EP1571233A1 - Verfahren zur Härtung eines Beta-Titan-Teils - Google Patents

Verfahren zur Härtung eines Beta-Titan-Teils Download PDF

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Publication number
EP1571233A1
EP1571233A1 EP05004743A EP05004743A EP1571233A1 EP 1571233 A1 EP1571233 A1 EP 1571233A1 EP 05004743 A EP05004743 A EP 05004743A EP 05004743 A EP05004743 A EP 05004743A EP 1571233 A1 EP1571233 A1 EP 1571233A1
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EP
European Patent Office
Prior art keywords
approximately
beta titanium
titanium member
minutes
heating
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.)
Withdrawn
Application number
EP05004743A
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English (en)
French (fr)
Inventor
Toru Iwai
Kenji Tsubouchi
Yoshikazu Kashimoto
Kentaro Hayashi
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Shimano Inc
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Shimano Inc
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Filing date
Publication date
Application filed by Shimano Inc filed Critical Shimano Inc
Publication of EP1571233A1 publication Critical patent/EP1571233A1/de
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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
    • C23C8/10—Oxidising

Definitions

  • the present invention is directed to metal hardening processes and, more particularly, to a method of hardening a beta titanium member.
  • titanium and titanium alloy are active metals and have low wear resistance. Also, surface processing of either material is extremely difficult.
  • Such methods include forming an outer hardened layer via surface plating or hardening the product surface itself via nitriding or carburizing.
  • plating processes encounter the problems of poor adhesion between the plating layer and the titanium surface and damage to the appearance of the titanium, and surface hardening via nitriding or carburizing encounter the problems of coarsening of the product surface and extended processing times.
  • JP 2003-73796 discloses a surface hardening method wherein a titanium member is heated while buried in a highly oxygen-absorbent powder. The powder reduces the oxygen concentration of the atmosphere surrounding the titanium member by physically preventing the titanium surface from coming into contact with oxygen. As a result, a TiO oxygen diffusion layer is formed in the surface of the titanium member while minimizing the formation of an oxidized outer surface layer.
  • the surface hardness can be increased using such methods, because the titanium member must be buried in oxygen-absorbing powder each time processing is carried out, the process is relatively inefficient and costly. Furthermore, because the titanium member is buried in the oxygen-absorbing powder, the desired cooling rate cannot be obtained following the heat processing, so an appropriate aging treatment cannot be performed.
  • a method of hardening the surface of a beta titanium member comprises the step of heating the beta titanium member in a gas mixture consisting essentially of an inert gas and oxygen. Additional inventive features will become apparent from the description below, and such features alone or in combination with the above features may form the basis of further inventions as recited in the claims and their equivalents.
  • Fig. 1 shows the basic construction of a particular embodiment of a beta titanium surface hardening apparatus 10 in the form of a titanium melting furnace for surface hardening a beta titanium member 11.
  • beta titanium member 11 is placed in a processing chamber S of beta titanium surface hardening apparatus 10, and then beta titanium member 11 is heated in an atmosphere comprising a gas mixture comprising oxygen and an inert gas such as argon gas.
  • an atmosphere comprising a gas mixture comprising oxygen and an inert gas such as argon gas.
  • the oxygen concentration ranges from approximately 0.05 vol% to approximately 20 vol% (preferably approximately 1.0 vol% to approximately 10 vol%)
  • the heating temperature ranges from approximately 700°C to approximately 1000°C (preferably approximately 850°C to approximately 950°C)
  • the heat processing time ranges from approximately 10 minutes to approximately 30 minutes (preferably approximately 15 minutes to approximately 25 minutes).
  • titanium member 11 undergoes an aging treatment at an ambient temperature of from approximately 400°C to approximately 550°C (preferably approximately 850°C to approximately 950°C) for a time of from approximately 6 hours to approximately 16 hours (preferably approximately 10 hours to approximately 14 hours).
  • Figs. 2A and 2B are graphs of surface hardness for various heat treating methods.
  • one line represents an unprocessed beta titanium member
  • another line represents a beta titanium member subjected to an Argon-Oxygen atmosphere of 5 vol% oxygen at 850°C for 10 minutes
  • another line represents a beta titanium member subjected to an Argon-Oxygen atmosphere of 10 vol% oxygen at 850°C for 10 minutes.
  • Fig. 2A one line represents an unprocessed beta titanium member
  • another line represents a beta titanium member subjected to an Argon-Oxygen atmosphere of 5 vol% oxygen at 850°C for 10 minutes
  • another line represents a beta titanium member subjected to an Argon-Oxygen atmosphere of 10 vol% oxygen at 850°C for 10 minutes.
  • one line represents an unprocessed beta titanium member
  • another line represents a beta titanium member subjected to an Argon-Oxygen atmosphere of 1.7 vol% oxygen at 900°C for 10 minutes
  • another line represents a beta titanium member subjected to an Argon-Oxygen atmosphere of 5 vol% oxygen at 900°C for 10 minutes
  • another line represents a beta titanium member subjected to an Argon-Oxygen atmosphere of 10 vol% oxygen at 900°C for 10 minutes.
  • a beta titanium member that was processed at a temperature of 850°C for 10 minutes in an atmosphere having an oxygen concentration of 5 vol% exhibited an HV hardness of 570-400 down to a depth of 0.10 mm (100 ⁇ m) below the surface, as compared to the more or less fixed HV hardness of 400 for an unprocessed beta titanium member.
