CN102628133B - Magnesium-aluminum based alloy - Google Patents
Magnesium-aluminum based alloy Download PDFInfo
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- CN102628133B CN102628133B CN201210022182.3A CN201210022182A CN102628133B CN 102628133 B CN102628133 B CN 102628133B CN 201210022182 A CN201210022182 A CN 201210022182A CN 102628133 B CN102628133 B CN 102628133B
- Authority
- CN
- China
- Prior art keywords
- grain
- magnalium
- refining agent
- alloy
- magnesium
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/20—Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
Abstract
The present invention relates to magnesium-aluminum based alloys having a small grain size and to a method of their production. The alloys are particularly useful in casting applications. The alloys comprise a grain refiner, the grain refiner having the chemical formula: Mg 100-x-y-z Al x C y R z wherein R is an element selected from the group consisting of silicon, calcium, strontium or a rare earth element, x is from 10 to 60 At.%, y is from 5 to 50 At.%, and z is from 0 to 20 At.%, provided that x+y+z is less than 100 At.%.
Description
Technical field
The present invention relates to and a kind of there is magnalium of little grain-size and preparation method thereof.This alloy is particularly useful for foundry applications.
The exploitation of magnesium alloy is generally space industry and drives the performance requirement that lightweight material improves constantly.The reason that magnesium alloy is so paid attention to by planners is just that it has low density, is only 2/3rds of aluminium.This is also the major reason that magnesium alloy is widely used in casting and forged article.
In recent years, due to the further requirement to high antiseptic property, the improvement of novel magnesium alloy has obtained suitable progress.Due to the improvement in mechanical characteristics and antiseptic property, magnesium alloy is subject to more attention day by day in aerospace and other special application fields.
Background technology
The suitability of magnesium alloy often improves due to less grain-size.Little grain-size can make magnesium alloy have better mechanical property and structural uniformity usually, thus has better machining property, good heat resistanceheat resistant cutting performance and more excellent extrudability energy.Have at present many products be by extruding strand, the mode of rolling and forging produces.Therefore, the fine grain size of magnesium alloy is not only conducive to the processing characteristics improving as cast condition product in casting, also contributes to the suitability for secondary processing improving product.
Magnesium alloy can be divided into two large classes usually: containing aluminium with containing the magnesium alloy of aluminium.Alloy not containing aluminium mainly refers to containing zinc or the alloy by zirconium improvement crystal grain, such as ZE41, ZK60, WE43 and EZ33.In these alloys, grain-size can be undertaken controlling or reducing by the mode of adding zirconium.But, the special crystal grain of zirconium is improved effect and is being contained aluminum magnesium alloy such as AM50, but can not work in AM60 and AZ91, this forms stable intermetallic phase because aluminium and zirconium can be easy to occur to interact, and it is just inoperative as the agent of magnesium alloy nucleation unfortunately.Therefore, still need to develop for the suitable grain-refining agent of magnalium.
State of art
Up to now, the method for existing multiple magnalium crystal grain thinning is developed.
Crossing in thermal means, magnesium alloy is heated to more than its fusing point about 150 to 250 DEG C, maintains 5 to 15 minutes at such a temperature, is cooled to pouring temperature rapidly afterwards.Its Grain Refinement Mechanisms is considered to the heterogeneous nucleation effect by Al-Mn-Fe compound.In the process crossing thermal means, observed several essential characteristic.The first, need temperature range certain more than pouring temperature could play the effect of grain refining to greatest extent.The second, the quick cooling from temperature of superheat to pouring temperature and of short duration hold-time are also vital conditions for formation fine-grain.Due to needs high temperature, the energy consumption of this method is quite high, and is preventing from melt oxidation and checking and safeguard also having suitable cost in casting ladle etc.
