021286C1 (en) | 1991-02-21 |
Family
ID=6409636
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE4021286A Expired - Lifetime DE4021286C1 (en) | 1990-07-04 | 1990-07-04 | |
DE59010178T Expired - Lifetime DE59010178D1 (en) | 1990-07-04 | 1990-12-28 | Process for applying nitride layers on titanium |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE59010178T Expired - Lifetime DE59010178D1 (en) | 1990-07-04 | 1990-12-28 | Process for applying nitride layers on 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 (7)
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 |
WO2008079977A2 (en) | 2006-12-22 | 2008-07-03 | Iap Research, Inc. | System and method for surface hardening of refractory metals |
CN101652319B (en) * | 2007-02-28 | 2014-03-19 | 沃特世科技公司 | Liquid-chromatography apparatus having diffusion-bonded titanium components |
CN100537805C (en) * | 2007-10-30 | 2009-09-09 | 沈阳宝鼎化工设备制造有限公司 | Wear-resistant and corrosion-resistant spare part and surface treatment process thereof |
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 (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1796212C (en) * | 1972-12-21 | Institut fur Harterei Technik, 2820 Bremen Lesum | Process for boriding titanium and its alloys | |
EP0105835B1 (en) * | 1982-09-07 | 1987-12-23 | 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 AT AT90125660T patent/ATE135058T1/en not_active IP Right Cessation
- 1990-12-28 ES ES90125660T patent/ES2085320T3/en not_active Expired - Lifetime
-
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 PL PL91290931A patent/PL166281B1/en unknown
- 1991-07-03 PT PT98195A patent/PT98195A/en not_active Application Discontinuation
- 1991-07-03 RU SU915001026A patent/RU1836484C/en active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1796212C (en) * | 1972-12-21 | Institut fur Harterei Technik, 2820 Bremen Lesum | Process for boriding titanium and its alloys | |
EP0105835B1 (en) * | 1982-09-07 | 1987-12-23 | Vereinigte Drahtwerke AG | Method of producing a hard layer on articles of ti or ti-alloys |
Also Published As
Publication number | Publication date |
---|---|
TW208721B (en) | 1993-07-01 |
AU627960B2 (en) | 1992-09-03 |
PL166281B1 (en) | 1995-04-28 |
CS198891A3 (en) | 1992-02-19 |
JPH04232247A (en) | 1992-08-20 |
DE59010178D1 (en) | 1996-04-11 |
PT98195A (en) | 1992-04-30 |
NO905209D0 (en) | 1990-11-30 |
JPH0649924B2 (en) | 1994-06-29 |
PL290931A1 (en) | 1992-10-05 |
EP0464265A1 (en) | 1992-01-08 |
BR9101899A (en) | 1992-01-14 |
ES2085320T3 (en) | 1996-06-01 |
EP0464265B1 (en) | 1996-03-06 |
CZ279472B6 (en) | 1995-05-17 |
NO905209L (en) | 1992-01-06 |
RU1836484C (en) | 1993-08-23 |
CN1020476C (en) | 1993-05-05 |
AU6760290A (en) | 1992-01-09 |
CN1057866A (en) | 1992-01-15 |
ATE135058T1 (en) | 1996-03-15 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
8100 | Publication of patent without earlier publication of application | ||
D1 | Grant (no unexamined application published) patent law 81 | ||
8364 | No opposition during term of opposition | ||
8339 | Ceased/non-payment of the annual fee |