CN101128609A - Method for casting titanium alloy - Google Patents
Method for casting titanium alloy Download PDFInfo
- Publication number
- CN101128609A CN101128609A CNA2006800059761A CN200680005976A CN101128609A CN 101128609 A CN101128609 A CN 101128609A CN A2006800059761 A CNA2006800059761 A CN A2006800059761A CN 200680005976 A CN200680005976 A CN 200680005976A CN 101128609 A CN101128609 A CN 101128609A
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- temperature
- alloy
- titanium
- titanium alloy
- solution annealing
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/002—Castings of light metals
- B22D21/005—Castings of light metals with high melting point, e.g. Be 1280 degrees C, Ti 1725 degrees C
-
- 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
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- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Forging (AREA)
- Powder Metallurgy (AREA)
- Materials For Medical Uses (AREA)
- Continuous Casting (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for casting objects from a ss-titanium alloy containing titanium molybdenum with a molybdenum content of 7.5 to 25 %. According to the invention: a melting of the alloy is carried out at a temperature of higher than 1770 DEG C; the molten alloy is precision cast into a mold corresponding to the object to be produced, and this cast object is subjected to a hot-isostatic pressing, solution annealing and subsequent quenching. An efficient production of objects made from ss-titanium alloys in the precision casting process is achieved using the inventive method. The invention thus creates the possibility of combining the advantageous properties of ss-titanium alloys, particularly their excellent mechanical properties, with the advantages of a production of objects in the precision casting process. Even objects having complex shapes, which could not or could not be sensibly produced by conventional forging methods, can be produced from a ss-titanium alloy thanks to the invention.
Description
The present invention relates to be used for by beta-titanium alloy, more specifically, titanium-molybdenum alloy, the method for cast object.
Titanium alloy is employed more and more widely owing to have numerous favourable character.Titanium alloy is especially owing to have good chemical stability (even when high temperature), mechanical properties that weight is low and excellent, and is used in the very high all areas of material requirements.Consider to have excellent biocompatibility, titanium alloy also preferentially is used for medical field, in particular for implant and prosthese.
Known have various methods that titanium alloy is shaped.Except machining, these methods mainly comprise casting and forging method.Be difficult to casting owing to it is found that titanium alloy, so titanium alloy is a wrought alloy in principle, what adopt usually is forging method for this reason.Complicated shape adopts described castmethod usually, but has caused the restriction aspect the selection appropriate alloy.Especially, have been found that, can only obtain to allow the unsatisfied result of people (US-A2004/0136859) when casting during beta-titanium alloy.
The present invention is based on the target that improved castmethod is provided for beta-titanium alloy, make like this and can prepare more complicated shape with good material character.
Solution according to the present invention is to have the method for the feature of main claim.Favourable limits the theme that has constituted dependent claims through a step.
According to the present invention, by containing in the method for beta-titanium alloy cast object that titanium molybdenum and molybdenum content are 7.5-25%, alloy is in the temperature fusion that surpasses 1770 ℃, the fused alloy by precision casting to the corresponding to casting mould of object to be prepared in, carry out hot isostatic pressing, solution annealing is quenched then.
In this article, object is construed as at the end-use formed article.Object can be the parts that are used for jet engine, rotor bearing, wing case (Fl ü gelkasten) or other supporting structure part in air system for example, perhaps can endoprosthesis in medical field, such as hip prosthesis, perhaps implant is such as plate or nail or dental implant.In the application's context, the term object does not comprise will be by the further briquet of processing of manufacturing process, that is, especially do not comprise by the diecasting preparation, be used for by forging the ingot of further processing.
The method according to this invention adopts casting method to realize preparing object economically by beta-titanium alloy.So, the invention provides favourable character, especially its excellent mechanical properties and the advantages that adopts casting method the to prepare object possibility of getting up with beta-titanium alloy.The invention enables and to prepare the complex-shaped object that can not or can not prepare economically by beta-titanium alloy by traditional forging method.So the present invention has also opened in the Application Areas aspect the complexity shaping object for beta-titanium alloy, have favourable mechanical properties and a biocompatibility and this alloy is known.
The content of molybdenum in the alloy or molybdenum equivalent is 7.5-25%.Such result is, especially for molybdenum content for at least 10% the situation, when being low to moderate room temperature range, β-phase is also fully stable.Preferred described content is 12-16%.Make like this and can obtain metastable β-phase by the quick cooling after precision casting.Usually need not to add other alloy forming element.Especially, need not to add vanadium or aluminium.Need not these elements and brought above-mentioned advantage, the toxicity that promptly comes from these alloy forming elements can be avoided.This equally correspondingly is applicable to bismuth, and bismuth does not have the biocompatibility identical with titanium yet.
