CN102827672A - Cutting liquid and preparation method thereof - Google Patents
Cutting liquid and preparation method thereof Download PDFInfo
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- CN102827672A CN102827672A CN2011101635427A CN201110163542A CN102827672A CN 102827672 A CN102827672 A CN 102827672A CN 2011101635427 A CN2011101635427 A CN 2011101635427A CN 201110163542 A CN201110163542 A CN 201110163542A CN 102827672 A CN102827672 A CN 102827672A
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Abstract
The invention provides a cutting liquid and a preparation method of the cutting liquid. The cutting liquid contains polyethylene glycol, a surfactant, alcohol amine and a chelating agent, wherein the chelating agent is inositol hexaphosphate. The cutting liquid has excellent solid-carrying performance, the cutting efficiency is greatly improved and the service life of the cutting liquid is greatly prolonged.
Description
Technical field
The present invention relates to a kind of cutting liquid and preparation method thereof, especially a kind of cutting liquid that is used for the polysilicon lines cutting and preparation method thereof.
Background technology
The environmental problem of face of mankind nowadays is increasingly serious, and suitability for industrialized production also is increasingly high to the requirement in the cutting processing process.For line cutting field, efficient, environmental protection, economy, toxicological harmless, the new type water-solubility cutting liquid that can be recycled become the target that modernized processing industry is pursued.
As everyone knows, cutting liquid has lubricated, cooling, cleaning and effect such as antirust, to improving cutting liquid processing quality and efficient, reduces tool wear etc. and all has unusual effect.Closely during the last ten years; The cutting liquid technical development of China is very fast, and cutting liquid new variety constantly occur, and performance also constantly is improved and is perfect; The particularly water base synthetic cutting liquid of late 1970s production and semi-synthetic cutting liquid (the microemulsified cutting liquid) promotion and application aborning that grew up in recent years; For mechanical workout to energy-conservation, reduce environmental pollution, reduce industrial production cost direction and develop and has opened up new route.Cutting liquid has oil base and water base two big classes, and the oilness of oil base cutting liquid wherein is quite a lot of, and the cooling property of water base cutting liquid is quite a lot of.But these two kinds certain shortcomings of cutting liquid ubiquity: oil base cutting liquid is prone to produce smog when high temperature, is prone to catch fire; Water base cutting liquid is prone to give birth to mycocriny and loses, and the usage period is short, gets rusty easily, and is unfavorable for reclaiming.For example, disclose a kind of cutting liquid in the prior art, comprised polyoxyethylene glycol, amine alkali, permeate agent, ether alcohol class promoting agent, YD 30 and deionized water.But the grittiness of taking of the cutting liquid of above-mentioned system can be all relatively poor, and the particle free settling in the cutting liquid greatly reduces the efficient of cutting and the work-ing life of cutting liquid.
Summary of the invention
Take the technical problem of sand poor performance in order to overcome cutting liquid of the prior art, the invention provides a kind of cutting liquid, this cutting liquid have excellent take grittiness can, improved the efficient of cutting and the work-ing life of cutting liquid greatly.
Cutting liquid disclosed by the invention comprises polyoxyethylene glycol, tensio-active agent, hydramine and sequestrant, and said sequestrant is nucite six phosphonic acid esters.
Simultaneously, the invention also discloses the preparation method of above-mentioned cutting liquid, comprise polyoxyethylene glycol, tensio-active agent, hydramine and sequestrant are mixed, and stir 30-40min with the rotating speed of 250-300rad/min.
Cutting liquid disclosed by the invention contains polyoxyethylene glycol.Polyoxyethylene glycol can be adsorbed in solid particulate (cutting sand) surface, produces sufficiently high barrier potential and builds with electricity, hinders not only that particle is approaching each other, coalescence, also can impel solid particulate group cracking to scatter, and what can guarantee to cut liquid to a certain extent takes the grittiness ability.But the contriver finds that the grittiness of taking of polyoxyethylene glycol can be still not enough, and cutting efficiency is still very short with the life-span of cutting liquid.And contriver of the present invention finds through a large amount of experiments, when adopting cutting liquid disclosed by the invention to carry out the line cutting, and each component acting in conjunction in the cutting liquid; Impel the effective complexing cutting of the sequestrant sand particle in the above-mentioned cutting liquid; Form more stable spacial framework, given cutting liquid excellent take grittiness can, prevent to cut the sedimentation of sand particulate; Cutting sand can be suspended in the cutting liquid for a long time, improve the efficient of cutting greatly.
