CN105050751A - Methods for repairing ceramic cores - Google Patents
Methods for repairing ceramic cores Download PDFInfo
- Publication number
- CN105050751A CN105050751A CN201480011403.4A CN201480011403A CN105050751A CN 105050751 A CN105050751 A CN 105050751A CN 201480011403 A CN201480011403 A CN 201480011403A CN 105050751 A CN105050751 A CN 105050751A
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- Prior art keywords
- mixture
- ceramic core
- core
- diluent
- reparation
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/10—Cores; Manufacture or installation of cores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
- B22C1/16—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents
- B22C1/20—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents
- B22C1/205—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents of organic silicon or metal compounds, other organometallic compounds
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Molds, Cores, And Manufacturing Methods Thereof (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Mold Materials And Core Materials (AREA)
Abstract
A method is provided for repairing defects in a ceramic core adapted for use in a casting process. The ceramic core is formed from a slurry comprising at least one refractory powder material suspended in a liquid vehicle. The method includes forming a repair mixture comprising a liquid diluent and the at least one refractory powder material suspended in the liquid vehicle of the slurry. The repair mixture is applied to a region of the ceramic core that includes at least one defect and then the ceramic core is fired to burn off the liquid vehicle in the repair mixture and form a ceramic composition that closes the defect.
Description
Technical background
The present invention generally relates to casting method and material.More particularly, the present invention relates to core (cores) and the core with defect (such as slight crack) for repairing formation.
Be assembly by multiple casting technique by metal alloy compositions casting mold, significant example is model casting (dewax) method.The wax of the assembly of expectation or plastic pattern or pattern immerse and comprise in the slurry of adhesive and refractory particulate material, to form pulp layer on pattern by model casting General Requirements.Conventional material for adhesive is silica containing material, such as colloidal silica.The general surface paint coating of refractory particulate material being applied to pulp layer, dry slurry/paint coating after this.Repeatedly can repeat abovementioned steps, to form the shell mould with suitable thickness around wax pattern.Such as by heating, wax pattern can be eliminated from shell mould subsequently, fire mould after this, to sinter refractory particulate material and to obtain suitable intensity.
In order to produce hollow component, such as, there is turbo blade and the impeller of complicated cooling air channel, must one or more core is placed in shell mould, to limit cooling duct and any internal features needed for other.Generally be used in carry out injection moulding or transfer molding in punch die or mold plasticized ceramic mixture to manufacture core, and make it harden by firing or toasting subsequently.Typical ceramic composition contains silica and/or aluminium oxide.Such as, the people such as McNutty are at United States Patent (USP) 7,287,573 and 7,732,526, in disclose the ceramic core formed by the slurry comprising ceramic powders, described ceramic powder comprises such as: the materials such as aluminium oxide, aloxite (AI2O3), fused silica, magnesia, zirconia, spinelle, mullite, glass glaze, tungsten carbide, carborundum, boron nitride, silicon nitride and their mixture, described material is suspended in comprise to be had in the silicone monomer of thiazolinyl and hydrogen functional group and/or the silicone fluid of oligomer.Metallic catalyst is added suspension, to make silicone monomer and/or oligomer be cross-linked, to produce firm ceramic particle core in based on the polymer substrate of silicone.McNutty discloses and fires core, substantially to decompose matrix, thus produces silica charcoal.
Subsequently one or more core of firing is placed in pattern die cavity, in chamber, introduces wax, plasticity or other suitable low melt material, to form wax pattern.The pattern with interior core can be used subsequently to form above-mentioned shell mould.Once shell mould completes and optionally removes pattern to retain shell mould and core, shell mould can be full of motlten metal, make described motlten metal solidify subsequently, to form the assembly of expectation.Remove mould and core subsequently, to retain the casting component with one or more inner passage, described inner passage is original core whereabouts.
