EP1464715B1 - Verfahren zur Herstellung von reinem Titanbaustoff - Google Patents

Verfahren zur Herstellung von reinem Titanbaustoff Download PDF

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Publication number
EP1464715B1
EP1464715B1 EP04006388A EP04006388A EP1464715B1 EP 1464715 B1 EP1464715 B1 EP 1464715B1 EP 04006388 A EP04006388 A EP 04006388A EP 04006388 A EP04006388 A EP 04006388A EP 1464715 B1 EP1464715 B1 EP 1464715B1
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EP
European Patent Office
Prior art keywords
pickling
pure titanium
titanium
building material
content
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Expired - Fee Related
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EP04006388A
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English (en)
French (fr)
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EP1464715A1 (de
Inventor
Takashi c/o Osaka Branch Kobe steel Ltd Yashiki
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Kobe Steel Ltd
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Kobe Steel Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • 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
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals

Definitions

  • the present invention relates to a method of manufacturing a pure titanium building material resistant to secular discoloration for constructing external walls of buildings, and reinforcing members.
  • a titanium material has a surface coated with an oxide film, which is perfectly resistant to rusting, is excellent in corrosion resistance and has desirable mechanical properties. Titanium building materials have been watched with keen interest for their excellent properties.
  • the discolored titanium materials do not glitter in beautiful metallic colors any longer and spoil the aesthetic design of buildings. Although it is possible to renew the original beautiful appearance of titanium materials discolored by aging by maintenance work including wiping or polishing, such maintenance work is very expensive, and some parts of buildings reject maintenance work. Accordingly, studies have been made to develop titanium materials resistant to secular discoloration.
  • JP 2002 242 359 discloses a pure Ti material for building material having Vietnamese oxide film formed through annealing.
  • JP 9 003 573 also discloses a pure Ti sheet for building material those composition includes controlled levels of Fe, Ni, Cr and oxygene.
  • Titanium and titanium alloy materials disclosed in Jpn. Pat. No. 3255610 have an oxide film of 100 ⁇ or below and a surface layer having a specified C content.
  • a technique intended to solve problems resulting from secular discoloration by specifying the C content of a surface layer is disclosed also in JP-A 2001-348634 .
  • a titanium sheet manufacturing process according to this technique anneals a cold-rolled titanium sheet at 750 to 800°C for 3 to 5 min to make a layer having a high C content, which is considered to cause secular discoloration, vanish.
  • Inventors of the present invention studied various titanium materials to solve the foregoing problems, and repeated sever evaluation of secular-discoloration resistance of the titanium materials and found that specific impurities contained in the titanium materials dominate the secular-discoloration resistance of the titanium materials.
  • Pure titanium and titanium alloys are used for forming pure titanium building materials.
  • Most pure titanium building materials are formed of industrial pure titanium of Grade 1 JIS containing impurities in a small quantity and excellent in formability. Even if titanium building materials are formed of a material not containing titanium scraps and containing only industrial titanium Grade 1, JIS, i.e., sponge titanium, the titanium building materials inevitably contain various impurities in small contents.
  • Chemical requirements for industrial titanium Grade 1, JIS specify impurity contents including oxygen content and iron content in terms of formability. Any attention has not been paid to such impurity contents at all in improving secular-discoloration resistance.
  • the inventors of the present invention found that pure building materials formed of pure titanium having specific impurity contents below predetermined levels are scarcely subject to secular discoloration and have developed a method according to the present claim 1.
  • a pure titanium building material manufacturing method comprises the steps of: forming a pure titanium building material of pure titanium having an Fe content of 0.08% by mass or below, a Nb content of 0.02% by mass or below and a Co content of 0.02% by mass or below, pickling the pure titanium building material; and heating the pickled pure titanium building material at a temperature X (°C) in the range of 130 to 280°C for a heating time T (min) so as to meet a condition expressed by: T ⁇ 239408 ⁇ X -2.3237 .
