SG174312A1 - Lead-free brass alloy - Google Patents
Lead-free brass alloy Download PDFInfo
- Publication number
- SG174312A1 SG174312A1 SG2011065042A SG2011065042A SG174312A1 SG 174312 A1 SG174312 A1 SG 174312A1 SG 2011065042 A SG2011065042 A SG 2011065042A SG 2011065042 A SG2011065042 A SG 2011065042A SG 174312 A1 SG174312 A1 SG 174312A1
- Authority
- SG
- Singapore
- Prior art keywords
- alloy
- lead
- alloys
- tellurium
- copper
- Prior art date
Links
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 80
- 239000000956 alloy Substances 0.000 title claims abstract description 80
- 229910001369 Brass Inorganic materials 0.000 title claims abstract description 17
- 239000010951 brass Substances 0.000 title claims abstract description 17
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 20
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical group [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 16
- 229910052802 copper Inorganic materials 0.000 claims description 16
- 239000010949 copper Substances 0.000 claims description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
- 229910052725 zinc Inorganic materials 0.000 claims description 13
- 239000011701 zinc Substances 0.000 claims description 13
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 4
- UQBKQFMSHMLFJK-UHFFFAOYSA-N copper;zinc Chemical compound [Cu+2].[Zn+2] UQBKQFMSHMLFJK-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000009428 plumbing Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001340 Leaded brass Inorganic materials 0.000 description 1
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000010622 cold drawing Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/04—Alloys based on copper with zinc as the next major constituent
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Conductive Materials (AREA)
- Contacts (AREA)
- Adornments (AREA)
Abstract
The invention relates to brass alloys that are substantially lead-free. In the alloys of the invention, lead is replaced with tellurium resulting in alloys that exhibit excellent machinability and conductivity.
Description
LEAD-FREE BRASS ALLOY
This application claims priority to U.S. Utility Patent Application Serial No. 12/400,283, filed March 09, 2009 which is incorporated by reference herein in its entirety.
[0001] The present invention relates to brass compositions with extremely low to no lead content. The compositions exhibit good machinability and strength similar to that of conventional leaded brass alloy free machining brass.
[0002] It has been common practice to add up to 4.5% lead to brass compositions to improve the machinability of the resulting product. Lead, however, is a toxic substance and its use in the production of alloys is surrounded by legislation and expensive control procedures.
For example, California adopted legislation which limits the amount of lead in plumbing fixtures to .25% or less beginning in 2010.
[0003] Furthermore, the lead phase in copper lead alloys can be affected by corrosive attacks with hot organic or mineral oil. For example, when temperature of such an alloy rises, it has been known that the oil can break down to form peroxides and organic gases which effect a degree of leaching on the lead phase within the alloy. If this leaching progresses to any appreciable extent, the component, if it is a bearing or structural component, may eventually malfunction or fail.
[0004] There is, therefore, considerable advantage in reducing, or if possible, eliminating the contents of lead within powder metallurgy compositions. Various proposals have been put forward for doing this. The considerable proportions of lead incorporated in powder metallurgy materials in the past has resulted in ease of machinability and durability of the resulting product component. Replacement of part of the lead by bismuth has been proposed in
International Application published under No. WQ091/14012. This results in successful replacement of part of the lead without significant reduction in the machinability. It is, however, accompanied by some reduction of transverse strength of the material. For many purposes this reduction in transverse strength is not a significant problem.
[0005] Another approach has been described in U.S. Patent 5,445,665. In this product 0.1 to 1.5% graphite is added to the alloy allowing for reduction of lead to 2% of the alloy or less.
[0006] While the alloys described above yield substantially lead-free alloys, they do not possess the same machinability as the lead containing alloys. This results in the need for substantial retooling of the equipment used to produce end product, such as plumbing equipment and the like. In addition, the scrap produced during the manufacturing of the lead products often cannot be readily recycled by the end product manufacturer. Recycling typically can only be done by the manufacturer of the alloys. The cost of shipping the scrap back to the initial foundry increases the overall product cost of the end product.