When such as above-mentioned formation core, the defect of such as slight crack and space can be there is in core material.The defective core of tool can not be used for cast technique usually, because core may rupture during casting, causes casting defect.Due to the difficulty (hollow mold core is all the more so) of repairing type cored structure integrality, general defective core will be dropped instead of repair.The example being intended to repairing type core in prior art is reported in the United States Patent (USP) 4,804 of the people such as Ferguson, in 562, wherein by following reparation core: the thermoplastic adhesives in (a) softening core; B (), while adhesive is softening, uses loose ceramic particle to defect, described particle has and forms similar composition with core entirety; C () makes adhesive reharden; (d) heat core, volatilize to make adhesive and ceramic particle is sintered each other.
Can understand from above, wish the method obtaining can be used for repairing defective core, to produce the core with the structural integrity being suitable for casting process.
Summary of the invention
The invention provides the method for the ceramic core being suitable for repairing the defect with such as one or more slight crack and/or space, present the sufficient structural intergrity being applicable to casting process to make core.
A first aspect of the present invention is provided for repairing the method for the defect be applicable in the ceramic core of casting process.Ceramic core is formed by the slurry comprising the refractory powder powder material that at least one suspends in a liquid carrier.Described method comprises being formed repairs mixture, the refractory powder powder material that at least one that described mixture comprises liquid diluent and described slurry suspends in a liquid carrier.Reparation mixture is applied to the ceramic core region comprising at least one defect, and firing ceramics core subsequently, repair the liquid-carrier in mixture with burning-off and form the ceramic composition of closure defect.
A second aspect of the present invention is provided for repairing the method for the defect be applicable in the silica containing ceramic core of casting process.Described silica containing ceramic core is formed by the slurry comprising the fire-resistant powder of at least one and silicone adhesive.Described method comprises being formed repairs mixture, and described reparation mixture comprises at least one refractory powder powder material and the silicone adhesive of siloxanes diluent and described slurry.Described reparation mixture is applied to the silica containing ceramic core region comprising at least one defect, and fire silica containing ceramic core subsequently, to repair silicone adhesive in mixture and siloxanes diluent described in burning-off, and form the silica containing ceramic composition of filling defect.
Technique effect of the present invention is for can repair defective ceramic core, otherwise described defective ceramic core will not be suitable for casting process.Especially, believe that the core through repairing has sufficient structural intergrity, to stand casting cycle by being used on composition and repairing defective ceramic core for the formation of the reparation mixture that the slurry of ceramic core is similar.In addition, believe that use adhesive/diluent dilutes described reparation mixture and can promote to make described reparation mixture adhere to ceramic core.
Other aspects and advantages of the present invention can be understood better by following detailed description.
Accompanying drawing explanation
Fig. 1 represents the hollow ceramic core being suitable for repairing according to the method for one aspect of the present invention.
Fig. 2 represents the cross section of the wall of the hollow ceramic core of Fig. 1.
Detailed description of the invention
Generally speaking, the present invention can be used for repair formed time have in the method for the core of defect (such as slight crack).Although relate to the method for the core containing silica containing material discussed below, can predict and can implement described method on the core comprising other material, therefore these are also within the scope of the invention.
Fig. 1 represents the ceramic core 10 together used with die assembly (not shown) according to an aspect of of the present present invention, for model casting hollow component (not shown), such as the assembly of gas-turbine unit, include but not limited to: turbo blade, nozzle or other screw assembly.Core 10 is formed by the slurry comprising the refractory material that at least one suspends in a liquid carrier.Suitable refractory material is including but not limited to silica, zirconia, aluminium oxide, mullite and/or similar material.Such as, the described slurry catalyst that can comprise the fire-resistant powder of silica, Zircon refractory powder, silicone adhesive and silicone adhesive can be made crosslinked.Preferred example is platinum group metal (PGM) catalyst causing the silicone monomer of silicone adhesive and/or oligomer to be cross-linked, if the people such as McNutty are at United States Patent (USP) 7,287,573 and 7,732, report in 526, be bonded to herein about the content of paste compound and using method in described patent.According to a preferred aspect of the present invention, ceramic core 10 comprises at least 5 % by weight silica, and the silica of more preferably from about 25-about 95 % by weight, and the zircon of aequum and other optional refractory material.Such as, but can predict, ceramic core 10 mainly can comprise other refractory material in addition to silica, maximum zircon of 95 % by weight, for special application.Other example being suitable as the composition of core 10 is described in the United States Patent (USP) 7,287,573 and 7,732 of the people such as McNutty, in 526.The method that can form core 10 is well known in the art, therefore will not do further discussion in this article.