  • the HV hardness increased to 570-400 from the surface down to a depth of 0.05 mm (50 ⁇ m) below the surface.
  • a beta titanium member that was processed at a temperature of 850°C for 10 minutes in an atmosphere having an oxygen concentration of 10 vol% also exhibited an HV hardness of 570-400 down to a depth of 0.10 mm (100 ⁇ m) below the surface.
  • the HV hardness increased to 570-450 from the surface down to a depth of 0.05 mm (50 ⁇ m) below the surface.
  • a beta titanium member that was processed at a temperature of 900°C for 10 minutes in an atmosphere having an oxygen concentration of 1.7 vol% exhibited an HV hardness of 590-420 from the surface down to a depth of 0.10 mm (100 ⁇ m) below the surface, as compared to the more or less fixed HV hardness of 450 for an unprocessed beta titanium member.
  • the HV hardness increased to 590-495 from the surface down to a depth of 0.05 mm (50 ⁇ m) below the surface.
  • a beta titanium member that was processed at a temperature of 900°C for 10 minutes in an atmosphere having an oxygen concentration of 5 vol% exhibited an HV hardness of 580-470 from the surface down to a depth of 0.10 mm (100 ⁇ m) below the surface.
  • the HV hardness increased to 585-515 from the surface down to a depth of 0.05 mm (50 ⁇ m) from the surface.
  • a beta titanium member that was processed at a temperature of 900°C for 10 minutes in an atmosphere having an oxygen concentration of 10 vol% exhibited an HV hardness of 545-395 down to a depth of 0.10 mm (100 ⁇ m) from the surface.
  • the HV hardness increased to 545-490 from the surface down to a depth of 0.05 mm (50 ⁇ m) below the surface.
  • a temperature of 900°C resulted in a greater increase in hardness over a greater range than a temperature of 850°C. More specifically, when the beta titanium member was subjected to a processing temperature of 900°C, the HV hardness declined more gradually beyond a depth of 0.02 mm (20 m) below the surface than it did when the beta titanium member was subjected to a processing temperature of 800°C. Therefore, taking into consideration the melting temperature of beta titanium, it is preferable that processing be carried out at a temperature in the range of from approximately 850°C to approximately 950°C.
  • Fig. 2B shows that HV hardness increases to a greater degree when the oxygen concentration is 1.7 vol% than when it is 5 vol%. The same is true when the oxygen concentration is 5 vol% than when it is 10 vol%. Therefore, in order to minimize the formation of an oxidized layer while increasing HV hardness, it is preferable that processing be carried out within an oxygen concentration in a range of from approximately 1 vol% to approximately 10 vol%.
  • Fig. 3 is a bar graph of the results of friction testing beta titanium members when subjected to the methods shown in Figs. 2A and 2B.
  • the beta titanium member that was heated at 850°C for 10 minutes in an oxygen concentration of 5 vol% is referred to as a first sample
  • the beta titanium member that was heated at 900°C for 10 minutes in an oxygen concentration of 10 vol% is referred to as a second sample
  • a beta titanium member that was heated at 900°C for 10 minutes in an oxygen concentration of 5 vol% is referred to as a third sample
  • a beta titanium member that was heated at 900°C for 10 minutes in an oxygen concentration of 1.7 vol% is referred to as a fourth sample.
  • the average amount of wear was 0.15 mm for the unprocessed beta titanium member, 0.138 mm for the first sample, 0.132 mm for the second sample, 0.110 mm for the third sample, and 0.104 mm for the fourth sample.
  • the average wear amount was lower for the processed beta titanium members than for the unprocessed beta titanium member.
  • processing at a temperature in a range of from approximately 850°C to approximately 900°C results in wear resistance and surface hardness values that are higher than the equivalent values for an unprocessed beta titanium member.
  • the average amount of wear can be reduced when heating is carried out at 850°C than at 900°C. Accordingly, heating at a temperature of 850°C may be preferred in some applications.
  • the average amount of wear can be reduced by reducing the oxygen concentration from 10 vol% to 1.7 vol%, so such oxygen concentration reduction also may be prefererable in some applications.
  • Fig. 4 is a cross sectional diagram of a surface hardened beta titanium member 11 formed according to the methods taught herein.
  • beta titanium member 11 comprises a topmost oxidized layer 11a, a hardened oxygen diffusion layer 11b having a thickness of approximately 100 ⁇ m below oxidized layer 11a, and an unprocessed layer 11c below hardened layer 11b.
  • Oxidized layer 11a has a thickness of from approximately 0 ⁇ m to approximately 5 ⁇ m.
  • Such a layer is significantly thinner than the oxidized layers formed in the prior art processes that heat the titanium member in atmospheric air.
  • removal of oxidized layer 11a created by the teachings herein is very easy.
  • hardened layer 11b can be formed to a thickness of at least 70 ⁇ m (preferably 100 ⁇ m) while minimizing the thickness of oxidized layer 11a, a beta titanium member 11 having increased surface hardness can be efficiently obtained.
  • a hardened layer may be formed to a thickness of 300 ⁇ m with an increased HV hardness of 500, but an oxidized layer having a thickness of 100 ⁇ m is formed on top of the hardened layer.
  • An oxidized layer on the surface of the product is undesirable because it tarnishes the product's appearance. Since the oxidized layer is hard and brittle, removal of such a thick layer is extremely cumbersome and impairs production efficiency.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
EP05004743A 2004-03-04 2005-03-03 Verfahren zur Härtung eines Beta-Titan-Teils Withdrawn EP1571233A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004060523 2004-03-04
JP2004060523A JP2005248256A (ja) 2004-03-04 2004-03-04 ベータ型チタンの表面硬化処理方法およびベータ型チタン系部材、ベータ型チタンの表面硬化処理装置