  • the heating step forms a surface oxide film of a proper thickness effective in suppressing detrimental coloring and reduces impurities that cause discoloration as well.
  • the pure titanium building material has a surface oxide film of 170 ⁇ or below in thickness.
  • a pure titanium building material having a thicker surface oxide film has lower secular-discoloration resistance
  • the pure titanium building material has a beautiful silver white color, and the growth of the surface oxide film can be effectively suppressed when the pure titanium building material has the composition defined as above and the surface oxide film is 170 ⁇ or below. Therefore, the pure titanium building material having a surface oxide film of 170 ⁇ or below in thickness is not subject to secular discoloration to an extent that spoils aesthetic design and maintains silver white appearance.
  • the pure titanium building material manufactured by the manufacturing method according to claim 1 is highly resistant to secular discoloration.
  • the pure titanium building material produced by the method of the present invention is very useful as a building material for constructing buildings to which high aesthetic design is essential, those exposed to sea wind and acid rain, those requiring high maintenance cost and those difficult to maintain.
  • the pure titanium building material produced by the method of the present invention is very industrially useful.
  • the pure titanium building material manufactured according to the method of present invention is formed of pure titanium having an Fe content of 0.08% by mass or below, a Nb content of 0.02% by mass or below, and a Co content of 0.02% by mass or below.
  • Fe, Nb and Co contained in a pure titanium forming a pure titanium building material cause the development of secular discoloration of the pure titanium building material. This fact was discovered by the inventors.
  • the development of the secular discoloration of the pure titanium building material can be remarkably retarded by controlling the Fe, Nb and Co contents of the pure titanium below the foregoing specified Fe, Nb and Co contents.
  • X% by mass or below signifies that pure titanium does not contain the impurity at all or contains the impurity in an ignorable amount.
  • the content is expressed in "percent by mass", which will be simply expressed by “percent” hereinafter.
  • Fe content is 0.06% or below (more preferably, 0.05% or below)
  • Nb content is 0.015% or below (more preferably, 0.01% or below)
  • Co content is 0.015% or below (more preferably, 0.01% or below).
  • the Fe, Nb and Co contents of a raw titanium material are adjusted. More concretely, the impurity contents of sponge titanium, i.e., a raw titanium material, are measured, and the sponge titanium is used if the sponge titanium has Fe, Nb and Co contents not exceeding the foregoing specified Fe, Nb and Co contents.
  • pure titanium used herein signifies a substance containing Fe, Nb and Co in contents not exceeding the specified Fe, Nb and Co contents, inevitable impurities, and Ti as the remainder.
  • the thickness of the surface oxide film of the pure titanium building material as manufactured is 170 ⁇ or below.
  • the pure titanium building material having the surface oxide film of 170 ⁇ or below in thickness and having a composition specified by the present invention has a beautiful silver white color characteristic of titanium.
  • the pure titanium building material produced by the method of the present invention effectively suppresses the growth of the surface oxide film that causes discoloration and hence the pure titanium building material is excellent as a building material.
  • the thickness of the surface oxide film can be adjusted by adjusting conditions for growing a surface oxide film during the manufacture of the pure titanium building material.
  • the surface oxide film grows when the pure titanium building material is exposed to oxygen contained in the atmosphere during an annealing process and is removed by pickling. Therefore, the thickness of the surface oxide film can be adjusted by adjusting vacuum for vacuum annealing, the temperature of the workpiece at the start of exposure of the vacuum annealed workpiece to the atmosphere or the degree of rinsing after a pickling process. More concretely, the thickness of a sample surface oxide film and conditions for forming a surface oxide film are adjusted repeatedly to determined desirable conditions.
  • the thickness of the surface oxide film can be measured by, for example, Auger electron spectroscopy.
  • the sputtering rate may be estimated from a sputtering rate at which a SiO 2 film is deposited by sputtering conforming to measuring sputtering conditions.