As shown in Figure 1, opening 16 left when core 10 comprises the inner chamber 14 of wall 12 restriction and forms described inner chamber 14.In order to make core 10 can be used for full form casting process, preferably close and sealed open 16.In addition, before core 10 is used for casting process, need to repair any defect in core 10, such as one or more slight crack, to promote the structural intergrity of core 10 and to make core 10 stand casting cycle.
According to the preferred aspect of the present invention, repairing mixture 20 to repair opening 16 in core 10 and slight crack by using core 10, in Fig. 2, representing the slight crack 18 of the wall 22 of the core 10 of blank map 1.Repair mixture 20 and preferably comprise the material similar with the initial slurry for the formation of core 10.Specifically, the refractory material that mixture 20 suspends in a liquid carrier containing at least one is repaired, in preferred embodiments, repair mixture 20 to comprise and be above-mentionedly disclosed in United States Patent (USP) 7,287,573 and 7,732, silica in 526 and Zircon refractory dusty material and silicone adhesive, and optional be disclosed in United States Patent (USP) 7,287,573 and 7,732, the catalyst in 526.In general, slurry is not adhere to well on silica containing core usually.But, research of the present invention shows, by using a certain amount of slurry for the preparation of core 10 of suitable liquid diluting dilution agent, can make that the reparation mixture 20 pairs of cores 10 being applied to core 10 are had suitable tack, to promote that repairing mixture 20 is attached to core 10.Diluent can be the adhesive identical with preparing the adhesive that uses in the slurry of core 10 of additional quantity, and in this case, preferred described diluent is cross-linked by optional catalyst.Preferably, described diluent comprises the siloxanes (people such as such as McNutty at United States Patent (USP) 7,287,573 and 7, those of report in 732,526) that at least one is considered to promote improve bonding strength.It is the t etram-ethyltetravinylcyclotetrasiloxane (D4Vi) of about 0.5-about 2.0 and the mixture of methylhydrogenpolysi,oxane that specially suitable diluent comprises mol ratio.
In order to promote the structural intergrity of repairing, reparation mixture 20 should be diluted to has not higher than the solid content (comprising refractory powder powder material) of about 70 volume %, all the other are adhesive, diluent and other fluid carrier components any, to promote to repair the ability that mixture 20 infiltrates slight crack 18 completely.Preferably, repair mixture 20 and comprise the refractory powder powder material of about 30-about 50 volume % by volume, altogether the adhesive of about 50-about 70 volume % and diluent, and the catalyst of optional about 100ppm at most.As above-mentioned, adhesive can be identical with diluent, such as, be siloxanes.In this case, just the amount of adhesive and diluent is simply added and, to reflect the total amount (or other adhesive/diluent) of the siloxanes for repairing mixture 20.
Use by one or many and repair mixture 20 to fill opening 16 and slight crack 18 (and/or other defect any).In certain embodiments of the invention, when initial, reparation mixture 20 one or many more diluted can be applied to core 10, to promote to repair the ability that mixture 20 infiltrates slight crack 18 and other defect completely.Believe and use the diluent of additional quantity to reduce the viscosity of repairing mixture 20, thus promote the infiltration to sending out hair check.This kind of reparation mixture 20 more diluted can contain the refractory powder powder material of about 20-about 40 volume % by volume, the adhesive of about 60-about 80 volume % and diluent, and the catalyst of optional about 100ppm at most.
