CN1902142B - 具有高电阻率的熔铸氧化锆耐火材料 - Google Patents
具有高电阻率的熔铸氧化锆耐火材料 Download PDFInfo
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- 239000011819 refractory material Substances 0.000 claims description 38
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 208000037656 Respiratory Sounds Diseases 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 238000005382 thermal cycling Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000000976 ink Substances 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007531 graphite casting Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052845 zircon Inorganic materials 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- 206010000117 Abnormal behaviour Diseases 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000146 host glass Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
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Abstract
提供一种熔铸耐火材料。该耐火材料包含0.8～2.5％的Al2O3、4.0～10.0％的SiO2、86～95％的ZrO2、0.1～1.2％的B2O3、最多为0.04％的Na2O、最多为0.4％的CaO、最多为0.1％的Fe2O3和最多为0.25％的TiO2。
Description
(对相关申请的交叉引用)
本申请根据35U.S.C.§120要求在2004年1月2日提交的美国临时申请No.60/533990的提交日期的权益。
技术领域
本发明涉及熔铸氧化锆材料，特别涉及适用于玻璃熔炉的具有高电阻率的熔铸氧化锆耐火材料。
背景技术
主要包含ZrO2(“氧化锆”)的熔凝耐火材料传统上被用于玻璃熔炉中。氧化锆提供优良的对于熔融的玻璃的耐蚀性。称为AZS耐火材料的利用Al2O3-ZrO2-SiO2的耐火材料在本技术领域中是公知的。这种ZrO2浓度为80重量％或更高的耐火材料被称为高氧化锆熔凝耐火材料。
特别是在诸如TFT-LCD玻璃和等离子显示器面板的高质量玻璃的生产中，希望用于玻璃熔炉中的耐火材料具有高电阻率。一般还希望耐火材料提供较高的对于腐蚀和热循环的耐受力。
例如在授权给Ishino等的美国专利No.5466643(“643专利”)和授权给Endo等的美国专利No.5679612(“612专利”)中公开了高氧化锆熔凝耐火材料，在此通过引入并入它们的全部内容。
所述643专利公开了为了软化基质玻璃利用0.05～1.0％的P2O5的熔凝氧化锆耐火材料。虽然这种耐火材料的电阻率的水平是可以接受的，但其主要目的是提高热循环抗力，并且它通过增加玻璃相的总量实现这种目的，这会降低耐火材料的耐蚀性。
所述612专利公开了不使用P2O5但为了降低由于消除P2O5导致的耐火材料的玻璃相中的应力添加总量为0.05～3.0％的BaO、SrO和MgO的熔凝氧化锆耐火材料。该612专利还公开了使用Na2O(以大于0.05％的量)和K2O以减少由于添加上面列出的碱土金属氧化物产生的拉伸应力。以不同的量存在的Na2O和K2O不能在耐火材料中提供最佳的电阻率。
因此，本发明寻求在使BaO、SrO、MgO、CaO、P2O5、Na2O和K2O的浓度最小化的同时在熔凝氧化锆耐火材料中实现高电阻率。
发明内容
为了实现上述目的，提供熔铸耐火材料。耐火材料包含0.8～2.5％的Al2O3、4.0～10.0％的SiO2、86～95％的ZrO2、0.1～1.2％的B2O3、最多为0.04％的Na2O、最多为0.4％的CaO、最多为0.1％的Fe2O3和最多为0.25％的TiO2。
具体实施方式
除非另外注明，下面包括在任何权利要求中列出的所有百分比均基于重量，并且是从浇注流(pourstream)测量的熔铸耐火材料的百分比。本发明提供包含0.8～2.5％的Al2O3、4.0～10.0％的SiO2、86～95％的ZrO2、0.1～1.2％的B2O3、最多为0.04％的Na2O、最多为0.4％的CaO、最多为0.1％的Fe2O3和最多为0.25％的TiO2的熔铸耐火材料。根据本发明制成的耐火材料的特征在于在1625℃具有至少80欧姆-厘米的电阻率。已认识到，也可以制造具有更低的ZrO2含量和更高的玻璃含量的耐火材料，但它们的效用有限。
在一个优选实施例中，本发明是包含0.9～2.0％的Al2O3、6.0～8.0％的SiO2、88～92％的ZrO2、0.3～0.9％的B2O3、最多为0.04％的Na2O、最多为0.2％的CaO、最多为0.05％的Fe2O3和最多为0.15％的TiO2的熔铸耐火材料。