Have been found that the invention enables to use the beta-titanium alloy that may be used for precision casting so far hardly, prepare than the α/beta-titanium alloy that up to the present is used for precision casting, such as for example TiA16V4, more complicated shape.The method according to this invention has obtained improved mould and has filled behavior.The present invention this means owing to can go out to have higher-quality, especially sharp-pointed limit in the precision casting process of preparing.Because improved mould is filled behavior, so interstitial trend also descends in the precision casting.
Adopt cold wall crucible vacuum induction equipment to come the fusion beta-titanium alloy to suit.Such equipment can reach reliable molten titanium molybdenum alloy to carry out the required high temperature of precision casting.For example, the fusing point of TiMo15 is 1770 ℃.In order to realize reliable precision casting, should add about 60 ℃.So, in general, for TiMo15, must reach 1830 ℃.
For hot isostatic pressing, preferably at the β-transition temperature that equals titanium maxter alloy at most but minimum temperature than low 100 ℃ of β-transition temperature carry out.
Hot isostatic pressing is by the precipitation of dissolving between the dendrite, and offset the following effect that occurs of not wishing: molybdenum is enrichment in dendrite, and in remainder melt poornessization.Being lower than β-transition temperature, especially being low to moderate many 100 ℃ temperature, is favourable.Verified, for the titanium maxter alloy that molybdenum content is 15%, under the argon pressure that approximately 1100-1200 clings to, 710 ℃-760 ℃ temperature, 740 ℃ of preferably approximatelies are suitable.
Verified, for solution annealing, at least 700 ℃ until 880 ℃, and preferred 800 ℃-860 ℃ temperature is suitable.In order to reach protective atmosphere, preferably use hydrogen.This has improved the ductility of alloy.
By water object being quenched after solution annealing is easily.The preferred cold water that adopts.In this article, term " cold " is construed as and is meant the not temperature of the tap water of heating.Have been found that quenching has remarkably influenced to the final mechanical properties that obtains of object.Perhaps, quench and also can in shielding gas, carry out, for example, cool off by argon gas.But the result that the result of acquisition does not adopt cold water to obtain is good.
It may be easily that object finally also hardens.If desired, Young's modulus is increased a little.For this reason, preferably be hardened in the about 600 ℃-about 700 ℃ temperature range and carry out.
Be explained in more detail the present invention below with reference to accompanying drawing, described accompanying drawing is for example understood advantageous embodiment.In the accompanying drawings:
The tabular of Fig. 1 has gone out the mechanical properties according to precision casting titanium alloy of the present invention;
Fig. 2 shows the microstructural image that is in as-cast condition after casting at once;
Fig. 3 shows the microstructure image behind hot isostatic pressing;
Fig. 4 shows the microstructure image after solution annealing and quenching subsequently; With
Fig. 5 shows the liquidus line and the solidus temperature of titanium maxter alloy.
Following text will be described the mode of implementing the inventive method.
Starting material are that molybdenum content is 15% beta-titanium alloy (TiMo15).This alloy can be buied with the form of little briquet (ingot).
The object that the first step precision casting is to be cast.Provide casting equipment to be used for fusion and casting TiMo15.This evaluation method selecting optimal equipment is cold wall crucible vacuum induction fusion and casting equipment.Can reach reliable molten Ti Mo15 to carry out the required high temperature of precision casting by such equipment.The fusing point of TiMo15 is 1770 ℃, for reliable precision casting, add about 60 ℃.So, in general, must reach 1830 ℃.Then,, for example adopt wax core and ceramic die, implement the precision casting of melt as consumptive mould (verloren Form) by known method.Such precision casting technology has been used for precision casting TiAl6V4.
Image from Fig. 2 can be found (1000 times of amplifications), has formed dendrite, and a large amount of precipitations has appearred in the zone between dendrite.This is the negative segregation that comes from known titanium maxter alloy.This effect is based on the liquidus line of titanium maxter alloy and the specific distribution of solidus temperature, as shown in Figure 5.Based on shown in liquid phase (T
L) and solid phase (T
S) melt temperature distribute, at first be that solidify in melt in the zone with high molybdenum content, form the dendrite that can find in the drawings in the method.Make the rest part of melt become poor like this, that is, molybdenum content descends.The molybdenum content in the zone between the dendrite in the casting structure is lower than 15%, even can drop to about 10%.Because the molybdenum poornessization, so the zone between the dendrite lacks the β-stablizer of q.s.The result makes α/beta transus temperature raise in the part, cause appearing at the throw out that can recognize among Fig. 2.