Reparation mixture 20 can be applied to any area to be repaired of core 10, comprise surface and chamber 14, use by any known method in this area, such as but not limited to: brush or make by hand or electronic injector to inject.Before using reparation mixture 20, can first use diluent region surface to be soaked, be repaired mixture 20 with promoted type wicking surface and soak.If core 10 size is relatively little, then can use not containing the reparation mixture 20 of catalyst.Believe that catalyst can change the viscosity of repairing mixture 20 during using reparation mixture 20, and before finally completing described reparation, repairing mixture will become solid.In addition, the reparation mixture 20 containing catalyst may have the shorter life-span, therefore may be difficult to process and storage.Believe if core 10 is less, then repairing mixture 20 can fill when not needing catalyst and remain within small-sized defect.If the size of core 10 is relatively large, then repair mixture 20 preferably containing catalyst.Believe that catalyst repairs the crosslinked of mixture 20 by promoting, thus improve the persistence of repairing.Repeatedly can use as required and repair mixture 20, to fill slight crack 18 in the surface of core 10 and other defect any.In addition, before core 10 is used for casting process, reparation mixture 20 (if core 10 is less, then not containing catalyst) or initial slurry can be injected the chamber 14 of hollow mold core 10, with all openings 16 of closed core 10.Preferably, before firing, use in the mode of thickness balance (namely relatively uniform) ensureing wall 12 and repair mixture 20.After using reparation mixture 20, restoring area can be made dry and make smooth surface.If repair mixture 20 to comprise catalyst, then once reparation mixture 20 is undesirably applied to core 10, core 10 can be solidified, be cross-linked to make adhesive and diluent.After adhesive is crosslinked, fire core 10, with burning-off adhesive and diluent, and sintering repairs the combustion-resistant solid inclusion of mixture 20.Preferably fire core 10 being greater than at the temperature of about 1000 DEG C, fully sintered to ensure the solid contents by repairing mixture 20, be bonded to one another to make fire-resistant powder particle and and be bonded to the surface of core 10.
Although adopted specific embodiments to describe the present invention, it is evident that, those skilled in the art can adopt other form.Such as, be applied to the order of core 10 and method can be different by repairing mixture 20, and can use except mention materials and methods except those.Therefore, scope of the present invention will only be limited by following claim.
Claims (20)
1., for repairing the method for the defect of the ceramic core being applicable to casting process, described ceramic core is formed by the slurry comprising the refractory powder powder material that at least one suspends in a liquid carrier, and described method comprises:
Formed and repair mixture, the refractory powder powder material that at least one that described reparation mixture comprises liquid diluent and described slurry suspends in a liquid carrier;
Described reparation mixture is applied to the region of described ceramic core, described region comprises at least one defect; With
Fire described ceramic core, to repair the described liquid-carrier in mixture described in burning-off, and form the ceramic composition closing described defect.
2. the process of claim 1 wherein that described at least one refractory powder powder material comprises the fire-resistant powder of silica and Zircon refractory powder.
3. the process of claim 1 wherein that described liquid-carrier comprises silicone adhesive.
4. the process of claim 1 wherein that described liquid diluent is siloxanes diluent.
5. the process of claim 1 wherein that described liquid diluent is the described liquid-carrier of additional quantity.
6. the process of claim 1 wherein that described reparation mixture comprises the catalyst that described liquid-carrier and described liquid diluent can be made to be cross-linked further.
7. the process of claim 1 wherein that described reparation mixture comprises the described refractory powder powder material of about 30-about 50% by volume and amounts to the described liquid-carrier of about 50-about 70% and described liquid diluent.
8. the method for claim 7, wherein said reparation mixture comprises the catalyst that described liquid-carrier and described liquid diluent can be made to be cross-linked of about 100ppm at most.
9. the method for claim 1, described method uses described liquid diluent to soak described region before being included in further and using described reparation mixture.
10. the process of claim 1 wherein that described ceramic core comprises the wall in restriction wherein at least one chamber.
