TWI481580B - 具有高氧化鋯含量的耐火產物 - Google Patents
具有高氧化鋯含量的耐火產物 Download PDFInfo
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Description
本發明係關於一種具有高氧化鋯含量之新穎熔鑄耐火產物。
在耐火產物中,熟知用於構建玻璃熔融爐之熔鑄產物與燒結產物之間存在區別。
不同於燒結產物,熔鑄產物最常包括連接結晶晶粒之晶粒間玻璃相。燒結產物及熔鑄產物所造成之問題不同,因此解決該等問題所採用之技術解決方案一般亦不同。因此,一種開發用於製造燒結產物之組成物顯然不適用於製造熔鑄產物,反之亦然。
熔鑄產物常被稱為電熔合產物,其係藉由在電弧爐中熔融合適原料之混合物或利用適用於該等產物之任一其他技術而獲得。熔料隨後被澆鑄至模具中,且所得產物接著經受控制冷卻循環以恢復室溫而不破裂。熟習此項技術者亦將此項操作稱為「退火」。
在熔鑄產物中,具有高氧化鋯含量,亦即包括超過85重量%之氧化鋯(ZrO2
)之電熔合產物之顯著特性在於其極高耐蝕性,而不會使所製造之玻璃著色且不會產生缺陷。
慣常地,具有高氧化鋯含量之熔鑄產物亦包括氧化鈉(Na2
O),以避免由存在於產物中之氧化鋯與二氧化矽形成鋯石。當鋯石之形成伴隨有約20%之體積減小時,其實際上為有害的,由此在裂痕起點處產生機械應力。
由Saint-Gobain SEFPRO製造及銷售且涵蓋於專利EP-B-403 387中之產品ER-1195現今廣泛用於玻璃熔融爐中。其化學組成包含約94%之氧化鋯、4%至5%之二氧化矽、約1%之氧化鋁、0.3%之氧化鈉及小於0.05重量%之P2
O5
。其為用於玻璃製造爐之典型的具有高氧化鋯含量之產物。
FR 2 701 022描述具有高氧化鋯含量之熔鑄產物,該等熔鑄產物含有0.05至1.0重量%之P2
O5
及0.05至1.0重量%之三氧化二硼B2
O3
。此等產物具有高電阻率。藉此,其可能宜穩定玻璃電熔融期間之耗電量且避免在耐火產物中出現任何會導致其快速降解之短路問題。實際上,在玻璃電熔融期間,部分電流通過該等耐火產物。增加此等耐火產物之電阻率能夠使能夠流經其之電流量減少。
WO 2005 068393描述具有高氧化鋯含量之熔鑄產物,該等熔鑄產物具有高電阻率,同時將BaO、SrO、MgO、CaO、P2
O5
、Na2
O及K2
O含量降至最低。針對氧化鋁含量介於0.9與2.5%之間,此等產物含有0.1至1.2重量%之B2
O3
。
JP 63 285173描述具有高氧化鋯含量之熔鑄產物,針對二氧化矽含量小於6.5%,該等熔鑄產物具有優良電阻率及抗破裂性。
目前開發之高品質玻璃,詳言之用於LCD型平面螢幕之玻璃板會增加對玻璃熔融爐之耐火產物的要求。詳言之,需要無須借助於摻雜劑而具有進一步增強的電阻率之耐火產物。
本發明旨在滿足此需要。
更特定言之,本發明係關於一種熔鑄耐火產物,其包含基於以下質量百分比之氧化物且該等氧化物之總量為100%:-ZrO2
+HfO2
:補足餘數至100%;-SiO2
:7.0%至12.5%;-Al2
O3
:0.2%至0.8%;-Na2
O+K2
O:<0.10%;-B2
O3
:0.3%至1.5%;-CaO+SrO+MgO+ZnO+BaO:<0.4%;-P2
O5
:<0.15%;-Fe2
O3
+TiO2
:<0.55%;-其他氧化物物質:<1.5%;Al2
O3
質量含量/B2
O3
質量含量,即「A/B」比小於或等於2.0。
如稍後可見,本發明者已意外地發現,具有該組成之本發明產物可能具有改良電阻率。
本發明之耐火產物可能接著包括一或多個以下可選特徵:
-Al2
O3
質量含量/B2
O3
質量含量,即「A/B」比小於或等於1.8,較佳小於1.5,較佳小於1.2,較佳小於1.0,小
於0.8或甚至小於0.7。
-Al2
O3
質量含量/B2
O3
質量含量,即「A/B」比大於0.1,或甚至大於0.2,或甚至大於0.3。