Carbon inoculation technique is at present another kind of for the main of magnalium and effective crystal fining method.The committed step of the method is just carbon to be incorporated in molten magnesium metal.Its Grain Refinement Mechanisms is considered to: reacted by the carbon in compound and the aluminium in melt and form aluminium carbide (Al
4c
3) nonhomogen-ous nucleation effect.In industrial processes, be add C
7cl
6as grain-refining agent, but owing to can produce a large amount of obnoxious flavoures, this method is no longer allowed to use.In addition, inorganic carbon, such as graphite is rare, carbon and paraffin also studied as grain-refining agent.But their Grain Refinement Effect is quite limited.
In Elfinal method, iron(ic) chloride is added in melt at about 760 DEG C, and described melt keeps 30 to 60 minutes at such a temperature, thus forms Al-Mn-Fe compound gradually, and this compound is considered to have Grain Refinement Effect.But have report to point out, in order to obtain significant grain refining effect, Fe content must higher than certain dividing value.The deterioration of corrosion resistance caused by the local element effect that the problem of this method is Fe and Mn.
Described by above method has in such as following document: Lee et al.Metallurgical andMaterials Transactions, Vol.31A, 2000, pages 2805-2906.
In brief, a kind of gratifying means of the grain refining for improving as cast condition magnalium are not also had up to now.Therefore, the object of the present invention is to provide the modification method of a kind of magnalium type alloy grain refinement.
Summary of the invention
In first aspect, the invention provides a kind of magnalium containing grain-refining agent, described grain-refining agent has following chemical formula:
Mg
100-x-y-zAl
xC
yR
z
Wherein, R be selected from silicon, calcium, strontium or rare earth element form the element of cohort, x is 10 to 60At.%, y be 5 to 50At.%, z is 0 to 20At.%, and condition is that x+y+z is less than 100At.%.Preferably x is 20 to 50At.%; Further preferably y is 10 to 35At.%; And further preferably z is 1 to 20At.%.
Preferably, described rare earth element is selected from lanthanum, cerium, neodymium, samarium, europium or mishmetal.
Magnalium preferably comprises grain-refining agent and its add-on is 0.1 to 2% weight of described alloy initial weight.Described magnalium can be the alloy containing magnesium and aluminium that any one is traditional.Preferably, described magnalium is selected from Mg-Al-Zn Alloy or magnalium manganese alloy; More preferably, described alloy is selected from AM50, the cohort that AM60, AM201, AZ10, AZ31, AZ63, AZ80 and AZ91 are formed.
In second aspect, present invention also offers a kind of method preparing the magnalium with fine-grain, it comprises and being melted under protective atmosphere by the alloy containing magnesium and aluminium, and adds the grain-refining agent with following chemical formula to magnalium melt:
Mg
100-x-y-zAl
xC
yR
z
Wherein, R be selected from silicon, calcium, strontium or rare earth element form the element of cohort, x is 10 to 60At.%, y be 5 to 50At.%, z is 0 to 20At.%, and condition is that x+y+z is less than 100At.%, and allows alloy graining.Preferably, described rare earth element is selected from the cohort that lanthanum, cerium, neodymium, samarium, europium or mishmetal are formed.
Magnalium preferably includes grain-refining agent and its add-on is 0.1 to 2% weight of alloy initial weight.Described magnalium can be any traditional alloy containing magnesium and aluminium.Described magnalium is preferably selected from the cohort that Mg-Al-Zn Alloy and magnalium manganese alloy are formed, and more preferably, described alloy is selected from AM50, the cohort that AM60, AM201, AZ10, AZ31, AZ63, AZ80, AZ91, AE44, AE42, AJ53, AS41 and AS42 are formed.
Preferably, the magnalium of the fusing containing grain-refining agent is cast allowing before alloy graining.Preferably described shielding gas comprises such as rare gas element, such as helium or argon gas.More preferably, described shielding gas is argon gas and SF
6mixture.
Described grain-refining agent is prepared preferably by high energy milling.Because grain-refining agent has relatively high fusing point, high energy milling is the effective ways being prepared suitable grain fining agent by solid state reaction.
Described grain-refining agent joins in magnalium melt can adopt to be similar to and joins zirconium not containing the mode of the magnesium alloy of aluminium.Then, ready fining agent is just added in magnesium alloy fused mass and serves as nucleator.