  • a pure titanium building material manufacturing method of the present invention includes, at least an ingot manufacturing process, a hot-rolling process, a cold-rolling process and a finishing process. Conditions for those processes may be the same as those for generally known processes. The finishing process subsequent to the cold-rolling process must be carefully designed because the finishing process has significant influence on the surface property of the titanium material.
  • the finishing process for finishing the titanium material is a vacuum annealing process (VA process) or an atmospheric annealing and pickling process (AP finishing process).
  • VA process vacuum annealing process
  • AP finishing process atmospheric annealing and pickling process
  • the surface oxide film of a titanium material finished by the VA process contains a large amount of C which causes secular discoloration. Therefore a pickling process is preferably employed in finishing the titanium material.
  • the pure titanium building material manufacturing method may include an additional process, provided that the additional process does not spoil the effect of pickling.
  • a workpiece processed by pickling may be finished by light rolling (skin pass) using dulling rolls in a dull surface to improve the design (sharpness) of the workpiece.
  • a titanium material having high secular discoloration resistance is obtained by subjecting the pickled workpiece to a heat treatment process that heats the pickled workpiece at a temperature X (°C) in the range of 130 to 280°C for a heating time T (min) so as to meet a condition expressed by: T ⁇ 239408 ⁇ X -2.3237 .
  • Heating the workpiece at temperatures in the range of 130 to 280°C does not cause detrimental discoloration that spoils the design, and the heat treatment process meeting the condition expressed by the expression has further improved secular discoloration resistance.
  • the reason why the heat treatment process improves the secular discoloration resistance is not clearly known, it is considered that the heat treatment process changes the construction of the oxide film.
  • detrimental discoloration occurs when the workpiece is heated at a high temperature not lower than 250°C (250 to 280°C) for a long time in the atmosphere. Therefore it is desirable to heat the workpiece for a heating time not longer than 30 min, more preferably 10 min or below, when the workpiece is to be heated at such a high temperature. Even if discoloration occurs, the workpiece is colored at the initial stage of discoloration in a very light golden color, which improves the design instead of spoiling the same. In some cases, the heating may be stopped at such an initial stage to provide a pure titanium building material discolored in a very light golden color.
  • the heat treatment process heats the workpiece in either a vacuum atmosphere or an atmospheric atmosphere. Any upper limit heating time is specified for the heat treatment process that heats the workpiece in a vacuum atmosphere because there is no possibility that the workpiece is discolored when the workpiece is heated in a vacuum atmosphere.
  • the pure titanium building material thus fabricated has very high secular discoloration resistance as compared with conventional titanium or titanium alloy building materials.
  • Specimens Nos. 1 to 21 of high-purity titanium (5N, Purity: 99.999% or higher) containing impurity elements in predetermined impurity element contents and respectively having different chemical compositions were produced to examine the effect of impurity contents on secular discoloration.
  • Titanium raw materials respectively having chemical compositions shown in Table 1 were melted in a vacuum button melting furnace and ingots of a weight in the range of 100 to 200 g were produced.
  • the ingots were heated by a first heating process at 1000°C for 1 hr, and then the ingots were hot-rolled by a first hot-rolling process to obtain 6 mm thick plates.
  • the 6 mm thick plates were heated by a second heating process at 1000°C for 10 min and by a third heating process at 850°C for 1 hr, and the thus heated 6 mm thick plates were hot-rolled by a second hot-rolling process to obtain 3 mm thick sheets.
  • the thus hot-rolled sheets were annealed by an annealing process at 800°C for 10 min, and the annealed 3 mm thick sheets were air-cooled.
  • Oxide scale formed on one surface of each of the annealed 3 mm thick sheets was removed by surface grinding in a depth of 0.5 mm.
  • the 3 mm thick sheets were cold-rolled by a cold-rolling process to obtain about 1 mm thick pure titanium sheets.
  • the about 1 mm thick pure titanium sheets were subjected to a final finishing process that annealed the about 1 mm thick pure titanium sheets under the following annealing conditions.
  • the specimens Nos. 13 to 15 having Fe contents outside the Fe content range specified by the present invention are conspicuously discolored, i.e., color differences are large.