-二氧化矽(SiO2
)之質量含量小於或等於11.0%,或甚至小於或等於10.0%,或甚至小於或等於9.5%。
-二氧化矽(SiO2
)之質量含量大於或等於7.5%,大於或等於7.7%,或甚至大於或等於8.0%。
-氧化鋁(Al2
O3
)之質量含量小於或等於0.7%,或甚至小於或等於0.6%,或甚至小於或等於0.5%。
-Al2
O3
之質量含量大於或等於0.25%,大於或等於0.3%。在一具體實例中,此含量大於或等於0.4%。
-氧化鋁(Al2
O3
)僅以雜質形式存在。
-(Na2
O+K2
O)之質量含量小於或等於0.05%,或甚至小於或等於0.03%。
-B2
O3
之質量含量大於或等於0.35%,或甚至大於或等於0.4%,或甚至大於或等於0.5%。
-B2
O3
之質量含量小於或等於1.2%,或甚至小於或等於1.0%,或甚至小於或等於0.80%,或小於或等於0.75%,或小於或等於0.70%,或小於或等於0.65%。
-P2
O5
之質量含量小於或等於0.05%。
-氧化鐵及/或氧化鈦及/或氧化鈣及/或氧化鍶及/或氧化鋇及/或氧化鎂及/或氧化鋅及/或五氧化二磷僅以雜質形式存在。
-氧化鐵及/或氧化鈦Fe2
O3
+TiO2
之質量含量小於
0.4%,較佳小於0.3%,較佳小於0.2%。
-氧化鈣及/或氧化鍶及/或氧化鋇及/或氧化鎂及/或氧化鋅之質量含量小於0.2%,較佳小於0.1%。
-氧化鈣及/或氧化鍶及/或氧化鋇及/或氧化鎂及/或氧化鋅CaO+SrO+BaO+MgO+ZnO之總質量含量小於0.3%,較佳小於0.2%。
-「其他氧化物物質」之總質量含量小於1.0%。
-「其他氧化物物質」僅由雜質組成,且「其他氧化物物質」之總質量含量小於0.6%,小於0.5%,或甚至小於0.3%。
-產物包括質量含量大於或等於0.1%,較佳大於或等於0.2%,較佳大於或等於0.25%及/或小於或等於1.3%,小於或等於1.0%,較佳小於或等於0.9%,更佳小於或等於0.6%之選自Nb2
O5
、Ta2
O5
及其混合物的摻雜劑。
-ZrO2
/(Nb2
O5
+Ta2
O5
)之莫耳比介於200與350之間。
-ZrO2
/(Nb2
O5
+Ta2
O5
)之莫耳比大於250。
-摻雜劑Ta2
O5
之質量含量大於或等於0.1%,較佳大於或等於0.2%,及/或小於或等於1.2%,較佳小於或等於0.6%。
-摻雜劑Nb2
O5
之質量含量大於或等於0.1%,較佳大於或等於0.2%,及/或小於或等於1.0%,較佳小於或等於0.6%。
-在一具體實例中,Nb2
O5
+Ta2
O5
之總質量含量小於或等於0.6%。
-二氧化矽(SiO2
)之質量含量大於或等於8.0%且小於
或等於10.0%,且選自Nb2
O5
、Ta2
O5
及其混合物之摻雜劑的質量含量小於或等於0.6%。
-三氧化二釔(Y2
O3
)之質量含量小於或等於1%,較佳小於0.5%,更佳小於0.3%,或甚至小於0.2%。
-在一具體實例中,BaO含量小於0.10%,或實質上為零。
-本發明不包括專利申請案第WO 2007 099 253號、第PCT/FR2008/051516號及第PCT/FR2008/051515號(及同族專利申請案)中所揭示之產物,且尤其不包括此等專利申請案之實施例中的產物。
-本發明不包括下列呈220×450×150mm3
之塊狀或呈直徑為30mm且高度為30mm之圓柱棒狀的產物,其組成由基於以下質量百分比之氧化物提供:
-在一具體實例中,所有具有上表中之組成之產物皆不包括在內,無論其為何種形式。
-在一具體實例中,所有組成接近於上表中之至少一種組成的產物皆不包括在內。在不考慮第一種組成之相關組分的情況下,當第一種組成中該組分之含量與第二種組成中該組分之含量的絕對差異以質量百分比計小於0.10%時,認為第一種組成「接近」於第二種組成。
在一較佳具體實例中,,較佳SiO2 10.0%,且,較佳。
更佳地,-且,其中Nb2