When preparing grain-refining agent by high energy milling, should preferably consider following processing parameter:
Preferably grinding rate is 600 to 1300rpm, is more preferably 800 to 1100rpm.
In process of lapping, described shielding gas preferably should to upgrade continuously or off and on to prevent in described process of lapping magnesium and/or aluminium oxidized.If shielding gas is intermittent renewal, the update times of shielding gas described in process of lapping is preferably at least 3 times, is more preferably at least 5 times.
Preferably, in process of lapping, adopt the detrimentally affect produced to reduce iron by the mill ball of zirconium white or high-strength steel manufacture.In ball mill, the ratio of ball and powder is preferably 5: 1 to 10: 1, is more preferably 6: 1 to 8: 1.Milling time is preferably chosen as 4 to 8 hours, is more preferably 5 to 7 hours.Hold-time before process of lapping starts preferably is chosen as 1 to 4 hour, is more preferably 1 to 3 hour.
When adopting high energy milling to prepare grain-refining agent, raw materials used preferably choice of powder form.Adopt high energy milling to prepare the raw materials used particle diameter of grain-refining agent and be preferably 100 μm to 400 μm, be more preferably 250 μm to 350 μm.Purity for the preparation of the raw material of grain-refining agent is preferably 99% to 99.999%, is more preferably 99.9% to 99.99%.
Particle diameter after described grain-refining agent grinding is preferably 0.1nm to 50nm, is more preferably 0.1nm to 10nm.
Grain-refining agent according to the present invention is especially effective for cast magnesium alloy.The alloy of this sample comprises, such as gravitational casting magnalium, die casting magnalium, semi-solid casting magnalium, rheocasting magnalium and continuous casting magnalium.
Have in the method for the magnalium of fine-grain in preparation, the temperature of molten alloy be preferably 720 DEG C or on, to prevent the fractional condensation of grain-refining agent nanoparticle.Described temperature is higher, and the time realizing grain refining is shorter.But, consider that too high temperature may be ignited the material of molten state, so temperature of fusion is preferably 720 DEG C to 760 DEG C, be more preferably about 750 DEG C.
The content adding the grain-refining agent of cast magnesium alloy to is preferably 0.1% to 2% weight, is more preferably 0.5% to 1.5% weight.When the content that it adds is lower than 0.1% weight, Grain Refinement Effect may be not enough.When the content that it adds is higher than 2% weight, remaining grain-refining agent likely can affect the performance of magnesium alloy.
Described melt preferably should stir the alloy obtaining equal Entropy density deviation.Stirring velocity is preferably 150rpm to 300rpm, is more preferably 150rpm to 250rpm.Churning time is preferably 10min to 60min, is more preferably 20min to 40min.
After adding grain-refining agent, have one period of hold-time, the grain refinement process for cast magnesium alloy is favourable.The described hold-time is preferably 10min to 90min, is more preferably 30min to 60min.
To be described some embodiments of the present invention below.But be interpreted as, the present invention is not limited to the following embodiment enumerated.
Accompanying drawing explanation
Fig. 1 (a)-(c) is for being presented at the microscopic optical structure that 750 DEG C are added to the grain refining effect of the original state powder of magnesium-3wt.% aluminium alloy.What Fig. 1 (a) showed is magnesium-3wt.% aluminium alloy.The grain-refining agent Mg that what Fig. 1 (b) showed is containing 1wt.%
0.3al
0.4c
0.15ca
0.15magnesium-3wt.% aluminium alloy, and milling time is 20 hours.Churning time during melting is 30 minutes.The grain-refining agent Mg that what Fig. 1 (c) showed is containing 1wt.%
0.3al
0.4c
0.15rE
0.15magnesium-3wt.% aluminium alloy, and milling time is 20 hours.Churning time during melting is 30 minutes.
