CN105683124A - 具有高氧化铝含量的产品 - Google Patents
具有高氧化铝含量的产品 Download PDFInfo
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- CN105683124A CN105683124A CN201480049988.9A CN201480049988A CN105683124A CN 105683124 A CN105683124 A CN 105683124A CN 201480049988 A CN201480049988 A CN 201480049988A CN 105683124 A CN105683124 A CN 105683124A
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Abstract
一种烧结的耐火产品,其具有块体形式且由尺寸大于100μm称为“粗粒”的所有粒子形成的颗粒和粘合所述粗粒且由尺寸小于或等于100μm的粒子组成的基质组成,所述颗粒占所述产品的45质量%至90质量%,所述产品基于氧化物具有如下质量百分比的组成:-Al2O3>80%,-SiO2<15%,-Na2O<0.15%,-Fe2O3<0.05%,-CaO<0.1%,-其构成至100%的余量的其他氧化物,基于所述产品的质量,基质中Na2O的含量大于0.010质量%。
Description
技术领域
本发明涉及具有高氧化铝含量的耐火产品,其包含通过含氧化铝的基质结合的聚集体。
本发明也涉及一种装置,且特别地涉及燃气轮机,其包含由根据本发明的产品制备的耐火内衬。
背景技术
氧化铝可以以多种形式出现,取决于它的制造工艺。
铝土矿熔融使可能得到被称为“棕刚玉”的氧化铝。对于最纯的产品,棕刚玉通常包含约0.2%至1%的铁氧化物含量。
或者,遵循Bayer工艺,铝土矿可用苏打处理,然后煅烧以实施纯化。然而,通常苏打以约0.1%至0.3%Na2O含量仍保留。所得到的氧化铝通常被称为“煅烧氧化铝”。
可研磨煅烧氧化铝直至得到典型地约0.5-50微米,或甚至0.3-10微米的粒度中值。所得到的氧化铝,被称为“活性氧化铝”,通常用于制造工业陶瓷。煅烧氧化铝颗粒的烧结使有可能制造粗颗粒或细颗粒,通常具有片晶形状。由此得到的氧化铝被称为“板状氧化铝”。活性氧化铝包含,如管状氧化铝和煅烧氧化铝,相对大量的苏打。
也可使煅烧氧化铝熔融以制造被称为“白刚玉”的氧化铝,其也包含大量的苏打,通常约0.2%-0.4%。
除这些通常的氧化铝外,制造商例如AluchemInc.提供非常纯的氧化铝粉末,包含小于0.1%苏打。这些氧化铝通常用于催化应用或单晶的制造。
包含通过铝基质结合的莫来石和/或板状氧化铝聚集体的具有高氧化铝含量的烧结的耐火产品是已知的。
该类型的耐火产品可特别地形成燃气轮机的燃烧室的所有或部分内衬。所述内衬从而通常具有10重量%至50重量%的莫来石,50%-90%的氧化铝和小于5%的二氧化硅。所述内衬通过燃烧气体且特别地通过高温蒸汽经受非常高的热机械应力且也经受显著的腐蚀。这特别地导致莫来石的分解和硅酸盐基玻璃相的攻击。
US3067050描述了由72%-90%的氧化铝和小于10%的无定形氧化硅的混合物在约1500℃下烧制产生的耐火材料。
US2009/0181257描述了旨在用于燃气轮机燃烧室的材料。
本发明的一个目的是提供具有高氧化铝含量的产品,其具有如下性能:改善的热机械抗性,和特别地改善的高温下挠曲强度,和高耐腐蚀性,特别地由燃气轮机中存在的蒸汽和气体引起的腐蚀。
发明内容