O5 0.6%,且-,或甚至,且-CaO+SrO+MgO+ZnO+BaO<0.3%,或甚至CaO+SrO+MgO+ZnO+BaO<0.2%,且-BaO<0.1%,且-Fe2
O3
+TiO2
<0.3%,且-Y2
O3
<0.3%。
本發明亦係關於一種製造本發明之耐火產物的方法,其包含以下連續步驟:
a) 混合原料以獲得初始負載;
b) 熔融該初始負載直至獲得熔料;
c) 澆鑄該熔料且藉由冷卻使其凝固,以獲得耐火產物,
該方法之顯著之處在於,該等原料係經選擇使得該耐火產物符合本發明。
較佳地,系統且有條理地添加需要極少含量之氧化物,尤其ZrO2
、SiO2
、B2
O3
或此等氧化物之前驅體。較佳地,考慮慣常將此等氧化物視為雜質之其他氧化物來源中此等氧化物之含量。
較佳控制冷卻,以便較佳以每小時小於20℃之速率進行冷卻,較佳以每小時約10℃之速率進行冷卻。
本發明亦係關於一種包括本發明之耐火產物或根據本發明方法製造之耐火產物或能夠根據本發明方法製造之耐火產物的玻璃熔融爐,詳言之,該玻璃熔融爐意欲在一定區域中與熔融玻璃接觸。在本發明之爐中,耐火產物宜成為藉由熔融、尤其藉由電熔融製備玻璃之容器的一部分,在該容器中耐火產物能夠在1,200℃以上之溫度下開始與熔融玻璃接觸。
定義
氧化物質量含量係指根據通常工業慣例,各表示為最穩定氧化物之對應化學元素的整體含量;因此,次氧化物及可能存在之氮化物、氮氧化物、碳化物、碳氧化物、碳氮化物或甚至上述元素中之金屬物質亦包括在內。
「熔料(molten material)」為液體塊,為保持其形狀,應將其容納於容器中。熔料可能含有少量固體粒子,但固體粒子之量不足以使其能夠構成該塊狀物。
「雜質(impurities)」意謂偶然但亦必然與原料一起引入或由該等組分反應所產生之不可避免的組分。雜質非所需組分,而僅為容許存在之組分。例如,鐵、鈦、釩及鉻之氧化物、氮化物、氮氧化物、碳化物、碳氧化物、碳氮化物及金屬物質之群中之部分化合物為雜質。
除非另外指明,否則所描述且主張之產物中所有氧化物之含量均為該等氧化物之質量百分比。
在本發明之具有高氧化鋯(ZrO2
)含量的熔鑄產物中,有可能滿足以下需求,即具有高耐蝕性,而不會使所製造之玻璃著色或產生對此玻璃之品質有害的缺陷。
在藉由熔融而獲得之產物中,HfO2
無法以化學方法與ZrO2
分離。因此,在此類產物之化學組成中,ZrO2
+HfO2
表示該兩種氧化物的總含量。然而,根據本發明,初始負載中之HfO2
並非特意添加的。因此,HfO2
僅表示痕量二氧化鉿,該氧化物始終以一般小於2%之含量天然存在於氧化鋯來源中。因此,為清晰起見,可由ZrO2
+HfO2
或由ZrO2
或另外由「氧化鋯含量」表示氧化鋯含量及二氧化鉿微含量。
在本發明產物中,二氧化鉿HfO2
含量小於或等於5%,一般小於或等於2%。
二氧化矽SiO2
之存在尤其會導致形成晶粒間玻璃相,晶粒間玻璃相在氧化鋯發生可逆性同素異形變態期間(亦即,自單斜晶相變化為四方晶相時)能夠有效地調節其體積變化。在質量含量大於7.0%之二氧化矽(SiO2
)存在下,可獲得高電阻率。
另一方面,所添加之二氧化矽不應超過12.5%,因為添加二氧化矽會對氧化鋯含量造成不利影響且因此可對耐蝕性造成不利影響。另外,過高二氧化矽含量可藉由釋放石塊(由於產物喪失內聚力而產生之耐火產物碎片)而在玻璃中產生缺陷,這在應用時被視為不良行為。
氧化鋁之存在會促進穩定玻璃相形成且會改良產物在模具中的可鑄性。含量過高會導致玻璃相不穩定(形成晶體),其對可行性產生消極影響,尤其在三氧化二硼存在下如此。因此,氧化鋁質量含量應保持低於0.8%。
在本發明產物中,認為氧化物Na2
O及K2
O具有類似效應。
Na2
O及K2
O氧化物對電阻率具有反效應。因此,Na2
O+K2
O之質量含量應小於0.1%。
B2
O3
質量含量之存在比例使得Al2
O3
質量含量/B2
O3
質量含量(即A/B比)小於或等於2,由此增加電阻率。
根據本發明,Fe2
O3
+TiO2
之質量含量小於0.55%且P2
O5