Fig. 2 is presented at the microscopic optical structure that 750 DEG C are added to the grain refining effect of the original state powder of magnesium-3wt.% aluminium alloy.What Fig. 2 (a) showed is containing 0.5wt.%Mg
0.3al
0.4c
0.15rE
0.15magnesium-3wt.% the aluminium alloy of grain-refining agent, and milling time is 20 hours.What Fig. 2 (b) showed is containing 0.8wt.%Mg
0.3al
0.4c
0.15rE
0.15magnesium-3wt.% the aluminium alloy of grain-refining agent, and milling time is 20 hours.What Fig. 2 (c) showed is containing 1wt.%Mg
0.3al
0.4c
0.15rE
0.15magnalium-3wt.% the alloy of grain-refining agent, and milling time is 20 hours.
Fig. 3 shows average grain size and the Mg of magnesium-3wt.% aluminium alloy
0.3al
0.4c
0.15rE
0.15relation between grain refiner content, wherein milling time is 20 hours.When adding the grain-refining agent of 1.5wt.%, the grain-size obtained is minimum.
Fig. 4 shows average grain size and the Mg of magnesium-3wt.% aluminium alloy
0.3al
0.4c
0.15rE
0.15relation between the milling time of grain-refining agent.Wherein Mg
0.3al
0.4c
0.15rE
0.15content be 1.0wt.%.Grind the situation of 20 hours at grain-refining agent, to obtain alloy grain size minimum.
Fig. 5 is presented at the Mg adding different content
0.3al
0.4c
0.15ca
0.15grain-refining agent and milling time are the situation of 20 hours, the average grain size of magnesium-3wt.% aluminium alloy.
Embodiment 1
The preparation of grain-refining agent:
In the present embodiment, the powder constituent before grinding lists in table 1, and wherein unit is " atom% " (atomic percent).
Table 1
Cylindrical cylinder of steel is adopted to prepare grain-refining agent.In order to prevent powder in process of lapping because temperature is too high and oxidized, use pure argon carries out filling for 5 times to be swept with excluding air.Grinding rate is 1000rpm.Select zirconia ball, and the ratio of ball and powder is 8: 1.Milling time is 5 to 20 hours (see table 1).In order to make reaction carry out continuously between different powder, the hold-time between twice grinding operation is 2 hours.In process of lapping, crucible cover can not be opened.After different milling time, the composition of gained sample is in table 1.
The Grain Refinement process of magnalium:
In the present embodiment, have employed magnesium-3wt.% aluminium alloy to study the effect of novel grain-refining agent.Through 700 grams of pure magnesium of 400 DEG C of preheatings in steel crucibles in 750 DEG C of fusings.SF
6with the mixed gas of argon gas as shielding gas.Then, 300 grams of preheated fine aluminiums are added in melt, then, spend within 15 minutes, stir melt.Grain-refining agent particle diameter being less than 20nm joins in melt.Add the operation of grain-refining agent in the melt in triplicate.After adding grain-refining agent, described melt is continued stirring 30 minutes.Then, the casting of alloy is carried out after 30 minutes in maintenance.With the grain morphology of observation by light microscope casting alloy.The average grain size of each sample is measured.
Fig. 1 (a)-(c) is for being presented at the microscopic optical structure that 750 DEG C are added to the grain refining effect of the original state powder of magnesium-3wt.% aluminium alloy.Visible, grain-size adds with different grain-refining agent and reduces.
Fig. 2 is presented at the microscopic optical structure that 750 DEG C are added to the grain refining effect of the original state powder of magnesium-3wt.% aluminium alloy.Grain-size reduces with the content increase of grain-refining agent.Detailed numerical value as shown in Figure 3.Adding the situation of grain-refining agent of 1.5wt.%, to obtain the value of grain-size minimum.Minimum average grain size is 67 μm.
Fig. 4 shows average grain size and the Mg of magnesium-3wt.% aluminium alloy
0.3al
0.4c
0.15rE
0.15relation between the milling time of grain-refining agent.Grind the situation of 20 hours at grain-refining agent, the grain-size that obtains in alloy minimum.
Embodiment 2
The preparation of grain-refining agent:
In the present embodiment, the powder constituent before grinding lists in table 2, and wherein unit is " atom% " (atomic percent).