The surf zone (Randzone) of that may form in castingprocesses, that be called the α phase, hard crisp layer form is easy to remove by pickling.The thickness of this layer is typically about 0.03mm.
In order to offset the sedimentary disadvantageous effect that occurs in the zone between negative segregation and the dendrite, according to the present invention, after precision casting, removed after the casting die, foundry goods is heat-treated.This specifically is included in the hot isostatic pressing (HIP) that the temperature that just is lower than β-transition temperature is carried out.Described temperature can be 710 ℃-760 ℃, 740 ℃ of preferably approximatelies.Make like this and do not wish that the throw out that occurs dissolves once more in the zone between dendrite.Need not before or after hot isostatic pressing, to carry out any preliminary age hardening (Vorauslagerung).But, in the process of cooling after hot isostatic pressing, especially preferentially between dendrite, be settled out two thin second phases (referring to Fig. 3,1000 * doubly) once more.Cause material to take place undesirably to become fragile like this.
Object only has low ductility behind hot isostatic pressing.
In order to eliminate destructive precipitation, with foundry goods under protective atmosphere (for example, argon gas) at batch annealing.For this reason, selecting temperature range is about 700 ℃-860 ℃, continues a few hours, generally is two hours.In this article, exist reciprocal relation in temperature with between the time length; Temperature is high more, and the shorter time is just enough, and vice versa.After solution annealing, with the foundry goods cold-water quench.Fig. 4 (1000 times of amplifications) shows the structure after solution annealing.Can find β-crystal grain and the precipitation between the superfine dendrite within the described crystal grain (referring to the cloud aggregate of figure upper left quarter).The object that has adopted the inventive method to carry out precision casting has the β-crystal grain of mean sizes greater than 0.3mm in its crystalline structure.This size is the typical sizes according to the crystalline structure of the inventive method acquisition.
Provided the mechanical properties that after solution annealing, obtains in the table in Fig. 1.
Can find, Young's modulus along with solution annealing during temperature increase and descend, particularly, be low to moderate 60000N/mm
2Level.Ductility increases along with the decline of intensity and hardness.For example, after 800 ℃ of solution annealing two hours, the Young's modulus that obtains is 60000N/mm
2, the extension at break amount is about 40%, breaking tenacity Rm is about 730N/mm
2
Claims (8)
1. be used for by comprising the method that titanium molybdenum and molybdenum content are the beta-titanium alloy cast object of 7.5-25%, be characterised in that at the temperature molten alloy that is higher than 1770 ℃, with the molten alloy precision casting to the corresponding to casting mould of object to be made in, hot isostatic pressing, solution annealing and quenching subsequently.
2. the method for claim 1 is characterised in that and adopts the described beta-titanium alloy of cold wall crucible vacuum induction equipment fusion.
3. claim 1 or 2 method are characterised in that described hot isostatic pressing carries out in the most high β-transition temperature and minimum temperature than low 100 ℃ of β-transition temperature in titanium maxter alloy.
4. claim 1 or 2 method are characterised in that about 700 ℃-about 900 ℃ temperature and carry out solution annealing.
5. the method for claim 4 is characterised in that 800 ℃-860 ℃ temperature and carries out solution annealing.
6. the method for one of aforementioned claim is characterised in that and preferably uses cold-water quench after solution annealing.
7. the method for one of aforementioned claim is characterised in that described object is finally hardened.