根据本发明的耐火材料的ZrO2含量是86～94％，并优选88～94％。高于94％的ZrO2含量不提供无裂纹的耐火材料，而低于86％的ZrO2含量导致对熔融的玻璃的耐受力较差。
根据本发明的耐火材料的SiO2含量是4～10％，或优选6～8％。当含量小于4％时，玻璃相不能形成为连续的基质相，而当含量高于10％时预计对熔融的玻璃的耐受力较差。
根据本发明的耐火材料的Al2O3含量是0.8～2.5％，并优选0.9～2.0％。当含量高于0.8％时Al2O3提高熔体的可流动性，而高于2.5％的含量导致玻璃相的不稳定，从而使得产品易于失效。
根据本发明的耐火材料的B2O3含量是0.1～1.2％，并优选0.3～0.9％。添加B2O3有助于在制造过程中抑制耐火材料中的裂纹。当含量小于0.1％时不能实现这种益处，而大于1.2％的浓度可导致玻璃相的异常行为。
CaO是根据本发明的耐火材料的任选成分，并以耐火材料的0.0～0.4％的量存在。为了在制造过程中帮助降低耐火材料中的应力并减少出现裂纹的可能，可以添加CaO。当本发明的耐火材料用于形成TFT-LCD或等离子显示器面板的玻璃熔炉中时，由于这些熔融的玻璃也可包含CaO，因此添加CaO也是有益的。
Na2O和K2O也是根据本发明的耐火材料的任选成分，并以耐火材料的0.0～0.04％的量存在。所述碱优选从耐火材料中被去除，因此它是玻璃中的导电性的主要来源。
TiO2和Fe2O3可以作为杂质存在，但是，由于它们可促进耐火材料的形成缺陷的潜力，因此，对于它们的单个浓度来说，TiO2不应超过0.25％，Fe2O3不应超过0.1％，并且总浓度不应超过0.35％。
实施例
原材料包括氧化锆(通过从锆砂中去除大部分的氧化硅得到)、锆砂、煅烧氧化铝、氧化硼、碳酸钙和僵烧镁氧(dead-burnedmagnesia)。选择这些原材料，使得将杂质(诸如Fe2O3、TiO2、Na2O、K2O)减少到最低水平。原材料被仔细称重并被混合成均匀的混合物，随后被放入大的熔炼用钢制坩锅。通过使用3相电流源由石墨电极对钢制坩锅供电。在操作过程中坩锅的外面连续被水冷却。
使原材料熔化一个小时，并将液体注入石墨铸型中。在正常的生产中，每小时、每24小时一天、最多每7天一星期重复一次该分批工艺。石墨铸型在大的钢制容器(称为大口箱)内被煅烧氧化铝粉末包围。在铸型被完全填充后，铸型的顶部被煅烧氧化铝粉末覆盖，并且大口箱被贮藏在建筑物内至少2星期的周期，以使铸件能缓慢冷却。这对于保证回收具有最少的裂纹乃至没有裂纹的铸件是重要的。
当填充铸型时，在从坩锅注入液体的过程中，在石墨容器中收集液体的小样。使该容器中的液体能够迅速冷却。通过使用X射线荧光谱仪对得到的样品进行化学测试。通过使用X射线荧光谱仪可以定量分析氧化锆耐火材料的一种成分以外的全部成分。通过使用感应耦合等离子谱仪(ICP)或DC电弧发射法分析B2O3。各种样品的化学成分示于下表中。
可以通过使用阿基米德水浸法或通过对整个铸件称重(在被机加工以去除铸型外皮后)并将重量除以铸件的外部体积，从直径为约25mm长度为约100mm的小圆柱芯体样品获得密度。
通过使用4点电极组件在直径为25mm长度为50mm的圆柱样品上测量电阻率。样品的端部被铂墨(platinum ink)涂敷。还将铂墨放在样品的外周上的分开25mm且距离各端12.5mm的两个位置上。然后在样品的各端部下面以及上述两个内部位置上缠绕铂导线。沿各端部施加电流，并跨过上述标距部分中的25mm带区测量电压降。通过使用交流和直流两种电流测量电阻率。
在一系列样品上检查显微结构，每一个样品约25mm长15mm宽，被安装在环氧树脂中并被抛光至1微米表面光洁度。这些样品可取自圆柱芯体，一般垂直穿过块体的最宽的面的中心钻取以代表平均的显微结构。一般从接近铸件的外表面及其芯部的区域制备抛光部分。可以通过使用光学显微镜和电子显微镜两种显微镜检查显微结构。通过使用X射线衍射仪进行晶体相的鉴别。可以通过使用电子显微镜中的能量色散谱仪(EDS)确定玻璃相化学成分。可以通过全量分析与100％的差估算玻璃相的平均硼含量。也可以从从对从同一样品获得的粉末进行的化学全分析(bulk chemical analysis)导出的数据-通过与由EDS和总体化学方法(bulk chemistry method)确定的硅含量的比-更精确地进行计算。
一般对取自铸件中的各个位置的直径为25mm长度为50mm的样品进行热循环耐受力试验。通过在电炉中使用受控的升温和冷却速率将样品从1250C到800C循环至少20次。在该试验之后，可以通过使用水浸法测量样品体积的变化。还可以通过使用照片证明裂纹的存在。
通过使用上述方法制造例子4～13。通过使用相同的方法制造比较例1～3。在下表中列出各例子的化学组成。还在下表中提供各例子的电阻率。
可以看出，从电阻率的观点说，例子4、12和13提供最理想的结果。例子4～13中的全部例子都实现至少80欧姆-厘米的希望的电阻率。在对于热循环的耐受力方面，所有的例子也都是可接受的。
很显然，本发明的许多修改和变更是可能的。因此，应当理解，在以下的权利要求书的范围内，可以以与具体说明的方式不同的方式实施本发明。
Claims (4)
1.一种耐火材料，基本由0.96～1.1％的Al2O3、6.6～8.8％的SiO2、89.3～91.2％的ZrO2、0.6～0.9％的B2O3、最多为0.02％的Na2O、最多为0.1％的CaO、最多为0.1％的Fe2O3和最多为0.1％的TiO2组成。
2.根据权利要求1的耐火材料，基本由0.96～1.1％的Al2O3、6.6～8.8％的SiO2、89.3～91.2％的ZrO2、0.6～0.9％的B2O3、最多为0.1％的CaO、最多为0.1％的Fe2O3和最多为0.1％的TiO2组成。