根据本发明,借助于烧结的耐火产品和基质来实现该目的,所述烧结的耐火产品具有块体形状且由尺寸均大于100μm的粒子(称为“粗粒”)形成的聚集体组成,所述基质使所述粗粒结合并由尺寸小于或等于100μm的粒子组成,所述聚集体占45重量%-90重量%的所述产品,所述产品具有基于氧化物的如下重量百分数的组成:
-Al2O3>80%,
-SiO2<15%,
-Na2O<0.15%,
-Fe2O3<0.05%,
-CaO<0.1%,
-其他氧化物,即除Al2O3、SiO2、Na2O、K2O、Fe2O3和CaO外的氧化物,其构成至100%的余量,
基质中Na2O的含量基于产品重量大于0.010重量%。
本发明人已发现,显著地,根据本发明的产品在1400℃具有非常高的挠曲断裂模量(MOR)而不减少耐腐蚀性能。更特别地,在该温度下MOR的改进相对于对具有相同的氧化铝含量但具有高于0.15%的Na2O含量的产品测得的MOR为约25%。该无法解释的发现是更加令人惊奇的,因为在低于1200℃的温度下该差异是极细微的。
本发明人也发现对于基质包含基于产品重量大于0.010重量%的含量的Na2O是有利的,以得到足够高的挠曲断裂模量。
根据本发明的产品也可具有一种或多种下面任选的特征:
-所述组成是如此的以使Na2O+K2O<0.20%;
-所述组成是如此的以使:
-Al2O3>85%和/或
-3%<SiO2<10%和/或
-Na2O+K2O<0.15%和/或
-Fe2O3<0.03%和/或
-CaO<0.05%和/或
-ZrO2<5%和/或
-TiO2<5%;
-所述组成是如此的以使:
-Al2O3>90%和/或
-SiO2>7%和/或
-Na2O<0.12%和/或
-ZrO2<1%和/或
-TiO2<1%;
-基于聚集体的重量,氧化铝聚集体中Na2O的含量小于0.070重量%;
-基于结晶相的重量,在一方面氧化铝的总量和另一方面莫来石和/或尖晶石和/或莫来石-氧化锆的总量大于95重量%;
-基于结晶相的重量,莫来石的量大于10重量%且小于50重量%;
-开孔率大于10体积%且小于30体积%,优选小于25体积%,小于20体积%;小于19体积%;
-使用水银测孔计测得的孔径分布是如此的以使:
-P50大于1μm并小于20μm,和/或
-P80大于10μm并小于50μm,和/或
-P90大于30μm并小于70μm;
-所述聚集体,对于大于90重量%,由粗莫来石粒子组成和/或由粗氧化铝粒子组成和/或由粗尖晶石粒子组成和/或由粗莫来石-氧化锆粒子组成;
-所述基质,对于大于90重量%,由氧化铝组成;
-尺寸小于或等于100μm且大于10μm的所述粒子占大于10%且小于30%的所述产品重量和/或尺寸小于或等于10μm的所述粒子占大于10%且小于30%的所述产品重量。
本发明还涉及用于制备根据本发明的烧结的块体形式的耐火产品特别是耐火瓷砖的方法,所述制备方法包含下面的连续步骤:
a)准备适合用于制备根据本发明的产品的原料;
b)将所述原料投入模具中并压缩所述原料以形成预制品;
c)将预制品从模具中移除;
d)干燥所述预制品;
c)烧结所述预制品。
本发明还涉及选自由燃气轮机,化学反应器,特别地二次重整反应器,特别地用于氨或甲烷的制造,烧制支撑物,特别地用于烧制陶瓷的支撑物,和玻璃熔炉上部结构形成的组的装置,所述装置包括至少部分由根据本发明的产品形成的一个壁。
定义
-“块体”理解为指不是颗粒的固体物体。其可特别地为砖形物和更特别地耐火板或瓷砖。
-“颗粒”理解为指尺寸小于10mm的固体物体。特别地尺寸大于100μm的颗粒(称为“粗颗粒”)、尺寸小于或等于100μm且大于10μm的那些(称为“细颗粒”)与尺寸小于或等于10μm的那些(称为超细颗粒)之间是有区别的。所有粗颗粒构成“粗粒部分”。所有细颗粒构成“细粒部分”。所有超细颗粒构成“超细粒部分”。所述细和超细颗粒统称为“基质颗粒”并构成“基质部分”。