In addition, above-mentioned cutting liquid has low-down specific conductivity, and when polycrystalline silicon used for solar battery being carried out the line cutting, the specific conductivity that can not cause cutting the silicon chip that obtains improves, and has avoided the influence to solar cell properties.
Embodiment
Clearer for technical problem, technical scheme and beneficial effect that the present invention is solved, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
The invention discloses a kind of cutting liquid, comprise polyoxyethylene glycol, tensio-active agent, hydramine and sequestrant, said sequestrant is nucite six phosphonic acid esters.
Cutting liquid disclosed by the invention is staple with the polyoxyethylene glycol.
At present; Performance index such as the planeness on solar silicon wafers surface, cleanliness factor, electroconductibility have strict requirement; In the cutting process of solar silicon wafers; Needs use the hardness height, granularity is little and microparticulate is cut sand (silicon-carbide particle) uniformly, in cutting process, can bump and rub between silicon-carbide particle and the silicon rod.Cut the influence that system temperature raises and warpage is taken place and silicon chip surface is carbonized the silicon grain over-mastication and influences its smooth finish for fear of the silicon chip that is cut out, must manage in time to take cutting heat and crushed particles out of the cutting system.Among the present invention, be staple with the polyoxyethylene glycol, and the cutting liquid that combines the specific sequestrant of the present invention and tensio-active agent, hydramine to prepare, have excellent lubricating properties, also improved the heat dispersion in the cutting process simultaneously greatly.
The polyoxyethylene glycol that adopts among the present invention is well known in the art, and its weight-average molecular weight is 200-600.Above-mentioned polyoxyethylene glycol can be commercially available, like PEG-200, PEG-400, PEG-600.
Also contain tensio-active agent in the cutting liquid disclosed by the invention.Road as is known to the person skilled in the art, the content of above-mentioned tensio-active agent can change in a big way, under the preferable case, is benchmark with the content of polyoxyethylene glycol, and the content of said tensio-active agent is 1.5-11wt%, more preferably 3-4wt%.
According to the present invention, above-mentioned tensio-active agent is this area tensio-active agent commonly used, and for example said tensio-active agent contains TX10 and/or AEO.Abovementioned alkyl phenol polyethenoxy ether and AEO are known in those skilled in the art, and for example said AEO can be in isooctyl alcohol Soxylat A 25-7, ethoxylated dodecyl alcohol, butanols Soxylat A 25-7, the lauryl alcohol Soxylat A 25-7 one or more.Said TX10 can all can be commercially available for one or more abovementioned alkyl phenol polyethenoxy ethers and the AEO in polyoxyethylene nonylphenol, polyoxyethylene octylphenol ether, the polyaryl phenol polyethenoxy ether; For example, AEO can adopt any one among O-10, O-15, O-20, the O-25.
For the abovementioned alkyl phenol polyethenoxy ether, its content can change in a big way, under the preferable case, is benchmark with the content of polyoxyethylene glycol, and the content of said TX10 is 3-4wt wt%.
For above-mentioned AEO, its content can change in a big way, under the preferable case, is benchmark with the content of polyoxyethylene glycol, and the content of said AEO is 1.5-2.5wt wt%.
According to the present invention, further under the preferable case, the tensio-active agent in the said cutting liquid comprises TX10 and AEO simultaneously.
Among the present invention,, can strengthen the lubrication of cutting liquid through adopting above-mentioned tensio-active agent; Make surfactant molecule can be adsorbed in silicon chip surface; The frictional force that in cutting process, can reduce to cut, the cut of minimizing silicon chip surface effectively raises the cutting yield.
