AU627960B2 - Process for applying nitrite layers to titanium - Google Patents

Process for applying nitrite layers to titanium Download PDF

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Publication number
AU627960B2
AU627960B2 AU67602/90A AU6760290A AU627960B2 AU 627960 B2 AU627960 B2 AU 627960B2 AU 67602/90 A AU67602/90 A AU 67602/90A AU 6760290 A AU6760290 A AU 6760290A AU 627960 B2 AU627960 B2 AU 627960B2
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AU
Australia
Prior art keywords
titanium
mpa
applying
nitride layers
ammonia
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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.)
Ceased
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AU67602/90A
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AU6760290A (en
Inventor
Friedrich Preisser
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Evonik Operations GmbH
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Degussa GmbH
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Publication date
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Anticipated expiration legal-status Critical
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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
    • C23C8/08Solid 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
    • C23C8/24Nitriding

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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)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Road Paving Structures (AREA)
  • Revetment (AREA)

Abstract

An economical method for applying nitride layers to titanium and titanium alloys. In a short time, layer thicknesses of 20 mu m are achieved by nitriding under pressure in an ammonia atmosphere. Temperatures of 500 to 1000 DEG C and pressures of 0.2 to 10 Mpa are required for this purpose.

Description

f F 13M S& F Ref: 148111 J- u 0J COMMONWEALTH OF AUSTRALIA PATENTS ACT 1952 COMPLETE SPECIFICATION
(ORIGINAL)
FOR OFFICE USE: Class Int Class 0o 0 4 o a o a o 4 oo 4444 Complete Specification Lodged: Accepted: Published: Priority: Related Art: Name and Address of Applicant: Degussa Aktieigesellschaft Rodenbacher Chaussee 4 D-6450 Hanau 1 FEDERAL REPUBLIC OF GERMANY o* l o o o 44 a 4 04 4 o f 0 a O Address for Service: Spruson Ferguson, Patent Attorneys Level 33 St Martins Tower, 31 Market Street Sydney, New South Wales, 2000, Australia Complete Specification for the invention entitled: Process for Applying Nitride Layers to Titanium The following statement is a full description of this invention, including the best method of performing it known to me/us 5845/3 -i Description: Process for applying nitride layers to titanium The invention relates to a process for 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 above 500 0
C.
Titanium has some advantages over steel as a construction e" 0 0 material, namely its low specific weight, its corrosion- 'oeo resistance, and its high strength. On the other hand, its 8 °hardness is relatively low, which necessitates a surface Qoo S 15 treatment to increase wear-resistance. This surface ooa 0o treatment generally consists in generating layers of titanium carbide or titanium nitride. Processes known hitherto for nitriding parts composed of titanium and titanium alloys involve the use of high-energy gases or S 20 electromagnetic fields. These processes are very expensive and are only applicable with parts having a simple geometry.
In DE-PS 17 96 212, the surface hardening of titanium by the 0 formation of nitride layers in an ammonia atmosphere at S 25 relatively high temperatures and normal pressure is mentioned.
Although this is intended to produce relatively thick, hard layers, this process has no practical application, since the hydrogen diffusion involved causes the core of the component to become brittle.
EP-OS 0 105 835 describes a process for manufacturing nitride layers on components composed of titanium and titanium alloys by exposing the components in an autoclave to pressures of at least 10 MPa and temperatures of at least 2001C in an ammonia atmosphere. In this case, the ammonia 3 i| must be very pure. Preferably, the nitriding takes place at to 130 MPa and temperatures of 930° to 10000C. This L.
process has the disadvantage that it is very expensive due to the use of autoclaves and very pure ammonia, and layers 20 pm thick can only be obtained in periods of three or more hours.
The object of the present invention is therefore to develop a process for applying nitride layers to parts composed of titanium and titanium alloys by -hermochemical treatment of the parts with ammonia or ammonia-containing gas mixtures o° under pressure and at temperatures of above 5000C which is economical and which permits nitride layers of 20 pm thick or more to be formed within relatively short periods.
This object is achieved according to the invention by carrying out the treatment at temperatures of 500 to 10000C and pressures of 0.2 to 10 MPa, in which case the ammonia partial pressure must be at least 0.2 MPa.
Temperatures of 700 to 9500C and pressures of 0.5 to 7 MPa 0 have proven particularly advantageous, in which case an ammonia partial pressure of at least 0.2 MPa is necessary.
o0o00~ 25 With this pressure process, components composed of titanium I and titanium alloys of any shape and tize can be provided with sufficiently thick nitride layers of 20 pm and more in 04' chamber furnaces. Surprisingly, no extremely pure gases are necessary, but the normal commercial-quality ammonia is j 30 sufficient. Furthermore, it is possible to mix nitrogen with the ammonia, in which case only an ammonia partial pressure of at least 0.2 MPa is needed for the nitriding process.
The layer thickness of the titanium nitride forming is dependent, within wide pressure ranges, on the temperature and treatment duration. The surface is golden and affords a *1I
V
i i i i m L ll~-T significant increase in hardness. At pressures in the range of above 6 MPa, the layer thickness is almost independent of the pressure.
The diagram shows the formation of a titanium nitride layer on parts composed of pure titanium as a function of the pressure and temperature of the ammonia-containing atmosphere.
Even at temperatures of 5000C, for example, at 2 MPa bar) absolute pressure, after one hour a TiN layer of 10 pm thick was measured. At 880 0 C, in this time a pure TiN layer of 20 pm is built up.
15 At a pressure of 6 MPa (=60 bar), a TiN layer of 30 pm is built up, for example, if the samples are kept at 880°C for one hour.
0 4, *0 0 4,04,0 0* 0* o 0 4 At a further increment of pressure to 9 MPa 90 bar), the 20 effect of the pressure on the thickness of the TiN layer oo decreases. The increase is no longer linear. At even higher pressures, due to the rapidly forming dense TiN 0 layer, only the diffusion of nitrogen through the layer is the time-determining factor.
S In the same way as pure titanium, titanium alloys, such as STiAl 6
V
4 for example, can be nitrided.
For these coatings, no autoclave is needed, but the treatment can take place in a standard commercial chamber furnace.