之質量含量小於0.15%,較佳小於0.10%,更佳小於0.05%。實際上,已知該等氧化物為有害的,且其作為雜質與原料一起引入時的含量應較佳限於痕量。
「其他氧化物物質」為以上未列出之物質,亦即,除ZrO2
、HfO2
、SiO2
、Al2
O3
、Na2
O、K2
O、B2
O3
、CaO、SrO、BaO、MgO、ZnO、P2
O5
、Fe2
O3
及TiO2
以外的物質。詳言之,Nb2
O5
及Ta2
O5
屬於「其他氧化物物質」。
在一具體實例中,「其他氧化物物質」限於非特別需要存在且一般以雜質形式存在於原料中之物質。
在另一具體實例中,「其他氧化物物質」亦可能包含宜存在之物質。因此,在一具體實例中,產物宜包括至少0.1%、較佳至少0.2%之可能進一步改良電阻率的摻雜劑,例如Nb2
O5
、Ta2
O5
或其混合物。然而,摻雜劑質量含量較佳小於或等於1.0%,較佳小於或等於0.9%,更佳小於或等於0.6%。
在一具體實例中,「其他氧化物物質」既不包括Nb2
O5
,亦不包括Ta2
O5
(產物不含此等氧化物)。
慣常地,在熔鑄產物中,氧化物佔產物質量之98.5%以上,99%以上,或實質上100%。上述情況亦適用於本發明產物。
本發明產物慣常可根據下述步驟a)至c)來製造:
a) 混合原料以形成初始負載;
b) 熔融該初始負載直至獲得熔料;
c) 藉由冷卻使該熔料凝固,以獲得本發明之耐火產物。
在步驟a)中,原料係經選擇以保證成品中氧化物之含量。
在步驟b)中,較佳藉助於不會引起任何還原之較長電弧與促進產物再氧化之混合的組合作用來實現熔融。
為將具有金屬態樣之生料粒的形成減至最少且為避免在最終產物中形成裂痕或裂紋,較佳在氧化條件下進行熔融。
優先使用法國專利第1 208 577號及其增補案第75893號及第82310號中所述之長弧熔融方法。
該方法係由以下步驟組成:使用電弧爐,其弧存在於負載與至少一個遠離該負載之電極之間;及調節弧長度使得其還原作用減少至最低程度,同時在熔化浴上方保持氧化氣氛且藉由弧本身之作用,或藉由使氧化氣體(例如空氣或氧氣)在浴中鼓泡或另外藉由向浴中添加釋放氧氣之物質(諸如過氧化物或硝酸鹽)來混合該浴。
詳言之,可在2,300℃以上之溫度下,較佳在介於2,400℃與2,500℃之間之溫度下進行熔融。
在步驟c)中,較佳以每小時小於20℃之速率,較佳以每小時約10℃之速率進行冷卻。
由此製造之本發明產物由玻璃相所圍繞的氧化鋯晶粒組成。以質量百分比計超過80%、超過90%、超過99%或實質上100%之氧化鋯可為單斜晶的。以基於玻璃相之質量百分比計,玻璃相可包括超過50%或甚至超過70%之二氧化矽、在5%與20%之間的B2
O3
及在1%與20%之間的氧化鋁。二氧化矽、B2
O3
及氧化鋁可佔玻璃相質量之95%以上、97%以上或實質上100%。
亦可應用任何基於意欲應用於玻璃熔融爐中之氧化鋯來製造熔合產物的習知方法,其限制條件為初始負載之組成允許獲得組成符合本發明產物之組成的產物。
實施例
給出以下非限制性實施例以達成說明本發明之目的。
在此等實施例中,使用以下原料:-氧化鋯,主要含有平均質量為98.5%之ZrO2
+HfO2
、為0.2%之SiO2
及為0.02%之Na2
O;-鋯砂,含有33%之二氧化矽;-三氧化二硼,純度超過99%。
在電弧爐中根據標準熔融方法熔融原料,隨後澆鑄熔料以獲得規格為220mm×450mm×150mm之塊。
實施例1對應於由Saint-Gobain SEFPRO銷售之產品ER1195,且為參考物。
對於所有所得產物而言,結晶分析顯示由玻璃相圍繞之單斜晶氧化鋯晶體通常包括超過70%之二氧化矽。在玻璃相中再次發現二氧化矽以及除氧化鋯以外之其他氧化物物質全體。
表1給出所得產物之化學分析;此分析為平均整體化學分析,以質量百分比形式給出。
在下表1中,*指示該實施例不在本發明內,空方框對應於含量小於或等於0.05質量%。用「其他氧化物物質」補足餘數至100%。