Simultaneously; Also comprise hydramine in the cutting liquid disclosed by the invention; Above-mentioned hydramine is a various hydramine well known in the art, and for example, said hydramine is selected from one or more in trolamine, AEEA, tri-isopropanolamine, diglycolamine, dimethylethanolamine, the N methyldiethanol amine.The content of above-mentioned hydramine can change in a big way, under the preferable case, in the said cutting liquid, is benchmark with the content of polyoxyethylene glycol, and the content of said hydramine is 1-3wt%.
According to the present invention, above-mentioned sequestrant is nucite six phosphonic acid esters.For the content of above-mentioned sequestrant, can in a big way, change, under the preferable case, in the said cutting liquid, be benchmark with the content of polyoxyethylene glycol, the content of said sequestrant is 0.1-0.3wt%.
According to the present invention, can also contain the Soxylat A 25-7 boric acid ester in the tensio-active agent of above-mentioned cutting liquid.The contriver finds, through adding the Soxylat A 25-7 boric acid ester, can reduce the water cut in the cutting liquid greatly, and moisture content influences the suspension of silit in the cutting process of avoiding causing owing to the moisture in the cutting liquid, and then influences cutting efficiency.
The content of above-mentioned Soxylat A 25-7 boric acid ester can change in a big way, under the preferable case, in the said cutting liquid, is benchmark with the content of polyoxyethylene glycol, and the content of said Soxylat A 25-7 boric acid ester is 3-4wt%.
Further under the preferable case, said tensio-active agent contains Soxylat A 25-7 boric acid ester, TX10 and AEO simultaneously.When containing above-mentioned three kinds of components in the tensio-active agent simultaneously, it doesn't matter for the content between the three, need be that three's total content gets final product in the 1.5-11wt% scope only.
In order further to improve the over-all properties of cutting liquid,, in the above-mentioned cutting liquid, also contain explosive agent and skimmer in the said cutting liquid according to the present invention.
Said explosive agent is well known in the art, can improve the hard power problem of cutting process, reduces the infringement of cutting process to the higher silicon chip of hardness, effectively raises cutting efficiency simultaneously.Above-mentioned explosive agent can be commercially available, and for example, can adopt the graduate explosive agent of cloud Qinghua, Shandong worker.The content of above-mentioned explosive agent is known in those skilled in the art, under the preferable case, is benchmark with the content of polyoxyethylene glycol, and the content of said explosive agent is 0.1-0.2wt%.
Simultaneously, in order to reduce the air bubble content in the cutting liquid, under the preferable case, can also contain skimmer in the above-mentioned cutting liquid.Above-mentioned skimmer is well known in the art, and for example silicone antifoam agent specifically can adopt methyl-silicone oil.The content of above-mentioned skimmer is known in those skilled in the art, under the preferable case, is benchmark with the content of polyoxyethylene glycol, and the content of said skimmer is 0.1-0.3wt%.
In addition, the invention also discloses the preparation method of above-mentioned cutting liquid, comprise polyoxyethylene glycol, tensio-active agent, hydramine and sequestrant are mixed, and stir 30-40min with the rotating speed of 250-300rad/min.
In order to make the cutting fluidity for preparing can be better more stable, under the preferable case, earlier polyoxyethylene glycol is stirred 10-15min, add tensio-active agent, hydramine and sequestrant then respectively, also comprise between adjacent twice interpolation and stir 15-20min; After adding completion, continue to stir 30-40min.For example, can earlier polyoxyethylene glycol be joined in the Mixer pot, begin to stir, then tensio-active agent (or hydramine or sequestrant) joined in the Mixer pot, stir; Again hydramine (or sequestrant or tensio-active agent) is joined in the Mixer pot, stir; Then sequestrant (or tensio-active agent or hydramine) is joined in the Mixer pot, stir.The interpolation order of above-mentioned tensio-active agent, hydramine and sequestrant can change, and only needs respectively each material to be added, and stirs then to get final product.When containing multiple material in the tensio-active agent, be preferably respectively various materials are added separately, and after interpolation, stir.
Can prepare cutting liquid disclosed by the invention through aforesaid method.
Through embodiment the present invention is further explained below.
Embodiment 1
Present embodiment is used to explain cutting liquid disclosed by the invention and preparation method thereof.