Claims (1)

  1. 2. Process for applying nitride layers according to claim 15 1, characterised in that the treatment takes place at temperatures of 700 to 9500C and at pressures of 0.5 to 7 MPa, and the ammonia partial pressure must be at least 0.2 MPa. 0 0 44 44 Q ID 00 0 d 0# 040 0.0a.. 0 0 4400 0 040 5 An econon titanium thicknesE an ammoni 1000CC an 0~4 20 0a 4 0 25 DATED this TWENTY-SIXTH day of NOVEMBER 1990 Degussa Aktiengesellschaft 4 0 0404B 0 4 04 0 0 04 Patent Attorneys for the Applicant SPRUSON FERGUSON 4440 0 0 04 0r 4 0 I I ii I Abstract: Process for applying nitride layers to titanium An economical process for applying nitride layers to titanium and titanium alloys. Within a short time, layer thicknesses of 20 pm are obtained by pressure-nitriding in an ammonia atmosphere. To this end, temperatures of 500 to 1000 0 C and pressures of 0.2 to 10 MPa are necessary. 0? 9 0 99 00*0 r.0 000 0 0 0 9 0* 0 *u 9 0 0 *o n)~IL L .II 'F 61h..-
AU67602/90A 1990-07-04 1990-11-29 Process for applying nitrite layers to titanium Ceased AU627960B2 (en)

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
AU6760290A AU6760290A (en) 1992-01-09
AU627960B2 true AU627960B2 (en) 1992-09-03

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AU67602/90A Ceased AU627960B2 (en) 1990-07-04 1990-11-29 Process for applying nitrite layers to titanium

Country Status (14)

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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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000063454A1 (en) * 1999-04-15 2000-10-26 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
CN102699516B (en) * 2007-02-28 2015-03-18 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 (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2804410A (en) * 1953-10-27 1957-08-27 Nat Lead Co Method for nitriding titanium surfaces

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH650532A5 (en) * 1982-09-07 1985-07-31 Ver Drahtwerke Ag METHOD FOR FORMING A HARD COATING IN THE COMPONENT FROM ELEMENTS OF THE FOURTH, FIFTH OR SIX SUB-GROUPS OF THE PERIODIC SYSTEM OR ITS ALLOYS.

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2804410A (en) * 1953-10-27 1957-08-27 Nat Lead Co Method for nitriding titanium surfaces

Also Published As

Publication number Publication date
CN1020476C (en) 1993-05-05
EP0464265B1 (en) 1996-03-06
DE59010178D1 (en) 1996-04-11
TW208721B (en) 1993-07-01
RU1836484C (en) 1993-08-23
ATE135058T1 (en) 1996-03-15
CN1057866A (en) 1992-01-15
BR9101899A (en) 1992-01-14
NO905209D0 (en) 1990-11-30
JPH0649924B2 (en) 1994-06-29
PT98195A (en) 1992-04-30
PL290931A1 (en) 1992-10-05
ES2085320T3 (en) 1996-06-01
AU6760290A (en) 1992-01-09
CZ279472B6 (en) 1995-05-17
NO905209L (en) 1992-01-06
JPH04232247A (en) 1992-08-20
CS198891A3 (en) 1992-02-19
DE4021286C1 (en) 1991-02-21
PL166281B1 (en) 1995-04-28
EP0464265A1 (en) 1992-01-08

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