3.根据权利要求1的耐火材料，其特征在于，所述耐火材料在1625℃的温度下具有至少250欧姆-厘米的电阻率。
4.根据权利要求1的耐火材料，其特征在于，所述耐火材料在1625℃的温度下具有至少300欧姆-厘米的电阻率。
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| PCT/US2004/044042 WO2005068393A1 (en) | 2004-01-02 | 2004-12-30 | Fusion-cast refractory with high electrical resistivity |
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| CN1902142B true CN1902142B (zh) | 2010-12-22 |
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| BR (1) | BRPI0418269B1 (zh) |
| RU (1) | RU2006124609A (zh) |
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| FR2897861B1 (fr) * | 2006-02-24 | 2008-06-13 | Saint Gobain Ct Recherches | Refractaire a forte teneur en zircone a grande resistivite |
| JP4658870B2 (ja) | 2006-06-28 | 2011-03-23 | 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鋳造耐火物 |
| FR2913013B1 (fr) * | 2007-02-23 | 2009-12-18 | Saint Gobain Ct Recherches | Bloc refractaire fondu et coule a forte teneur en zircone |
| FR2920153B1 (fr) | 2007-08-24 | 2010-11-26 | Saint Gobain Ct Recherches | Produit refractaire a forte teneur en zircone dope. |
| FR2920152B1 (fr) * | 2007-08-24 | 2009-12-04 | Saint Gobain Ct Recherches | Refractaire a fortre teneur en zircone et teneur en silice elevee. |
| JP5270913B2 (ja) * | 2007-12-26 | 2013-08-21 | 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鋳造耐火物 |
| FR2932475B1 (fr) | 2008-06-16 | 2010-09-03 | Saint Gobain Ct Recherches | Produit refractaire a forte teneur en zircone |
| FR2942468B1 (fr) | 2009-02-25 | 2012-06-29 | Saint Gobain Ct Recherches | Produit refractaire a forte teneur en zircone. |
| WO2010116960A1 (ja) | 2009-04-06 | 2010-10-14 | 旭硝子株式会社 | 高ジルコニア質耐火物及び溶融窯 |
| 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 |
| FR2955577B1 (fr) | 2010-01-28 | 2014-06-20 | Saint Gobain Ct Recherches | Produit refractaire a forte teneur en zircone. |
| KR101206365B1 (ko) * | 2010-02-24 | 2012-11-29 | 주식회사 케이씨씨 | 세라믹 섬유 제조용 조성물 및 그로부터 제조된 고온단열재용 생체용해성 세라믹 섬유 |
| CN102718511A (zh) * | 2012-06-27 | 2012-10-10 | 巨石集团有限公司 | 半轻质高锆耐火材料 |
| JP6030953B2 (ja) * | 2012-12-28 | 2016-11-24 | Ａｇｃセラミックス株式会社 | 高ジルコニア質電鋳耐火物 |
| 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 |
| FR3032962A1 (fr) * | 2015-02-24 | 2016-08-26 | Saint-Gobain Centre De Rech Et D'Etudes Europeen | Bloc refractaire et four de fusion de verre |