8. the method for claim 7 is characterised in that 600 ℃-700 ℃ temperature and carries out described sclerosis.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP05004173A EP1696043A1 (en) | 2005-02-25 | 2005-02-25 | Process for casting a Titanium-alloy |
| EP05004173.0 | 2005-02-25 | ||
| PCT/EP2006/001790 WO2006089790A1 (en) | 2005-02-25 | 2006-02-27 | Method for casting titanium alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101128609A true CN101128609A (en) | 2008-02-20 |
| CN100594248C CN100594248C (en) | 2010-03-17 |
Family
ID=34933944
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200680005976A Expired - Fee Related CN100594248C (en) | 2005-02-25 | 2006-02-27 | Method for casting titanium alloy |
Country Status (18)
| Country | Link |
|---|---|
| EP (2) | EP1696043A1 (en) |
| JP (1) | JP5155668B2 (en) |
| KR (1) | KR101341298B1 (en) |
| CN (1) | CN100594248C (en) |
| AR (1) | AR052391A1 (en) |
| AT (1) | ATE438746T1 (en) |
| AU (1) | AU2006218029B2 (en) |
| BR (1) | BRPI0607832A2 (en) |
| CA (1) | CA2597248C (en) |
| DE (1) | DE502006004443D1 (en) |
| DK (1) | DK1851350T3 (en) |
| ES (1) | ES2328955T3 (en) |
| MX (1) | MX2007010366A (en) |
| PL (1) | PL1851350T3 (en) |
| RU (1) | RU2402626C2 (en) |
| TW (1) | TWI395821B (en) |
| WO (1) | WO2006089790A1 (en) |
| ZA (1) | ZA200707586B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102019401A (en) * | 2010-12-30 | 2011-04-20 | 哈尔滨工业大学 | Cast forming method of small titanium alloy or titanium-aluminum alloy complicated casting |
| CN102978554A (en) * | 2012-11-13 | 2013-03-20 | 安徽春辉仪表线缆集团有限公司 | Titanium alloy valve rod preparation method of plug valve |
| CN104550949A (en) * | 2013-10-24 | 2015-04-29 | 中国科学院金属研究所 | Method for rapidly forming Ti-6Al-4V three-dimensional metal parts by electron beams |
| CN105817608A (en) * | 2016-04-29 | 2016-08-03 | 南京宝泰特种材料股份有限公司 | Titanium alloy smelting and casting method |
| CN111850346A (en) * | 2020-08-06 | 2020-10-30 | 西部金属材料股份有限公司 | High-strength titanium alloy without solid solution aging treatment and preparation method thereof |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9827605B2 (en) * | 2011-02-23 | 2017-11-28 | National Institute For Materials Science | Ti—Mo alloy and method for producing the same |
| CN102294436B (en) * | 2011-09-19 | 2013-01-02 | 哈尔滨实钛新材料科技发展有限公司 | Method for precisely casting titanium alloy and titanium aluminum alloy with low cost |
| RU2492275C1 (en) * | 2012-01-11 | 2013-09-10 | Открытое Акционерное Общество "Корпорация Всмпо-Ависма" | Method of producing plates from two-phase titanium alloys |
| KR20220122374A (en) | 2021-02-26 | 2022-09-02 | 창원대학교 산학협력단 | Method for vacuum centrifugal casting of titanium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS4852614A (en) * | 1971-11-04 | 1973-07-24 | ||
| JPS5217307A (en) * | 1975-07-31 | 1977-02-09 | Kobe Steel Ltd | Process for heat treatment of beta-type titanium alloy |
| JPH0686638B2 (en) * | 1985-06-27 | 1994-11-02 | 三菱マテリアル株式会社 | High-strength Ti alloy material with excellent workability and method for producing the same |
| US4612066A (en) * | 1985-07-25 | 1986-09-16 | Lev Levin | Method for refining microstructures of titanium alloy castings |
| US4857269A (en) * | 1988-09-09 | 1989-08-15 | Pfizer Hospital Products Group Inc. | High strength, low modulus, ductile, biopcompatible titanium alloy |
| JP2541341B2 (en) * | 1990-05-15 | 1996-10-09 | 大同特殊鋼株式会社 | Precision casting method and precision casting apparatus for Ti and Ti alloy |
| JP3041080B2 (en) * | 1991-04-19 | 2000-05-15 | 電気興業株式会社 | Precision casting equipment |
| US5226982A (en) * | 1992-05-15 | 1993-07-13 | The United States Of America As Represented By The Secretary Of The Air Force | Method to produce hollow titanium alloy articles |
| US5947723A (en) * | 1993-04-28 | 1999-09-07 | Gac International, Inc. | Titanium orthodontic appliances |
| JPH0841565A (en) * | 1994-07-29 | 1996-02-13 | Mitsubishi Materials Corp | Titanium alloy casting having high strength and high toughness |
| JPH10130757A (en) * | 1996-10-25 | 1998-05-19 | Daido Steel Co Ltd | Inplant made of ti alloy |