  • the specimens Nos. 16 and 17 having Nb contents and Co contents outside a Nb content range and a Co content range specified by the present invention the specimen Nos. 19 and 21 having Nb contents outside the specified Nb content range, and the specimens Nos. 18 and 20 having Co contents outside the specified Co content range are discolored excessively and have color differences ⁇ E* exceeding 5, even though those specimens have Fe contents within the specified Fe content range.
  • specimens Nos. 1 to 12 having Fe, Nb and Co contents within the specified Fe, Nb and Co content ranges have color differences ⁇ E* below 5, and high secular discoloration resistance.
  • the specimens Nos. 22 and 23 were subjected to pickling instead of vacuum annealing in the last process; that is, the specimens Nos. 22 and 23 were treated by atmospheric annealing at 700°C for 20 s after cold rolling, salt immersion at 550°C for 15 s, and pickling of 40 ⁇ m in thickness using a mixture heated at 40°C and containing 15% by mass nitric acid and 1.5% by mass hydrofluoric acid.
  • the thickness of the surface oxide film of each of the specimens was measured before immersing the specimens in a sulfuric acid solution for a secular discoloration resistance test. More concretely, the specimens were subjected to ultrasonic cleaning in acetone, the specimens were dried and oxygen concentration was measured under the following conditions.
  • the thickness of the surface oxide film was calculated using measured data. The thickness was determined by multiplying sputtering time (measured time) required for oxygen concentration to decrease to a middle oxygen concentration between a maximum oxygen concentration and a base oxygen concentration by sputtering rate of about 1.9 nm/min.
  • the pure titanium materials having Fe, Nb and Co contents within the specified Fe, Nb and Co content ranges have color differences ⁇ E* below 5 and have high secular discoloration resistance.
  • the color differences ⁇ E* of the specimens finished by vacuum annealing are greater than those of the specimens finished by pickling. Thus, it is preferable to finish pure titanium building materials by pickling.
  • specimens having the surface oxide films of a thickness not greater than 170 ⁇ have desirably small color differences ⁇ E* and sufficient secular discoloration resistance.
  • Pure titanium sheets in specimens Nos. 46 to 83 were produced by using a pickling process similar to that employed in Example 2.
  • the specimens Nos. 46 to 83 had an Fe content of 0.06 or 0.03% by mass, an Nb content of 0.001% by mass and a Co content of 0.001% by mass.
  • the specimens were finished by heat treatment processes under conditions shown in Table 3. Values of 239408 ⁇ X -2.3237 were calculated.
  • the measured data shown in Table 4 proves that finishing pure titanium building materials by a finishing process including pickling and subsequent heating treatment improves the secular discoloration resistance remarkably.
  • Heating times for the heat treatment processes P, Q and R were shorter than the minimum heating time expressed by 239408 ⁇ X -2.3237 and hence the effect of the heat treatment processes P, Q and R is somewhat low.
  • the heating time T must meet an expression: T ⁇ 239408 ⁇ X -2.3237 for the further improvement of the secular discoloration resistance.
  • Fig. 2 shows the relation between heating time and heating temperature.
  • the specimen processed by the heat treatment process S has a small color difference ⁇ E*, the specimen was colored in a golden color due to heating in the atmosphere at a high temperature of 280°C for a long time of 150 min.
  • pure titanium building materials colored in such a golden color are unsuitable when noncolored pure titanium building materials are desired, pure titanium building materials colored in such a golden color have uses.
  • the color difference ⁇ E* of the specimen processed by the heat treatment process L specifying a heating temperature of 280°C and a heating time of 120 min is greater than that of the specimen processed by the heat treatment process S, the color difference ⁇ E* is satisfactorily small.
  • the specimen processed by the heat treatment process L was colored less than that processed by the heat treatment process S, and was colored in a golden color.
  • Heating time must be 30 min or shorter, more preferably, 10 min or shorter to prevent coloring due to high-temperature heating in the atmosphere.
  • Table 1 Specimen No. Fe content (% by mass) Nb content (% by mass) Co content (% by mass) ⁇ E* 1 0.08 0.02 0.02 4.5 2 0.08 0.01 0.01 4.0 3 0.08 0.005 0.005 3.3 4 0.08 0.001 0.001 2.9 5 0.06 0.02 0.02 2.5 6 0.06 0.01 0.01 2.4 7 0.06 0.005 0.005 2.1 8 0.06 0.001 0.001 1.9 9 0.03 0.02 0.02 2.2 10 0.03 0.01 0.01 2.1 11 0.03 0.005 0.005 1.8 12 0.03 0.001 0.001 1.3 13 0.10 0.001 0.001 9.1 14 0.15 0.001 0.001 14.7 15 0.20 0.001 0.001 18,2 16 0.08 0.03 0.03 8.9 17 0.03 0.03 0.03 6.9 18 0.08 0.005 0.03 6.6 19 0.08 0.03 0.00