[0007] Thus, there remains a need for a lead-free brass alloy which exhibits machinability similar to that of lead containing products and that can be recycled by the customer.
[0008] The present invention comprises a brass alloy containing from about 0.20% to 1.5% tellurium as a substitute for lead, typically added to the brass composition. In one series of embodiments the tellurium ranges from about 0.4% to about 1.0%. The resulting alloy typically has a lead content of from less than about 0.025% to less than about 0.001% which is considered “lead-free.”
[0009] Brass alloys of the invention typically have a copper content of from about 98% to about 57%, a zinc content of from about 43% to about 2%, a tellurium content of from about 1.0% to about 0.02%, a lead content of from about 0.025% to about 0.001%, and a maximum phosphorous content of about 0.05%.
[0010] The resulting alloys exhibit excellent machinability and conductivity.
Depending on the composition of the alloy, the tensile strength will vary between 240 MPa and 530 MPa and yield strength will vary from about 200 to about 450 MPa. Conductivity will range from about 28% to about 49% IACS. The machinability of the novel alloys of the invention is similar to that for lead containing compositions. This eliminates or reduces the amount of retooling needed to use the novel alloys to produce finished products such as plumbing fixtures.
[0011] The composition of the novel alloys also allows the end product manufacturers to recycle the scrap from the manufacturing process itself. This eliminates the need to return the scrap to the alloy manufacturer for recycling. Yet another key feature of the present invention is that the alloys containing less than about 15% zinc exhibit excellent dezincification resistance.
[0012] The foregoing has outlined rather broadly the features and technical advantages of the present invention in order that the detailed description of the invention that follows may be better understood. Additional features and advantages of the invention will be described hereinafter which form the subject of the claims of the invention. It should be appreciated by those skilled in the art that the conception and specific embodiment disclosed may be readily utilized as a basis for modifying or designing other structures for carrying out the same purposes of the present invention. It should also be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the invention as set forth in the appended claims. The novel features which are believed to be characteristic of the invention, both as to its organization and method of operation, together with further objects and advantages will be better understood from the following description when considered in connection with the accompanying figures. It is to be expressly understood, however, that each of the figures is provided for the purpose of illustration and description only and is not intended as a definition of the limits of the present invention.
[0013] Figure 1 is a photomicrograph of the alloy used in Sample C1 after draw.
[0014] Figure 2 is a photomicrograph of the alloy used in Sample C2 after draw.
[0015] Figure 3 is a photomicrograph of the alloy used in Sample C3 after draw.
[0016] The brass alloys of the present invention are prepared by first melting copper at a temperature of about 1050°C. Zinc and tellurium are then added to the molten copper. Brass alloy is then cast into billets utilizing horizontal or vertical casting methods.
[0017] The copper used to make the alloys is typically copper cathode or high grade uncontaminated and pure copper scrap comprising 99.95% minimum copper and to .05% impurities. Lead is a typical impurity, comprising less than 0.025% of the copper used. In the formation of the alloys of the invention, copper comprises from about 57.00 to about 98.00% of the alloy.
[0018] Zinc is the next major component comprising from about 2.00% to about 43.00% of the alloy.
[0019] Tellurium is used as a replacement for lead. Like lead, tellurium is added to improve machinability of the alloy without the negative contribution of lead. Tellurium is added in an amount ranging from about .20% to about 1.5% of the alloy. In one series of embodiments, the tellurium ranges from about 0.4 to about 1.0%. In one embodiment, tellurium comprises about .5% of the alloy. The amount of tellurium used will depend, in part, on the amount of copper used in the alloy, as copper levels increase the amount of tellurium used with decrease.
Like lead, the addition of tellurium to the alloy creates discontinuities in the copper and zinc phases of the alloy like those shown in Figs 1-3. The good dispersion of these discontinuities leads to the improved machinability of the alloys.
[0020] One advantage of the present invention is that the alloys exhibit machinability similar to that of lead containing alloys while using significantly lower amounts of tellurium.
[0021] Other materials which may be added to the brass alloys include arsenic, nickel, manganese, silicon, and phosphorous. When phosphorous is used, the amount present will typically be less than 0.05% of the alloy.