Publications (1)

Publication Number Publication Date
EP1571233A1 true EP1571233A1 (de) 2005-09-07

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EP05004743A Withdrawn EP1571233A1 (de) 2004-03-04 2005-03-03 Verfahren zur Härtung eines Beta-Titan-Teils

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US (1) US20050194075A1 (de)
EP (1) EP1571233A1 (de)
JP (1) JP2005248256A (de)
CN (1) CN1664160A (de)
TW (1) TW200536960A (de)

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Publication number Priority date Publication date Assignee Title
US8566943B2 (en) * 2009-10-01 2013-10-22 Kaspersky Lab, Zao Asynchronous processing of events for malware detection
CN102162080A (zh) * 2011-03-31 2011-08-24 戚培毅 医用钛植入器械表面改性层及其制备方法
CN105349934B (zh) * 2015-07-03 2018-03-20 苏州大学 一种钛合金的表面强化处理方法
CN106637049A (zh) * 2017-01-03 2017-05-10 中山源谥真空科技有限公司 一种纯钛或钛合金及其表面硬化方法
WO2018128160A1 (ja) * 2017-01-03 2018-07-12 カシオ計算機株式会社 合金部材およびその表面硬化方法
JP7107501B2 (ja) * 2018-07-11 2022-07-27 株式会社オー・ケー・シー β型チタン合金及びその製造方法
CN113174511A (zh) * 2021-04-02 2021-07-27 西安交通大学 一种具有优良力学性能的β钛合金材料及其制备方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998002595A1 (en) * 1996-07-17 1998-01-22 The University Of Birmingham Surface oxidation of a titanium or titanium alloy article
WO2002008623A1 (en) * 2000-07-18 2002-01-31 Nsk Ltd. Rolling apparatus

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Publication number Priority date Publication date Assignee Title
WO1997010066A1 (fr) * 1995-09-13 1997-03-20 Kabushiki Kaisha Toshiba Procede de fabrication de pales de turbine en alliage de titane et pales de turbines en alliage de titane
JPH11223221A (ja) * 1997-07-01 1999-08-17 Nippon Seiko Kk 転がり軸受
FR2778845B1 (fr) * 1998-05-25 2001-05-04 Oreal Composition de teinture pour fibres keratiniques avec un colorant direct cationique et un polymere substantif
JP2002097914A (ja) * 2000-07-18 2002-04-05 Fuji Oozx Inc チタン合金製エンジンバルブ及びその製造方法
JP2003073796A (ja) * 2001-09-03 2003-03-12 Fuji Oozx Inc チタン系材料の表面処理方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998002595A1 (en) * 1996-07-17 1998-01-22 The University Of Birmingham Surface oxidation of a titanium or titanium alloy article
WO2002008623A1 (en) * 2000-07-18 2002-01-31 Nsk Ltd. Rolling apparatus
EP1225353A1 (de) * 2000-07-18 2002-07-24 Nsk Ltd., Rollvorrichtung

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LIU Z ET AL: "EFFECTS OF OXYGEN AND HEAT TREATMENT ON THE MECHANICAL PROPERTIES OF ALPHA AND BETA TITANIUM ALLOYS", METALLURGICAL TRANSACTIONS A. PHYSICAL METALLURGY AND MATERIALS SCIENCE, METALLURGICAL SOCIETY OF AIME. NEW YORK, US, vol. 19A, March 1988 (1988-03-01), pages 527 - 542, XP002041099 *
MUSHIAKE M ET AL: "DEVELOPMENT OF TITANIUM ALLOY VALVE SPRING RETAINERS", SAE SPECIAL PUBLICATIONS, no. 864, 25 February 1991 (1991-02-25), pages 41 - 49, XP009046186, ISSN: 0099-5908 *

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JP2005248256A (ja) 2005-09-15
TW200536960A (en) 2005-11-16
US20050194075A1 (en) 2005-09-08
CN1664160A (zh) 2005-09-07

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