在烧结产品的制备过程中,颗粒彼此结合。所述“粒子”在烧结产品中,实质上对应于原料中的颗粒。所述粒子的尺寸和它们在产品中的尺寸分布可通过例如使用激光粒度分析仪测量的原料中的颗粒粉末的颗粒尺寸和分布评估。
-一组颗粒形成“粉末”。
-粉末的粒度通常通过使用激光粒度分析仪实施的粒度分布表征来评估。所述激光粒度分析仪可为,例如,来自HORIBA的ParticaLA-950。
-总体的性质A(例如颗粒或孔的总体性能A)的百分位数(percentiles)或“百分位数(centiles)”10(A10)、50(A50)、90(A90)和99.5(A99.5)和更通常地“n”An是在关于该性能的累积分布曲线上分别对应于10%、50%、90%、99.5%和n%百分数的该性能的值,涉及该性能的值以递增次序分类。特别地,百分位数Dn和Pn分别涉及粒度和孔径。
根据所考虑的性能,所述百分数可为重量百分数,例如对于百分位数Dn,或体积百分数,例如对于百分位数Pn。
百分位数50通常被称为“中值”百分位数。例如,百分位数D50通常称为颗粒的“粒度中值”。
例如,10重量%的粉末的颗粒具有小于D10的尺寸且90重量%的颗粒具有大于或等于D10的尺寸。可借助于使用激光粒度仪产生的粒度分布确定涉及颗粒尺寸的百分位数。
相似地,例如,10体积%的产品的孔具有小于P10的尺寸且90体积%的孔具有大于或等于P10的尺寸。这些百分位数可根据标准ISO15901-1.2005第一部分,在通过由水银测孔计例如MicromeriticsAutoPoreIV9500系列水银测孔计产生的分布的辅助下确定。
-原料氧化物的颗粒混合物的粒度分布使有可能评估在对应的烧结产物中的粒子尺寸。
-“烧结”指通过在大于1100℃下热处理,预制品的固结,任选地具有其成分中一些(但不是其全部成分,以使所述预制品不转化为液体团liquidmass)的部分或完全熔融。
-“耐火”理解为指“具有1000℃以上的熔点或离解点”。
-“杂质”理解为指不可避免的成分,其与原料一起被无意和必定引入或来源于与这些成分的反应。所述杂质是不必要的成分而仅是可接纳的成分。
-除非另有说明,所有涉及含量的百分数均是基于氧化物的重量百分数。
-“Na2O+K2O”指Na2O和K2O含量的总和,这两种氧化物的每一个都是任选的。
-成分的重量含量通常表示为最稳定的氧化物形式。通常用于确定组成的装置(微探针、X射线荧光光谱仪、ICP(电感耦合等离子体)光谱仪)自动将非氧化物成分含量转化为等价的氧化物含量。
-当涉及ZrO2或(ZrO2+HfO2)时,应理解为ZrO2和痕量的HfO2。这是因为不可与ZrO2化学分离且具有相似性质的少量的HfO2通常基于ZrO2+HfO2以小于3重量%的含量天然存在于ZrO2的来源中。不认为二氧化铪是杂质。
-为了清楚的目的,氧化物的化学式用于唯一地表示这些氧化物在组分中的含量。例如,“ZrO”、“HfO2”、“SiO2”或“Al2O3”表示这些氧化物在组分中的含量且“氧化锆”、“二氧化铪”、“二氧化硅”和“氧化铝”唯一地用于表示分别由ZrO2、HfO2、SiO2和Al2O3组成的这些氧化物的结晶相。然而,这些氧化物也可以其他相特别地以莫来石的形式存在。
-“游离”二氧化硅通常表示SiO2相,其分子不与其他分子相关联,例如为耐火硅酸盐的形式,特别地锆石和莫来石的形式。
-除非另有说明,“包含一种(Containinga)”、“包括一种(comprisinga)”或“具有一种”理解为指“具有至少一种”。
具体实施方式
产品
所述产品可特别地为块体形式,且特别地为板或瓷砖形式。优选地,所述块体的厚度小于60mm,小于50mm,小于40mm,或甚至小于30mm和/或大于10mm,优选大于15mm。优选地,所述块体的长度和/或宽度大于10cm,大于20cm和/或小于50cm,优选小于40cm。