Table 2
Cylindrical cylinder of steel is adopted to prepare grain-refining agent.In order to prevent powder in process of lapping because temperature is too high and oxidized, use pure argon carries out filling for 5 times to be swept with excluding air.Grinding rate is 1000rpm.Select zirconia ball, and the ratio of ball and powder is 8: 1.Milling time is 5 to 20 hours (see table 2).In order to make reaction carry out continuously between different powder, the hold-time between twice grinding operation is 2 hours.In process of lapping, crucible cover can not be opened.After different milling time, the composition of gained sample is in table 2.
The Grain Refinement process of magnalium:
In the present embodiment, have employed magnesium-3wt.% aluminium alloy to study the effect of novel grain-refining agent.Through 700 grams of pure magnesium of 400 DEG C of preheatings in steel crucibles in 750 DEG C of fusings.SF
6with the mixed gas of argon gas as shielding gas.300 grams of preheated fine aluminiums are added in the melt of magnesium alloy.Then, spend within 15 minutes, stir gained liquid.Grain-refining agent particle diameter being less than 20nm joins in liquid.Add the operation of grain-refining agent in the melt in triplicate.After adding grain-refining agent, described melt is continued stirring 30 minutes.Then, the casting of alloy is carried out after 30 minutes in maintenance.With the grain morphology of observation by light microscope casting alloy.The average grain size of each sample is measured.
Be added with the grain-refining agent Mg of 1wt.%
0.3al
0.4c
0.15ca
0.15the typical microstructure of magnesium-3wt.% aluminium alloy as shown in Fig. 1 (b).Compare with magnesium-3wt.% aluminium alloy, after the interpolation of this fining agent, crystal grain is by refinement significantly.Fig. 5 shows average grain size and adds grain-refining agent Mg in magnesium-3wt.% aluminium alloy to
0.3al
0.4c
0.15ca
0.15content between mutual relationship.Grain-size reduces with the content increase of fining agent.When the fining agent added is more than 1wt.%, grain-size just tends towards stability.
Claims (11)
1. a magnalium, containing grain-refining agent, the chemical formula of described grain-refining agent is:
Mg
100-x-y-zAl
xC
yR
z
Wherein, R is selected from the cohort that silicon, calcium and strontium are formed, and x is 10 to 60At.%, y be 5 to 50At.%, z is 0 to 20At.%, and condition is that x+y+z is less than 100At.%.
2. magnalium according to claim 1, it comprises the described grain-refining agent that addition is 0.1% to 2% weight of described magnalium initial weight.
3. magnalium according to claim 1, wherein R is selected from the cohort that silicon, calcium, strontium and rare earth element are formed, and described rare earth element is selected from the cohort that lanthanum, neodymium, samarium and europium are formed further.
4. magnalium according to claim 1, wherein said magnalium is selected from the cohort that Mg-Al-Zn Alloy and magnalium manganese alloy are formed.
5. magnalium according to claim 4, wherein said alloy is selected from AM50, the cohort that AM60, AM201, AZ10, AZ31, AZ63, AZ80, AZ91, AE44, AE42, AJ53, AS41 and AS42 are formed.
6. prepare the method for the magnalium containing trickle crystal grain for one kind; it comprises and being melted in shielding gas atmosphere by the alloy containing magnesium and aluminium; and joined by grain-refining agent according to any one of claim 1 to 5 in the magnalium of described fusing, and make described alloy graining.
7. method according to claim 6, the magnalium of the described fusing wherein containing described grain-refining agent was cast before making described alloy graining.
8. method according to claim 6, wherein said shielding gas comprises argon gas.
9. method according to claim 6, wherein said shielding gas comprises SF further
6.
10. method according to claim 6, wherein said grain-refining agent has the abrasive dust being less than 50nm particle size.