| US20040136859A1 (en) * | 2000-04-12 | 2004-07-15 | Cana Lab Corporation | Titanium alloys having improved castability |
| JP2005530929A (en) * | 2002-06-27 | 2005-10-13 | メムリー コーポレーション | Beta titanium compounds and their production |
| US20040168751A1 (en) * | 2002-06-27 | 2004-09-02 | Wu Ming H. | Beta titanium compositions and methods of manufacture thereof |
| DE102004022458B4 (en) * | 2004-04-29 | 2006-01-19 | Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. | Cold-formable titanium-based alloy bodies and process for their production |
| EP1695676A1 (en) * | 2005-02-25 | 2006-08-30 | WALDEMAR LINK GmbH & Co. KG | Method of producing a medical implant made of a beta-Titanium-Molybdenum-alloy and according implant |
-
2005
- 2005-02-25 EP EP05004173A patent/EP1696043A1/en not_active Withdrawn
-
2006
- 2006-02-24 AR ARP060100693A patent/AR052391A1/en active IP Right Grant
- 2006-02-24 TW TW095106325A patent/TWI395821B/en not_active IP Right Cessation
- 2006-02-27 PL PL06707301T patent/PL1851350T3/en unknown
- 2006-02-27 DK DK06707301T patent/DK1851350T3/en active
- 2006-02-27 DE DE502006004443T patent/DE502006004443D1/en active Active
- 2006-02-27 AU AU2006218029A patent/AU2006218029B2/en not_active Ceased
- 2006-02-27 EP EP06707301A patent/EP1851350B1/en not_active Not-in-force
- 2006-02-27 CN CN200680005976A patent/CN100594248C/en not_active Expired - Fee Related
- 2006-02-27 KR KR1020077021726A patent/KR101341298B1/en active IP Right Grant
- 2006-02-27 WO PCT/EP2006/001790 patent/WO2006089790A1/en active Application Filing
- 2006-02-27 RU RU2007135062/02A patent/RU2402626C2/en not_active IP Right Cessation
- 2006-02-27 JP JP2007556567A patent/JP5155668B2/en not_active Expired - Fee Related
- 2006-02-27 CA CA2597248A patent/CA2597248C/en not_active Expired - Fee Related
- 2006-02-27 ES ES06707301T patent/ES2328955T3/en active Active
- 2006-02-27 BR BRPI0607832-0A patent/BRPI0607832A2/en not_active Application Discontinuation
- 2006-02-27 MX MX2007010366A patent/MX2007010366A/en active IP Right Grant
- 2006-02-27 AT AT06707301T patent/ATE438746T1/en active
-
2007
- 2007-09-04 ZA ZA200707586A patent/ZA200707586B/en unknown
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102019401A (en) * | 2010-12-30 | 2011-04-20 | 哈尔滨工业大学 | Cast forming method of small titanium alloy or titanium-aluminum alloy complicated casting |
| CN102019401B (en) * | 2010-12-30 | 2012-05-23 | 哈尔滨工业大学 | Cast forming method of small titanium alloy or titanium-aluminum alloy complicated casting |
| CN102978554A (en) * | 2012-11-13 | 2013-03-20 | 安徽春辉仪表线缆集团有限公司 | Titanium alloy valve rod preparation method of plug valve |
| CN104550949A (en) * | 2013-10-24 | 2015-04-29 | 中国科学院金属研究所 | Method for rapidly forming Ti-6Al-4V three-dimensional metal parts by electron beams |
| CN105817608A (en) * | 2016-04-29 | 2016-08-03 | 南京宝泰特种材料股份有限公司 | Titanium alloy smelting and casting method |
| CN105817608B (en) * | 2016-04-29 | 2019-01-18 | 南京宝泰特种材料股份有限公司 | A kind of titanium alloy smelting casting method |
| CN111850346A (en) * | 2020-08-06 | 2020-10-30 | 西部金属材料股份有限公司 | High-strength titanium alloy without solid solution aging treatment and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1851350A1 (en) | 2007-11-07 |
| WO2006089790A1 (en) | 2006-08-31 |
| DE502006004443D1 (en) | 2009-09-17 |
| CN100594248C (en) | 2010-03-17 |
| ES2328955T3 (en) | 2009-11-19 |
| ATE438746T1 (en) | 2009-08-15 |
| DK1851350T3 (en) | 2009-10-19 |
| TWI395821B (en) | 2013-05-11 |
| EP1851350B1 (en) | 2009-08-05 |
| AU2006218029B2 (en) | 2011-07-21 |
| CA2597248C (en) | 2016-04-19 |
| PL1851350T3 (en) | 2010-01-29 |
| RU2402626C2 (en) | 2010-10-27 |
| TW200643182A (en) | 2006-12-16 |
| JP5155668B2 (en) | 2013-03-06 |
| AU2006218029A1 (en) | 2006-08-31 |
| RU2007135062A (en) | 2009-03-27 |
| EP1696043A1 (en) | 2006-08-30 |
| KR101341298B1 (en) | 2013-12-12 |
| CA2597248A1 (en) | 2006-08-31 |
| BRPI0607832A2 (en) | 2009-06-13 |
| JP2008531288A (en) | 2008-08-14 |
| ZA200707586B (en) | 2008-10-29 |
| AR052391A1 (en) | 2007-03-14 |
| MX2007010366A (en) | 2007-10-17 |
| KR20070105379A (en) | 2007-10-30 |
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