所述块体也可以为砖形物的形式,且特别地为平行六面体(parallelepipedal)砖形物的形式。所述砖形物的长度可为大于15cm,或甚至大于20cm和/或小于35cm,小于30cm,或甚至小于25cm。所述砖形物的宽度和/或厚度优选大于4cm,大于5cm和/或小于10cm,或甚至小于8cm。
组成
优选地,所述氧化物占大于90%,大于95%,大于99%或甚至基本100%的所述产品重量。
SiO2、Na2O、K2O、Fe2O3和CaO是任选的氧化物。
优选地,
80%<Al2O3<95%,
2%<SiO2<15%,
0.01%<Fe2O3<0.05%,
0.05%<Na2O+K2O<0.20%,且0.03%<Na2O<0.15%,
CaO<0.1%,
构成至100%余量的其他氧化物。
优选地,Al2O3>85%和/或SiO2<10%和/或Na2O+K2O<0.15%和/或Fe2O3<0.03%和/或CaO<0.05%和/或Na2O<0.15%和/或ZrO2<5%和/或TiO2<5%。
优选地,SiO2>3%和/或Na2O<0.12%和/或ZrO2<1%和/或TiO2<1%。
在一个实施方案中,Al2O3>90%。
优选地,SiO2>3%,优选地SiO2>5%,优选地SiO2>7%。
优选地,基于二氧化硅,小于20重量%,小于10重量%,小于5重量%,或甚至小于1重量%的二氧化硅是游离的。优选存在非游离的二氧化硅,大于90重量%或甚至基本100重量%,以耐火硅酸铝的形式,更特别地以莫来石的形式。
优选地,其他氧化物比Al2O3更不可还原(lessreducible)。它们优选选自ZrO2、TiO2、MgO和稀土元素例如Y2O3、CeO2和HfO2。
优选地,MgO<1%,优选地MgO<0.5%,优选地MgO<0.2%,优选地MgO<0.1%,优选地MgO<0.05%,优选地MgO<0.01%。
优选地,ZrO2<0.01%,或甚至ZrO2<0.005%。
优选地,TiO2<0.01%,优选地TiO2<0.004%。
微观结构
根据本发明的产品的微探针分析显示,相比总体Na2O含量大于0.15%的产品基质较少富有钠。不能被理论解释,看起来是在将板状氧化铝粒子烧制或烧结为所述基质过程中,钠扩散,而不与莫来石相互作用。
然而,令人惊奇地本发明人已发现在所述基质中存在特别地最小含量的Na2O对于挠曲强度是有利的。
优选地,在一方面氧化铝的总量和另一个方面莫来石和/或尖晶石和/或莫来石-氧化锆的总量,优选氧化铝的总量和莫来石的总量基于烧结的耐火产品的总量大于95%,优选大于99%,或甚至基本100%。
优选地,莫来石的量大于10%,大于20%,大于30%和/或小于50%,小于40%。
莫来石的存在对于在燃气轮机中的应用是特别有利的。优选地,所述莫来石是电熔莫来石。
优选地,氧化铝(Al2O3相)的量大于50%,大于55%,大于60%和/或小于80%,小于70%。
开孔率优选小于20体积%,和/或优选大于10体积%,或甚至大于15体积%。由此提升对热冲击和热循环的抗性。
有利地,使用水银测孔计测得的孔径分布是如此的以使:
-P50大于1μm,大于5μm,大于10μm,和/或小于20μm,小于15μm,优选地10-20μm,和/或
-P80大于10μm,大于20μm,大于25μm,和/或小于50μm,小于40μm,或甚至小于35μm,和/或
-P90大于30μm,大于40μm,大于45μm,和/或小于70μm,小于60μm,或甚至小于55μm。
聚集体
大于45%的聚集体的量的存在有利地提升了热冲击抗性。
所述聚集体占大于50%,大于55%和/或小于85%,小于80%,小于70%,小于60%的所述产品重量。
组成