100 weight part polyoxyethylene glycol (PEG-400), 2.5 weight part butanols Soxylat A 25-7s, 1 weight part AEEA, 0.1 weight part explosive agent (cloud Qinghua, Shandong worker research institute) and 0.1 weight part nucite, six phosphonic acid esters, 0.1 weight part silicone antifoam agent are added in the Mixer pot; Start stirrer, with the rotating speed stirring 40min of 250rad/min.Obtain cutting liquid S1.
Embodiment 2
Present embodiment is used to explain cutting liquid disclosed by the invention and preparation method thereof.
100 weight part polyoxyethylene glycol (PEG-400) are added in the Mixer pot, start stirrer, the rotating speed stirring 15min with 250rad/min adds 1.5 weight part ethoxylated dodecyl alcohols then, stirs 20min; Add 1 weight part diglycolamine again, stir 20min; Add 0.1 weight part explosive agent (cloud Qinghua, Shandong worker research institute) again, stir 20min; Add 0.1 weight part nucite, six phosphonic acid esters again, stir 20min; Add 0.1 weight part silicone antifoam agent then, stir 30min; Obtain cutting liquid S2.
Embodiment 3
Present embodiment is used to explain cutting liquid disclosed by the invention and preparation method thereof.
100 weight part polyoxyethylene glycol (PEG-400) are added in the Mixer pot, start stirrer, the rotating speed stirring 13min with 250rad/min adds 2 weight part isooctyl alcohol Soxylat A 25-7s then, stirs 20min; Add 3 weight part polyoxyethylene octylphenol ethers again, stir 20min; Add 1 weight part trolamine again, stir 20min; Add 0.1 weight part explosive agent (cloud Qinghua, Shandong worker research institute) again, stir 20min; Add 0.1 weight part nucite, six phosphonic acid esters again, stir 20min; Add 0.1 weight part silicone antifoam agent then, stir 30min; Obtain cutting liquid S3.
Embodiment 4
Present embodiment is used to explain cutting liquid disclosed by the invention and preparation method thereof.
100 weight part polyoxyethylene glycol (PEG-400) are added in the Mixer pot, start stirrer, the rotating speed stirring 10min with 300rad/min adds 2 weight part isooctyl alcohol Soxylat A 25-7s then, stirs 20min; Add 4 weight part polyoxyethylene nonylphenols again, stir 20min; Add 3 weight part Soxylat A 25-7 boric acid esters again, stir 20min; Add 2 weight part trolamines again, stir 20min; Add 0.1 weight part explosive agent (cloud Qinghua, Shandong worker research institute) again, stir 20min; Add 0.2 weight part nucite, six phosphonic acid esters again, stir 20min; Add 0.1 weight part silicone antifoam agent then, stir 30min; Obtain cutting liquid S4.
Embodiment 5
Present embodiment is used to explain cutting liquid disclosed by the invention and preparation method thereof.
100 weight part polyoxyethylene glycol (PEG-400) are added in the Mixer pot, start stirrer, the rotating speed stirring 12min with 300rad/min adds 2 weight part isooctyl alcohol Soxylat A 25-7s then, stirs 20min; Add 3.4 weight part polyoxyethylene nonylphenols again, stir 20min; Add 3.8 weight part Soxylat A 25-7 boric acid esters again, stir 20min; Add 2.2 weight part trolamines again, stir 20min; Add 0.18 weight part explosive agent (cloud Qinghua, Shandong worker research institute) again, stir 20min; Add 0.25 weight part nucite, six phosphonic acid esters again, stir 20min; Add 0.1 weight part silicone antifoam agent then, stir 30min; Obtain cutting liquid S5.
Embodiment 6
Present embodiment is used to explain cutting liquid disclosed by the invention and preparation method thereof.
100 weight part polyoxyethylene glycol (PEG-400) are added in the Mixer pot, start stirrer, the rotating speed stirring 12min with 300rad/min adds 2 weight part isooctyl alcohol Soxylat A 25-7s then, stirs 20min; Add 4 weight part polyoxyethylene nonylphenols again, stir 20min; Add 4 weight part Soxylat A 25-7 boric acid esters again, stir 20min; Add 3 weight part trolamines again, stir 20min; Add 0.2 weight part explosive agent (cloud Qinghua, Shandong worker research institute) again, stir 20min; Add 0.3 weight part nucite, six phosphonic acid esters again, stir 20min; Add 0.1 weight part silicone antifoam agent then, stir 30min; Obtain cutting liquid S6.