自不同的所得例示性塊上取出直徑為30mm且高度為30mm之產物圓柱棒。分別使此等棒在1,500℃或1,600℃下以100赫茲之頻率經受1伏特電位差,以分別進行電阻率量測「R1500」及「R1600」。
實施例6至9之比較證實,在二氧化矽含量實質上恆定且不存在Na2
O的情況下,小於2.0或甚至小於1.5且甚至小於0.8之A/B比會引起正效應,實施例9為較佳實施例。
結果亦展示,儘管不存在摻雜劑,但本發明之測試產物仍具有改良電阻率。
為證實此等最初結果,本發明者在熔合之1kg玻璃相塊上繼續進行其他電阻率量測。分別使此等塊在1,500℃或1,600℃下以2,500赫茲之頻率經受1伏特電位差,以分別進行電阻率量測「R1500」及「R1600」。結果概述於表2中。
此等測試證實A/B比之重要性。
表2進一步展示,在A/B比為0.6之實施例12中,針對R1500所獲得之最佳效能類似於針對R1600所獲得之最佳效能。
當然,本發明不限於所描述且說明之具體實例,該等具體實例作為說明性及非限制性實施例提供。
Claims (14)
- 一種熔鑄耐火產物,其包括基於以下質量百分比之氧化物且該等氧化物總計為100%:ZrO2 +HfO2 :補足餘數至100%;SiO2 :7.0%至11.0%;Al2 O3 :0.2%至0.7%;Na2 O+K2 O:<0.10%;B2 O3 :0.3%至1.5%;CaO+SrO+MgO+ZnO+BaO:<0.4%;P2 O5 :<0.15%;Fe2 O3 +TiO2 :<0.55%;其他氧化物物質:<1.5%;選自Nb2 O5 、Ta2 O5 及其混合物之摻雜劑的質量含量小於或等於1.0%;Al2 O3 質量含量/B2 O3 質量含量,即「A/B」比小於或等於2.0;不包括呈220×450×150mm3 之塊或直徑為30mm且高度為30mm之圓柱棒狀的熔鑄產物,其具有以下化學組成(以氧化物之質量百分比計):
- 如申請專利範圍第1項之產物,其中該A/B比小於1.5。
- 如申請專利範圍第1項之產物,其中該A/B比小於0.8。
- 如申請專利範圍第1項之產物,其包括質量含量大於或等於0.1%之該摻雜劑。
- 如申請專利範圍第1項之產物,其包括質量含量小於或等於0.6%之該摻雜劑。
- 如申請專利範圍第1項之產物,其既不包括Nb2 O5 ,亦不包括Ta2 O5 。
- 如申請專利範圍第1項之產物,其中二氧化矽SiO2 之質量含量小於或等於10.0%。
- 如申請專利範圍第1項之產物,其中二氧化矽SiO2 之質量含量大於或等於8.0%。
- 如申請專利範圍第1項之產物,其中B2 O3 之質量含量大於或等於0.5%。
- 如申請專利範圍第1項之產物,其中B2 O3 之質量含量小於或等於1.0%。
- 如申請專利範圍第10項之產物,其中B2 O3 之質量含量小於或等於0.8%。
- 如申請專利範圍第1項之產物,其中Al2 O3 之質量含量小於或等於0.7%。
- 如申請專利範圍第1項至第12項中任一項之產物,其中CaO+SrO+BaO+MgO+ZnO<0.2%且其他氧化物 物質之含量小於1.5%,其限制條件為Y2 O3 <0.3%。
- 如申請專利範圍第1項之產物,其中Na2 O+K2 O之質量含量大於或等於0.05%,氧化鐵及/或氧化鈦Fe2 O3 +TiO2 之質量含量小於0.4%,P2 O5 之質量含量小於或等於0.05%,氧化鈣及/或氧化鍶及/或氧化鋇及/或氧化鎂及/或氧化鋅CaO+SrO+BaO+MgO+ZnO之總質量含量小於0.3%,且「其他氧化物物質」之總質量含量小於0.6%。
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FR2953825B1 (fr) * | 2009-12-16 | 2013-12-20 | Saint Gobain Ct Recherches | Produit refractaire a forte teneur en zircone. |