优选地,所述聚集体对于大于90重量%,大于95重量%,或甚至基本100重量%由莫来石粗粒(大约72-80%Al2O3/20-28%SiO2)组成和/或由几乎纯的氧化铝粗粒(>99.5%Al2O3)组成,特别地由板状氧化铝组成,和/或由尖晶石粗粒组成和/或由莫来石-氧化锆粗粒组成。
优选地,产品的大于80%,大于90%,大于95%或甚至基本100%的莫来石和/或尖晶石(MgAl2O4)和/或莫来石-氧化锆(37重量%ZrO2;17重量%SiO2;46重量%Al2O3)存在于聚集体中。
基于产品的重量,在聚集体中Na2O+K2O的含量,优选Na2O的含量,优选小于0.14重量%,优选小于0.12重量%,优选小于或等于0.11重量%,或甚至小于0.09重量%。
基于聚集体的重量,在聚集体中Na2O+K2O的含量,优选Na2O的含量,优选在氧化铝聚集体特别地板状氧化铝聚集体中的含量,优选小于0.070重量%,优选小于0.050重量%,优选小于0.040重量%,优选小于0.030重量%。有利地,非常纯的聚集体赋予提升的性能。
优选地,大于90重量%,大于95重量%,或甚至基本100重量%的产品的SiO2在聚集体中,优选在粗莫来石粒子中。这特别暗示了在旨在制备根据本发明的产品的原料中很少或不使用粘土。
粒度分布
优选地,聚集体的百分位数D90小于5mm,优选小于3mm,优选小于2mm,优选小于1mm和/或大于0.2mm,优选大于0.3mm,优选大于0.4mm。
聚集体的粒度中值D50优选小于2mm,优选小于1mm和/或大于0.2mm,优选大于0.3mm。
基质
组成
基质对于大于95重量%或甚至基本100重量%优选由氧化铝,优选板状和/或煅烧氧化铝组成。优选地,所述基质基本不包含硅。
基于产品的重量,Na2O在基质中的含量大于优选大于0.015重量%,优选大于0.020重量%,和/或优选小于0.14重量%,优选小于0.1重量%,优选小于0.09重量%,优选小于0.08重量%。这样的Na2O含量范围使有可能在经济的烧结条件(大气压力,下降的温度,通常在小于1700℃的温度下,或甚至小于或等于1650℃的温度下,在氧化氛围中,优选在空气中,在间歇或连续式炉中)下得到具有满意的热机械性能的产品。
粒度分布
尺寸小于或等于100μm且大于10μm的粒子优选占大于10%,大于15%和/或小于25%,小于20%的产品重量。
尺寸小于或等于10μm的粒子优选占大于10%,大于15%或甚至大于20%和/或小于30%,小于27%的产品重量。
制备过程
步骤a)至e)是通常用于制备烧结的产品的步骤。
在步骤a)中,原料包含由超细颗粒、细颗粒和粗颗粒组成的氧化物的颗粒混合物。
本领域技术人员充分知道测定原料中氧化物的量作为它们在将被制备的产品中的含量的函数的方法。特别地,本领域技术人员知道原料中存在的耐火氧化物发现于烧结的耐火产品中。然而,对于同一耐火产品,原料的组成可不同,特别地作为原料中存在的添加剂的量和性质的函数。
优选地,基于原料的氧化物,原料包含:
-大于10重量%,优选大于20重量%和/或小于35重量%,小于30重量%,或甚至小于25重量%的煅烧氧化铝和/或活性氧化铝,和/或
-大于30重量%,大于35重量%,大于40重量%和/或小于55重量%,小于50重量%或甚至小于45重量%的板状氧化铝。
煅烧和/或活性氧化铝的存在有利地使有可能限制烧结温度。
基于氧化物,原料优选包含大于1重量%,优选大于1.5重量%的尺寸小于2mm的板状氧化铝颗粒。
优选地,基于氧化物,原料包含小于1重量%的MgO,更优选不含MgO,除杂质的形式外,以小于0.5%,优选小于0.2%的含量。所述过程由此简化。
粗粒部分