Comparative Examples 1
This Comparative Examples is used for comparative illustration cutting liquid disclosed by the invention and preparation method thereof.
According to the method preparation cutting liquid of embodiment 5, different is not add nucite six phosphonic acid esters.Obtain cutting liquid D1.
Comparative Examples 2
This Comparative Examples is used for comparative illustration cutting liquid disclosed by the invention and preparation method thereof.
According to the method preparation cutting liquid of embodiment 5, different is to adopt sodium ethylene diamine tetracetate (EDTA) replacement nucite six phosphonic acid esters.Obtain cutting liquid D2.
Comparative Examples 3
This Comparative Examples is used for comparative illustration cutting liquid disclosed by the invention and preparation method thereof.
According to the method preparation cutting liquid of embodiment 5, different is to adopt hydroxy ethylene diphosphonic acid replacement nucite six phosphonic acid esters.Obtain cutting liquid D3.
Performance test
The above-mentioned cutting liquid S1-S6 for preparing and D1, D2 are carried out following performance test.
1, rust-preventing characteristic
On the ingot iron polished face, drip 4-5 with dropper and drip cutting liquid, then ingot iron is placed on the moisture eliminator dividing plate, the moisture eliminator bottom need be injected zero(ppm) water in advance; The dryer door of closing; Place thermostat container, the humidity with 95% is taken out and is observed behind 35 ℃ ± 2 times maintenance 48H.
2, suspension
Testing method: adopt the same trade mark 1200
#Silit is investigated 48 hours suspending powers of mortar.Wherein, suspensibility test is the mortar of joining sand: liquid=80g:80ml under 25 ℃, fully stir 2-3 minute after, in 100ml tool plug graduated cylinder, slowly add the 100ml mortar, clear liquid height behind the record 48h.
Suspensibility=((80-clear liquid height)/80) * 100%.
3, specific conductivity
Testing method: use conductivitimeter (model: the new river rising in Ningxia and flowing into central Shaanxi of thunder magnetic, the Shanghai DDS-11A of Instr Ltd. digital display conductivitimeter) test, need to use standard KCl to proofread and correct before the conductivitimeter test.
4, density
Testing method: use specific gravity hydrometer (model: density is tested westernization appearance (Beijing) Science and Technology Ltd.).
5, viscosity
Testing method: use viscometer (model: LVDV-1+) test.
The test result that obtains is inserted table 1.
Test result through table 1 can find out that cutting liquid disclosed by the invention has excellent suspension property, and particle wherein is free settling not, has improved cutting efficiency greatly.Simultaneously, the test result of comparative example 3 and embodiment 4 can be found out, adds the Soxylat A 25-7 boric acid ester to the moisture in the further reduction cutting liquid, and the suspension property that improves cutting liquid is very favourable, and its rustless property also is improved.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (11)
1. a cutting liquid comprises polyoxyethylene glycol, tensio-active agent, hydramine and sequestrant, it is characterized in that said sequestrant is nucite six phosphonic acid esters.
2. cutting liquid according to claim 1 is characterized in that, in the said cutting liquid, is benchmark with the content of polyoxyethylene glycol, and the content of said sequestrant is 0.1-0.3wt%.
3. cutting liquid according to claim 1 and 2 is characterized in that, in the said cutting liquid, is benchmark with the content of polyoxyethylene glycol, and the content of said tensio-active agent is 1.5-11wt%, and the content of said hydramine is 1-3wt%.
4. cutting liquid according to claim 1 is characterized in that said tensio-active agent contains TX10 and/or AEO.
5. cutting liquid according to claim 4 is characterized in that, in the said cutting liquid, is benchmark with the content of polyoxyethylene glycol, and the content of said TX10 is 3-4wt%, and the content of said AEO is 1.5-2.5wt%.