[0022] The resulting alloys will generally exhibit excellent machinability and conductivity as indicated by Ultimate Tensile Strength (UTS) ranging from about 240 to about 530 MPa and a yield strength of from about 200 MPa to about 450 MPa as determined using
ASTM method B140. The actual Tensile strength and Yield strength will depend, in part, on the actual composition of the alloy. Conductivity of the alloys will range from about 28 to about 45% IACS.
[0023] A series of brass alloys were prepared where the added lead (typically about 2%) was replaced with approximately 0.5% tellurium. The composition of each alloy is shown in Table 1.
EC CE a BC 0 Je | wo [sw [os oon
EEE RC RE
Ton [ow eae [wm [oo on 0 oa [on [me [an ow
[0024] The billets were then changed into an extrusion press at a temperature ranging from about 780°C to about 860°C. The billets were then hot extruded through a variety of dies and at different pressures to produce numerous sizes. Each shot was lubricated prior to extrusion and the extrusion dies were preheated. The results are shown in Table 2.
C3a 22.23mm AF 830°C 312MPa 21.5m
Hex
C3b 22.23mm AF 837°C 324MPa 21.5m
Hex
D3a 22.23mm AF 648°C 235MPa 21.5m
Hex
[0025] The bars were then passed through a bath of sulfuric pickling acid and then cold drawn so as to induce the correct mechanical properties and grain size requirements. Also this process ensures that the correct size tolerances are met. The cold drawing operation was accomplished effortlessly. The products were then tested for tensile strength, hardness, conductivity, and machinability. The results are shown in Table 3.
TABLE 3
Sample Reduction | Ultimate Tensile | Yield Strength | ELONGATION | HARDNESS in Area Strength (MPa) (MPa) (Rb)
[0026] Conductivity tests were then conducted on various samples. Conductivity diminishes as the ratio of zinc content increases. The results ranged from at least about 28% to about 49% maximum.
[0027] Photomicrographs of Samples C1, C2 and C3 were taken after draw and are shown in FIGS 1-3. The micro structure in the alloys were uniform indicating good dispersion of the tellurium throughout the alloy.
[0028] Although the present invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims. Moreover, the scope of the present application is not intended to be limited to the particular embodiments of the process, machine, manufacture, composition of matter, means, methods and steps described in the specification. As one of ordinary skill in the art will readily appreciate from the disclosure of the present invention, processes, machines, manufacture, compositions of matter, means, methods, or steps, presently existing or later to be developed that perform substantially the same function or achieve substantially the same result as the corresponding embodiments described herein may be utilized according to the present invention.
Accordingly, the appended claims are intended to include within their scope such processes, machines, manufacture, compositions of matter, means, methods, or steps.
Claims (19)
1. A brass alloy comprising: Copper; Zinc; Tellurium; and Lead Wherein lead comprises less than 0.25% of the alloy and the tellurium comprises from about 0.025% to about 1% of the alloy.
2. The alloy of claim 1 wherein the copper comprises from about 57% to about 98% of the alloy.
3. The alloy of claim 1 wherein the zinc comprises from about 2.0% to about 43% of the alloy.
4. The alloy of claim 1 further comprising less than about 0.02% phosphorous.
5. A brass alloy comprising: about 57% to about 98% copper; about 2% to about 43% zinc; and about 0.025% to about 1.0% tellurium.
6. The alloy of claim 5 further comprising less than about 0.025% lead.
7. The alloy of claim 1 having a tensile strength of from about 240MPa to about 530MPa.
8. The alloy of claim 1 having a yield strength of from about 200MPa to about 450MPa.
9. The alloy of claim 1 having a conductivity of from about 28% to about 49% IACS.
10. The alloy of claim 1 wherein the zinc comprises about 5% of the alloy.
11. The alloy of claim 1 wherein the zinc comprises about 10% of the alloy.
12. The alloy of claim 1 wherein the zinc comprises about 15% of the alloy.
13. The alloy of claim 1 when the zinc comprises about 40% of the alloy.
14. A brass alloy comprising: from about 57% to about 98% copper; from about 43 to about 2% zinc; from about 0.025 % to about 1.0% tellurium.