FR2955578B1 (fr) * | 2010-01-28 | 2014-06-13 | Saint Gobain Ct Recherches | Produit refractaire a forte teneur en zircone |
JP5718599B2 (ja) * | 2010-08-20 | 2015-05-13 | 株式会社ノリタケカンパニーリミテド | ジルコニア焼結体、並びにその焼結用組成物及び仮焼体 |
FR2969145B1 (fr) * | 2010-12-16 | 2013-01-11 | Saint Gobain Ct Recherches | Produit refractaire a haute teneur en zircone. |
FR2986227B1 (fr) * | 2012-01-27 | 2014-01-10 | Saint Gobain Isover | Procede de production de laine minerale |
EP2835364B1 (en) * | 2012-04-06 | 2020-06-10 | AGC Inc. | High zirconia fused cast refractory |
FR2996843B1 (fr) * | 2012-10-15 | 2020-01-03 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Produit d'oxyde de chrome. |
JP5763823B1 (ja) * | 2014-10-07 | 2015-08-12 | サンゴバン・ティーエム株式会社 | 高ジルコニア電気溶融鋳造耐火物 |
JP5806424B1 (ja) * | 2015-02-02 | 2015-11-10 | サンゴバン・ティーエム株式会社 | 高電気抵抗高ジルコニア電気溶融鋳造耐火物 |
FR3032963A1 (fr) * | 2015-02-20 | 2016-08-26 | Saint Gobain Ct Recherches | Produit fondu a forte teneur en zircone |
US20190169073A1 (en) * | 2016-05-20 | 2019-06-06 | Corning Incorporated | Purified ceramic materials and methods for making the same |
CN114394842A (zh) * | 2022-02-18 | 2022-04-26 | 中钢集团洛阳耐火材料研究院有限公司 | 一种烧结的致密高锆砖的制备方法 |
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BRPI1008905A2 (pt) | 2016-03-15 |
CN102325729B (zh) | 2015-08-26 |
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EA201190131A1 (ru) | 2012-02-28 |
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EP2401233B1 (fr) | 2013-07-10 |
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US8563454B2 (en) | 2013-10-22 |
FR2942468B1 (fr) | 2012-06-29 |
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US20120046156A1 (en) | 2012-02-23 |
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