6. according to any described cutting liquid in the claim 1,4 or 5, it is characterized in that said tensio-active agent contains the Soxylat A 25-7 boric acid ester.
7. cutting liquid according to claim 6 is characterized in that, in the said cutting liquid, is benchmark with the content of polyoxyethylene glycol, and the content of said Soxylat A 25-7 boric acid ester is 3-4wt%.
8. according to claim 1 or 3 described cutting liquid, it is characterized in that said hydramine is selected from one or more in trolamine, AEEA, tri-isopropanolamine, diglycolamine, dimethylethanolamine, the N methyldiethanol amine.
9. cutting liquid according to claim 1 is characterized in that, in the said cutting liquid, also contains explosive agent and skimmer in the said cutting liquid; Content with polyoxyethylene glycol is benchmark, and the content of said explosive agent is 0.1-0.2wt%; The content of said skimmer is 0.1-0.3wt%.
10. the preparation method of cutting liquid as claimed in claim 1 comprises polyoxyethylene glycol, tensio-active agent, hydramine and sequestrant is mixed, and stirs 30-40min with the rotating speed of 250-300rad/min.
11. preparation method according to claim 10 is characterized in that, earlier polyoxyethylene glycol is stirred 10-15min, adds tensio-active agent, hydramine and sequestrant then respectively, also comprises between adjacent twice interpolation stirring 15-20min; After adding completion, continue to stir 30-40min.
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Cited By (6)
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| CN103274882A (en) * | 2013-06-09 | 2013-09-04 | 河南师范大学 | Linear cutting metal processing exploder, and preparation method and application thereof |
| CN104277890A (en) * | 2013-07-02 | 2015-01-14 | 江阴江化微电子材料股份有限公司 | Solar-energy silicon-chip cutting liquid |
| CN110511811A (en) * | 2019-08-20 | 2019-11-29 | 山东大海新能源发展有限公司 | A kind of photovoltaic silicon wafer aqueous cutting fluid and preparation method thereof |
| CN113293431A (en) * | 2021-06-02 | 2021-08-24 | 内蒙古和光新能源有限公司 | Square silicon core and preparation method thereof |
| CN114480009A (en) * | 2022-03-25 | 2022-05-13 | 广东高景太阳能科技有限公司 | Cutting fluid for thin slice fine-line large-size solar-grade silicon wafer |
| CN114989883A (en) * | 2022-07-21 | 2022-09-02 | 天津开放大学 | Environment-friendly low-freezing-point water-based cutting fluid |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274882A (en) * | 2013-06-09 | 2013-09-04 | 河南师范大学 | Linear cutting metal processing exploder, and preparation method and application thereof |
| CN103274882B (en) * | 2013-06-09 | 2015-08-19 | 河南师范大学 | A kind of Linear cut intermetallic composite coating explosive agent and its preparation method and application |
| CN104277890A (en) * | 2013-07-02 | 2015-01-14 | 江阴江化微电子材料股份有限公司 | Solar-energy silicon-chip cutting liquid |
| CN110511811A (en) * | 2019-08-20 | 2019-11-29 | 山东大海新能源发展有限公司 | A kind of photovoltaic silicon wafer aqueous cutting fluid and preparation method thereof |
| CN113293431A (en) * | 2021-06-02 | 2021-08-24 | 内蒙古和光新能源有限公司 | Square silicon core and preparation method thereof |
| CN114480009A (en) * | 2022-03-25 | 2022-05-13 | 广东高景太阳能科技有限公司 | Cutting fluid for thin slice fine-line large-size solar-grade silicon wafer |
| CN114480009B (en) * | 2022-03-25 | 2022-09-16 | 广东高景太阳能科技有限公司 | Cutting fluid for thin slice fine-line large-size solar-grade silicon wafer |
| WO2023179650A1 (en) * | 2022-03-25 | 2023-09-28 | 高景太阳能股份有限公司 | Cutting fluid for thin fine-wire large-size solar-grade silicon wafer |
| CN114989883A (en) * | 2022-07-21 | 2022-09-02 | 天津开放大学 | Environment-friendly low-freezing-point water-based cutting fluid |
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Application publication date: 20121219 |