The method of 11. claims 10, injects described chamber by described reparation mixture before described method is included in further and fires, to close at least one opening of the described wall of described ceramic core.
12. ceramic cores repaired by the method for claim 1.
13. for repairing the method for the defect be applicable in the silica containing ceramic core of casting process, and described silica containing ceramic core is formed by the slurry comprising at least one refractory powder powder material and silicone adhesive, and described method comprises:
Formed and repair mixture, described mixture comprises at least one refractory powder powder material and the silicone adhesive of siloxanes diluent and described slurry;
Described reparation mixture is applied to the region of described silica containing ceramic core (10), described region comprises at least one defect; With
Fire described silica containing ceramic core, to repair described silicone adhesive in mixture and described siloxanes diluent described in burning-off, and form the silica containing ceramic composition of filling described defect.
The method of 14. claims 13, wherein said reparation mixture comprises the catalyst that described silicone adhesive can be made crosslinked.
The method of 15. claims 13, wherein said siloxanes diluent has the composition identical with described silicone adhesive.
The method of 16. claims 13, wherein said at least one refractory powder powder material comprises the fire-resistant powder of silica and/or Zircon refractory powder.
The method of 17. claims 13, wherein said silica containing ceramic core comprises the wall in restriction wherein at least one chamber.
The method of 18. claims 17, injects described chamber by described reparation mixture before described method is included in further and fires, to close at least one opening of the described wall of described silica containing ceramic core.
The method of 19. claims 13, wherein said silica containing ceramic core is applicable to cast the assembly be configured in gas-turbine unit.
The method of 20. claims 13, wherein said reparation mixture comprises by volume the fire-resistant powder of described silica of about 30-about 50% altogether and described Zircon refractory powder, about 50-about silicone adhesive described in 70% and described siloxanes diluent altogether, and the catalyst that described silicone adhesive and described siloxanes diluent can be made to be cross-linked of optional about 100ppm at most.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/780763 | 2013-02-28 | ||
| US13/780,763 US20140238632A1 (en) | 2013-02-28 | 2013-02-28 | Methods for repairing ceramic cores |
| PCT/US2014/011748 WO2014133678A1 (en) | 2013-02-28 | 2014-01-16 | Methods for repairing ceramic cores |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105050751A true CN105050751A (en) | 2015-11-11 |
Family
ID=50031617
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201480011403.4A Pending CN105050751A (en) | 2013-02-28 | 2014-01-16 | Methods for repairing ceramic cores |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US20140238632A1 (en) |
| EP (1) | EP2961546A1 (en) |
| JP (1) | JP2016514054A (en) |
| CN (1) | CN105050751A (en) |
| BR (1) | BR112015019088A2 (en) |
| CA (1) | CA2902008A1 (en) |
| WO (1) | WO2014133678A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107716864A (en) * | 2017-09-18 | 2018-02-23 | 东方电气集团东方汽轮机有限公司 | A kind of method for repairing and mending of silica sol ceramic mold shell shake line |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160144423A1 (en) * | 2014-11-21 | 2016-05-26 | General Electric Company | Casting cores and methods for making |
| US9950358B2 (en) * | 2015-11-19 | 2018-04-24 | General Electric Company | Compositions for cores used in investment casting |