15. The alloy of claim 14 having a lead content of less than about
0.5%.
16. The alloy of claim 14 having a lead content of less than about
0.01%.
17. The alloy of claim 14 having a tensile strength of from about 240MPa to about 530MPa.
18. The alloy of claim 14 having a yield strength of from about 200MPa to about 450MPa.
19. The alloy of claim 14 having a conductivity of from about 28% to about 49% IACS.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12/400,283 US20100226815A1 (en) | 2009-03-09 | 2009-03-09 | Lead-Free Brass Alloy |
| PCT/US2009/053505 WO2010104527A1 (en) | 2009-03-09 | 2009-08-12 | Lead-free brass alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SG174312A1 true SG174312A1 (en) | 2011-10-28 |
Family
ID=42678418
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SG2011065042A SG174312A1 (en) | 2009-03-09 | 2009-08-12 | Lead-free brass alloy |
Country Status (17)
| Country | Link |
|---|---|
| US (3) | US20100226815A1 (en) |
| EP (1) | EP2406406B1 (en) |
| JP (1) | JP2012519781A (en) |
| KR (1) | KR20110131272A (en) |
| CN (1) | CN102414337A (en) |
| AU (1) | AU2009341842A1 (en) |
| BR (1) | BRPI0924388B1 (en) |
| CA (1) | CA2754813A1 (en) |
| CO (1) | CO6450681A2 (en) |
| ES (1) | ES2655893T3 (en) |
| IL (1) | IL215077A0 (en) |
| MX (1) | MX2011009526A (en) |
| PL (1) | PL2406406T3 (en) |
| RU (1) | RU2011140852A (en) |
| SG (1) | SG174312A1 (en) |
| WO (1) | WO2010104527A1 (en) |
| ZA (1) | ZA201106652B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266900A (en) * | 2018-12-07 | 2019-01-25 | 宁波艾维洁具有限公司 | A kind of Anti-dezincificationyellow yellow brass alloy of lead-free corrosion resistant and preparation method thereof |
| US11427891B2 (en) | 2019-07-24 | 2022-08-30 | Nibco Inc. | Low silicon copper alloy piping components and articles |
Family Cites Families (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2027807A (en) * | 1932-05-13 | 1936-01-14 | Chase Companies Inc | Copper base alloy |
| US2102388A (en) * | 1933-09-21 | 1937-12-14 | American Brass Co | Copper-sulphur alloy |
| JPS6274037A (en) * | 1985-09-26 | 1987-04-04 | Furukawa Electric Co Ltd:The | High strength copper alloy having high electric conductivity |
| JPH03170646A (en) * | 1989-11-28 | 1991-07-24 | Nippon Mining Co Ltd | Manufacture of copper alloy having fine crystalline grains as well as low strength |
| JPH03193849A (en) * | 1989-12-22 | 1991-08-23 | Nippon Mining Co Ltd | Copper alloy having fine crystalline grain and low strength and its production |
| CA2077654A1 (en) | 1990-03-06 | 1991-09-07 | Paul E. Matthews | Powder metallurgy compositions |
| JPH04128332A (en) * | 1990-09-18 | 1992-04-28 | Sumitomo Metal Mining Co Ltd | Te-added brass excellent in corrosion resistance |
| GB9101828D0 (en) | 1991-01-29 | 1991-03-13 | Us Bronze Powders Inc | Improvements in and relating to brass compositions |
| US5137685B1 (en) * | 1991-03-01 | 1995-09-26 | Olin Corp | Machinable copper alloys having reduced lead content |
| JP3418301B2 (en) * | 1997-01-09 | 2003-06-23 | 古河電気工業株式会社 | Copper alloy for electrical and electronic equipment with excellent punching workability |
| US6413330B1 (en) * | 1998-10-12 | 2002-07-02 | Sambo Copper Alloy Co., Ltd. | Lead-free free-cutting copper alloys |