| EP3286157A4 (en) | 2015-04-24 | 2018-12-05 | Corning Incorporated | Bonded zirconia refractories and methods for making the same |
| FR3092579B1 (fr) * | 2019-02-11 | 2023-04-14 | Saint Gobain Ct Recherches | Produit refractaire a haute teneur en zircone |
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| US5679612A (en) * | 1994-08-10 | 1997-10-21 | Toshiba Monofrax Co., Ltd. | High-zirconia fused refractories |
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| JPS4880610A (zh) * | 1972-02-03 | 1973-10-29 | ||
| JPS5912619B2 (ja) * | 1980-03-18 | 1984-03-24 | 旭硝子株式会社 | 高ジルコニア質熱溶融耐火物 |
| JPS6259576A (ja) * | 1985-09-10 | 1987-03-16 | 旭硝子株式会社 | 高ジルコニア質熱溶融耐火物 |
| FR2648455B1 (fr) * | 1989-06-15 | 1993-04-23 | Produits Refractaires | Produits refractaires fondus et coules a forte teneur en zircone |
| JP2926966B2 (ja) * | 1989-11-28 | 1999-07-28 | 旭硝子株式会社 | 高ジルコニア質熱溶融鋳造耐火物 |
| JPH04193776A (ja) | 1990-10-24 | 1992-07-13 | Nippon Concrete Ind Co Ltd | 無機質吸音材及びその製造方法 |
| JP2870188B2 (ja) * | 1990-11-27 | 1999-03-10 | 旭硝子株式会社 | 高ジルコニア質溶融鋳造耐火物 |
| US5344801A (en) * | 1992-06-26 | 1994-09-06 | Asahi Glass Company Ltd. | High zirconia fused cast refractory |
| FR2701022B1 (fr) * | 1993-02-03 | 1998-07-10 | Asahi Glass Co Ltd | Refractaires coules par fusion a forte teneur en zircone. |
| JP3570740B2 (ja) * | 1993-02-03 | 2004-09-29 | 旭硝子セラミックス株式会社 | 高ジルコニア質溶融鋳造耐火物 |
| JP3524629B2 (ja) | 1995-04-06 | 2004-05-10 | サンゴバン・ティーエム株式会社 | 高ジルコニア溶融耐火物 |
| JP3518560B2 (ja) * | 1994-08-10 | 2004-04-12 | サンゴバン・ティーエム株式会社 | 高ジルコニア溶融耐火物 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5679612A (en) * | 1994-08-10 | 1997-10-21 | Toshiba Monofrax Co., Ltd. | High-zirconia fused refractories |
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| Publication number | Publication date |
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| WO2005068393A1 (en) | 2005-07-28 |
| ATE510804T1 (de) | 2011-06-15 |
| ZA200605017B (en) | 2008-01-08 |
| EP1711445A1 (en) | 2006-10-18 |
| JP4714697B2 (ja) | 2011-06-29 |
| BRPI0418269B1 (pt) | 2016-03-08 |
| BRPI0418269A (pt) | 2007-05-02 |
| US20070249481A1 (en) | 2007-10-25 |
| AU2004313955A1 (en) | 2005-07-28 |
| JP2007517754A (ja) | 2007-07-05 |
| EP1711445A4 (en) | 2008-12-03 |
| EP1711445B1 (en) | 2011-05-25 |
| US7598195B2 (en) | 2009-10-06 |
| CN1902142A (zh) | 2007-01-24 |
| RU2006124609A (ru) | 2008-01-20 |
| AU2004313955B2 (en) | 2009-09-10 |
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