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Physical Vapour Deposition (AREA)
  • ing And Chemical Polishing (AREA)

Claims (1)

  1. Herstellungsverfahren für reines Titanbaustoffmaterial, umfassend die Schritte:
    das Bilden eines reinen Titanbaustoffmaterials von reinem Titan mit einem Fe-Gehalt von 0,08 Masse-% oder darunter, einem Nb-Gehalt von 0,02 Masse-% oder darunter und einem Co-Gehalt von 0,02 Masse-% oder darunter, und
    das Beizen des reinen Titanbaustoffmaterials, und
    das Erwärmen des gebeizten reinen Titanbaustoffmaterials bei einer Temperatur X (°C) in dem Bereich von 130 bis 280°C für eine Erwärmungsdauer T (min), um derart eine Bedingung, ausgedrückt durch: T ≥ 239408 x X-2,3237, zu erfüllen.
EP04006388A 2003-03-20 2004-03-17 Verfahren zur Herstellung von reinem Titanbaustoff Expired - Fee Related EP1464715B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2003078522 2003-03-20
JP2003078522 2003-03-20

Publications (2)

Publication Number Publication Date
EP1464715A1 EP1464715A1 (de) 2004-10-06
EP1464715B1 true EP1464715B1 (de) 2008-03-05

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EP04006388A Expired - Fee Related EP1464715B1 (de) 2003-03-20 2004-03-17 Verfahren zur Herstellung von reinem Titanbaustoff

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US (1) US20040187983A1 (de)
EP (1) EP1464715B1 (de)
CN (1) CN1261605C (de)
DE (1) DE602004012183T2 (de)
RU (1) RU2266345C1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109612991A (zh) * 2018-10-29 2019-04-12 成都飞机工业（集团）有限责任公司 一种tc21钛合金热处理表面氧化色的标定方法

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007114218A1 (ja) * 2006-03-30 2007-10-11 Kabushiki Kaisha Kobe Seiko Sho チタン合金及びエンジン排気管
JP4666271B2 (ja) * 2009-02-13 2011-04-06 住友金属工業株式会社 チタン板
CN102899508B (zh) * 2012-09-11 2017-04-12 西安赛特金属材料开发有限公司 一种高强度纯钛材料
CN105887133B (zh) * 2016-06-28 2018-06-29 湖南新发科技有限责任公司 一种电解二氧化锰生产用高变形抗力钛阳极的制备方法
RU2758704C1 (ru) * 2020-12-08 2021-11-01 Андрей Петрович Орлов Способ обработки тонких листов из титана

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JP3052787B2 (ja) * 1995-06-16 2000-06-19 住友金属工業株式会社 建材用純チタン、純チタン板およびその製造方法
JP3219690B2 (ja) * 1996-06-18 2001-10-15 株式会社神戸製鋼所 耐変色性に優れた屋外用チタンまたはチタン合金材
JP3255610B2 (ja) * 1998-06-18 2002-02-12 株式会社神戸製鋼所 耐変色性に優れたチタン材またはチタン合金材およびその製造方法並びに建築用外装材
JP3406898B2 (ja) * 2000-07-28 2003-05-19 新日本製鐵株式会社 変色を生じにくいチタン材とその製造方法
JP3562475B2 (ja) * 2001-02-14 2004-09-08 住友金属工業株式会社 建材用純チタン材

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109612991A (zh) * 2018-10-29 2019-04-12 成都飞机工业（集团）有限责任公司 一种tc21钛合金热处理表面氧化色的标定方法

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DE602004012183D1 (de) 2008-04-17
RU2266345C1 (ru) 2005-12-20
CN1261605C (zh) 2006-06-28
US20040187983A1 (en) 2004-09-30
EP1464715A1 (de) 2004-10-06
DE602004012183T2 (de) 2009-03-12
RU2004108146A (ru) 2005-09-20
CN1534103A (zh) 2004-10-06

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