| US6471792B1 (en) * | 1998-11-16 | 2002-10-29 | Olin Corporation | Stress relaxation resistant brass |
| JP4729680B2 (en) * | 2000-12-18 | 2011-07-20 | Ｄｏｗａメタルテック株式会社 | Copper-based alloy with excellent press punchability |
| CA2559103A1 (en) * | 2004-03-12 | 2005-09-22 | Sumitomo Metal Industries, Ltd. | Copper alloy and method for production thereof |
| CN1563449A (en) * | 2004-04-07 | 2005-01-12 | 四川鑫炬矿业资源开发股份有限公司 | Forged in good quality, environmental protective alloy material of tellurium brass in high plasticity |
| DK1777305T3 (en) * | 2004-08-10 | 2011-01-03 | Mitsubishi Shindo Kk | Copper base alloy casting with refined crystal grains |
| EP1812612B1 (en) * | 2004-10-11 | 2010-05-05 | Diehl Metall Stiftung & Co. KG | Copper/zinc/silicon alloy, use and production thereof |
| JP5116976B2 (en) * | 2006-02-10 | 2013-01-09 | 三菱伸銅株式会社 | Raw brass alloy for semi-fusion gold casting |
-
2009
- 2009-03-09 US US12/400,283 patent/US20100226815A1/en not_active Abandoned
- 2009-08-12 ES ES09841636.5T patent/ES2655893T3/en active Active
- 2009-08-12 SG SG2011065042A patent/SG174312A1/en unknown
- 2009-08-12 RU RU2011140852/02A patent/RU2011140852A/en unknown
- 2009-08-12 MX MX2011009526A patent/MX2011009526A/en not_active Application Discontinuation
- 2009-08-12 CA CA2754813A patent/CA2754813A1/en not_active Abandoned
- 2009-08-12 CN CN2009801588751A patent/CN102414337A/en active Pending
- 2009-08-12 JP JP2011554028A patent/JP2012519781A/en active Pending
- 2009-08-12 AU AU2009341842A patent/AU2009341842A1/en not_active Abandoned
- 2009-08-12 EP EP09841636.5A patent/EP2406406B1/en active Active
- 2009-08-12 BR BRPI0924388-7A patent/BRPI0924388B1/en active IP Right Grant
- 2009-08-12 WO PCT/US2009/053505 patent/WO2010104527A1/en active Application Filing
- 2009-08-12 KR KR1020117023686A patent/KR20110131272A/en not_active Application Discontinuation
- 2009-08-12 PL PL09841636T patent/PL2406406T3/en unknown
-
2011
- 2011-09-11 IL IL215077A patent/IL215077A0/en unknown
- 2011-09-12 ZA ZA2011/06652A patent/ZA201106652B/en unknown
- 2011-10-06 CO CO11131873A patent/CO6450681A2/en not_active Application Discontinuation
-
2016
- 2016-10-10 US US15/289,580 patent/US20170145544A1/en not_active Abandoned
-
2023
- 2023-01-02 US US18/149,139 patent/US20230151457A1/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| EP2406406A4 (en) | 2015-09-02 |
| WO2010104527A1 (en) | 2010-09-16 |
| AU2009341842A1 (en) | 2011-10-06 |
| JP2012519781A (en) | 2012-08-30 |
| EP2406406B1 (en) | 2017-11-22 |
| PL2406406T3 (en) | 2018-05-30 |
| CA2754813A1 (en) | 2010-09-16 |
| KR20110131272A (en) | 2011-12-06 |
| US20230151457A1 (en) | 2023-05-18 |
| BRPI0924388A2 (en) | 2017-06-06 |
| ZA201106652B (en) | 2012-05-30 |
| BRPI0924388B1 (en) | 2021-05-04 |
| US20170145544A1 (en) | 2017-05-25 |
| IL215077A0 (en) | 2011-12-01 |
| US20100226815A1 (en) | 2010-09-09 |
| RU2011140852A (en) | 2013-04-20 |
| CN102414337A (en) | 2012-04-11 |
| CO6450681A2 (en) | 2012-05-31 |
| MX2011009526A (en) | 2011-12-16 |
| ES2655893T3 (en) | 2018-02-22 |
| EP2406406A1 (en) | 2012-01-18 |
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