11. methods according to claim 6, wherein after adding described grain-refining agent, stir the magnalium of described fusing 10 to 60 minutes.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP11152825.3A EP2481822B1 (en) | 2011-02-01 | 2011-02-01 | Magnesium-aluminum based alloy with grain refiner |
| EP11152825 | 2011-02-01 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102628133A CN102628133A (en) | 2012-08-08 |
| CN102628133B true CN102628133B (en) | 2015-07-08 |
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| CN201210022182.3A Expired - Fee Related CN102628133B (en) | 2011-02-01 | 2012-02-01 | Magnesium-aluminum based alloy |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US20120195789A1 (en) |
| EP (1) | EP2481822B1 (en) |
| CN (1) | CN102628133B (en) |
| CA (1) | CA2765465A1 (en) |
| ES (1) | ES2424005T3 (en) |
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| US9230601B2 (en) | 2005-07-01 | 2016-01-05 | Invention Science Fund I, Llc | Media markup system for content alteration in derivative works |
| US9065979B2 (en) | 2005-07-01 | 2015-06-23 | The Invention Science Fund I, Llc | Promotional placement in media works |
| US9092928B2 (en) | 2005-07-01 | 2015-07-28 | The Invention Science Fund I, Llc | Implementing group content substitution in media works |
| US9583141B2 (en) | 2005-07-01 | 2017-02-28 | Invention Science Fund I, Llc | Implementing audio substitution options in media works |
| US8126938B2 (en) | 2005-07-01 | 2012-02-28 | The Invention Science Fund I, Llc | Group content substitution in media works |
| US20070276757A1 (en) * | 2005-07-01 | 2007-11-29 | Searete Llc, A Limited Liability Corporation Of The State Of Delaware | Approval technique for media content alteration |
| US7860342B2 (en) | 2005-07-01 | 2010-12-28 | The Invention Science Fund I, Llc | Modifying restricted images |
| US8126190B2 (en) | 2007-01-31 | 2012-02-28 | The Invention Science Fund I, Llc | Targeted obstrufication of an image |
| US9215512B2 (en) | 2007-04-27 | 2015-12-15 | Invention Science Fund I, Llc | Implementation of media content alteration |
| CN104087804B (en) * | 2014-07-28 | 2016-09-07 | 胡贤晨 | A kind of creep resistance Dow metal and preparation method thereof |
| CN112030049A (en) * | 2020-07-14 | 2020-12-04 | 中国石油天然气股份有限公司 | Controllable dissolution magnesium alloy material and preparation method thereof |
| CN112921225B (en) * | 2021-02-16 | 2022-06-21 | 河南工学院 | Aluminum-coated nano Al for Mg-Al alloy4C3Granular grain refiner and preparation method thereof |
| CN115198128A (en) * | 2022-07-08 | 2022-10-18 | 宝胜（宁夏)线缆科技有限公司 | Zero-carbon manufacturing process for high-quality regenerated aluminum-silicon alloy |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135013A (en) * | 2007-10-11 | 2008-03-05 | 武汉理工大学 | Magnesium and magnesium alloy composite grain refiner and method for making same |
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| CA1289748C (en) * | 1985-03-01 | 1991-10-01 | Abinash Banerji | Producing titanium carbide |
| CN1151293C (en) * | 2002-11-25 | 2004-05-26 | 山东大学 | Fining agent used for magnesium alloy and its preparation method |
| US8016957B2 (en) * | 2006-02-03 | 2011-09-13 | GM Global Technology Operations LLC | Magnesium grain-refining using titanium |
| CN101774013B (en) * | 2010-02-26 | 2012-05-23 | 华南理工大学 | Composite grain finer for Mg-Al alloy and preparation method thereof |
-
2011
- 2011-02-01 ES ES11152825T patent/ES2424005T3/en active Active
- 2011-02-01 EP EP11152825.3A patent/EP2481822B1/en not_active Not-in-force
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| CN101135013A (en) * | 2007-10-11 | 2008-03-05 | 武汉理工大学 | Magnesium and magnesium alloy composite grain refiner and method for making same |
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| CN102628133A (en) | 2012-08-08 |
| EP2481822A1 (en) | 2012-08-01 |
| ES2424005T3 (en) | 2013-09-26 |
| EP2481822B1 (en) | 2013-05-08 |
| US20120195789A1 (en) | 2012-08-02 |
| CA2765465A1 (en) | 2012-08-01 |
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