| KR102062107B1 (en) * | 2017-08-10 | 2020-01-03 | 서울시립대학교 산학협력단 | A Coating Material with Crack Healing and Anti-fire for Substrates and It's Coating Method |
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| US4804562A (en) * | 1987-09-21 | 1989-02-14 | United Technologies Corporation | Method for repairing ceramic casting cores |
| US20050070651A1 (en) * | 2003-09-30 | 2005-03-31 | Mcnulty Thomas | Silicone binders for investment casting |
| CN101074159A (en) * | 2007-06-27 | 2007-11-21 | 天津大学 | Synthesis of densified siloxate ceramic by liquified polysiloxane |
| CN101215155A (en) * | 2008-01-18 | 2008-07-09 | 天津大学 | Flawless silicon-containing ceramic accessories and preparing method thereof |
| CN101423410A (en) * | 2008-11-21 | 2009-05-06 | 太原高科耐火材料有限公司 | Composite combining silica thermal repairing material and preparation method thereof |
| CN101508583A (en) * | 2008-02-13 | 2009-08-19 | 赢创戈尔德施米特有限公司 | Reactive liquid ceramics bonding agent |
| CN101808958A (en) * | 2007-07-05 | 2010-08-18 | Fib环球服务股份公司 | Method of treating a chamber having refractory walls |
| CN102531648A (en) * | 2011-12-26 | 2012-07-04 | 北京航空航天大学 | Calcium oxide-based ceramic core for casting titanium alloy and manufacturing method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5798066A (en) * | 1995-07-12 | 1998-08-25 | Certech Incorporated | Method of forming hollow ceramic articles |
| US6024787A (en) * | 1998-06-05 | 2000-02-15 | Industrial Technology Research Institute | Water soluble ceramic core for use in die casting, gravity and investment casting of aluminum alloys |
| CN1785883B (en) * | 2005-12-09 | 2010-10-27 | 重庆长安汽车股份有限公司 | Film covered sand core fast drying repair paste |
-
2013
- 2013-02-28 US US13/780,763 patent/US20140238632A1/en not_active Abandoned
-
2014
- 2014-01-16 EP EP14702399.8A patent/EP2961546A1/en not_active Withdrawn
- 2014-01-16 JP JP2015560183A patent/JP2016514054A/en not_active Withdrawn
- 2014-01-16 CN CN201480011403.4A patent/CN105050751A/en active Pending
- 2014-01-16 CA CA2902008A patent/CA2902008A1/en not_active Abandoned
- 2014-01-16 WO PCT/US2014/011748 patent/WO2014133678A1/en active Application Filing
- 2014-01-16 BR BR112015019088A patent/BR112015019088A2/en not_active IP Right Cessation
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4804562A (en) * | 1987-09-21 | 1989-02-14 | United Technologies Corporation | Method for repairing ceramic casting cores |
| US20050070651A1 (en) * | 2003-09-30 | 2005-03-31 | Mcnulty Thomas | Silicone binders for investment casting |
| US20080027163A1 (en) * | 2003-09-30 | 2008-01-31 | General Electric Company | Silicone binders for investment casting |
| CN101074159A (en) * | 2007-06-27 | 2007-11-21 | 天津大学 | Synthesis of densified siloxate ceramic by liquified polysiloxane |
| CN101808958A (en) * | 2007-07-05 | 2010-08-18 | Fib环球服务股份公司 | Method of treating a chamber having refractory walls |
| CN101215155A (en) * | 2008-01-18 | 2008-07-09 | 天津大学 | Flawless silicon-containing ceramic accessories and preparing method thereof |
| CN101508583A (en) * | 2008-02-13 | 2009-08-19 | 赢创戈尔德施米特有限公司 | Reactive liquid ceramics bonding agent |
| CN101423410A (en) * | 2008-11-21 | 2009-05-06 | 太原高科耐火材料有限公司 | Composite combining silica thermal repairing material and preparation method thereof |
| CN102531648A (en) * | 2011-12-26 | 2012-07-04 | 北京航空航天大学 | Calcium oxide-based ceramic core for casting titanium alloy and manufacturing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107716864A (en) * | 2017-09-18 | 2018-02-23 | 东方电气集团东方汽轮机有限公司 | A kind of method for repairing and mending of silica sol ceramic mold shell shake line |
Also Published As
| Publication number | Publication date |
|---|---|
| CA2902008A1 (en) | 2014-09-04 |
| WO2014133678A1 (en) | 2014-09-04 |
| US20140238632A1 (en) | 2014-08-28 |
| BR112015019088A2 (en) | 2017-07-18 |
| EP2961546A1 (en) | 2016-01-06 |
| JP2016514054A (en) | 2016-05-19 |
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