基于原料的氧化物,以重量百分率计,板状氧化铝的粗颗粒,或甚至所有的粗颗粒,具有小于1500ppm,优选小于1000ppm和优选小于500ppm的Na2O+K2O,优选Na2O的重量含量。不被该理论束缚,本发明人认为该低的含量阻止将导致不利相的反应。
Fe2O3粗颗粒的平均重量含量优选小于500ppm,或甚至小于300ppm。
基于原料的氧化物,所述粗粒部分优选包含:
-大于重量10%,大于15重量%,大于20重量%,和/或小于45重量%,小于35重量%,小于30重量%,或甚至小于25重量%的氧化铝颗粒,优选板状氧化铝颗粒,和/或
-大于1重量%,优选大于5重量%,大于15重量%,大于25重量%,大于30重量%和/或小于45重量%,小于40重量%的莫来石颗粒。
所述粗颗粒优选具有小于2mm的尺寸。
细粒部分
基于原料的氧化物,所述细粒部分优选包含大于1重量%,大于5重量%,大于10重量%,大于15重量%,和/或小于25重量%,小于20重量%的板状氧化铝颗粒,所述颗粒优选具有大于10μm且小于100μm的尺寸。
基于原料的氧化物,所述超细部分优选包含大于5重量%,优选大于10重量%,优选大于15重量%,优选大于20重量%和/或小于30重量%,小于25重量%的煅烧或活性氧化铝颗粒。
优选地,所有的煅烧氧化铝颗粒和/或活性氧化铝颗粒的粒度中值D50小于10μm,优选小于5μm和/或大于1微米,优选大于2μm。
添加剂
原料也可包含一种或多种添加剂,任选以颗粒形式,通常用于在成形步骤b)的过程中赋予原料充分塑性和用于赋予预制品充分的机械强度。添加剂的量是不限制的。特别地,在已知的烧结过程中传统使用的量是合适的。然而,选择添加剂以使它们的组分,和特别地它们的碱金属和碱土金属含量,与本发明的耐火产品的制备相适合。
可通过添加剂引入某些氧化物。作为可被使用的添加剂的实例,可非限制性地提及:
-临时(即,在干燥和烧制步骤中完全或部分消除)有机粘结剂,例如树脂,纤维素或木质素的衍生物,例如羧甲基纤维素和葡聚糖,和聚乙烯醇,等,优选地,临时粘结剂的量相对于原料的氧化物的颗粒混合物的重量为0.1重量%至6重量%;
-化学粘结剂,例如磷酸或单磷酸铝;
-水硬性粘结剂,如高铝水泥,例如SECAR71水泥或CaO铝酸盐型水泥;
-反凝剂,例如碱金属多磷酸盐或甲基丙烯酸酯衍生物;
-烧结促进剂,例如二氧化钛(以不超过约2%的原料的重量的比例)或氢氧化镁;
-成形剂,例如硬脂酸镁或硬脂酸钙;
-天然硅-铝酸盐型添加物,例如粘土,或合成硅-铝酸盐型添加物。这些添加物,特别地天然粘土,可引入氧化铝、氧化硅和一些碱金属和碱土金属氧化物或甚至铁氧化物。
在原料中,通常添加水。基于氧化物的颗粒混合物,添加水的量优选小于5%,小于4%,或甚至小于3%。
继续原料中多种成分的混合直至得到基本均匀的原料。
在步骤b)中,将原料放置在模具中,然后压紧,优选通过振动和/或按压和/或捣实,以形成预制品。
在通过按压成型的情况下,400-800kg/cm2的单位压力适合用于得到无塑性糊状物。所述按压优选单向或等压实施,例如通过液压机实施。通过手动或气动冲压操作和/或振动操作将是有利的。
在步骤d)中,优选在空气中或控制湿度的气氛中实施干燥,优选在环境温度至200℃的温度下。优选持续所述干燥直至预制品残留的水分小于0.5%,通常在10小时至一周之间,取决于预制品的规格。
在步骤e)中,烧制所述干燥的预制品以使其被烧结。烧结操作对本领域技术人员是周知的。烧结对应于材料的热固结。其通常伴随孔隙率的下降和尺寸的收缩。
烧结温度取决于原料的组分。优选1300℃-1800℃之间的温度。优选在氧化性气氛中更优选在空气中实施烧结。优选在大气压力下实施。烧制的持续时间,优选从冷至冷约1-15天,不仅根据将被制备的耐火产品的尺寸和形状还根据材料而变化。
步骤e)将预制品转化为根据本发明的耐火产品,特别有用于作为工业厂房燃烧室的耐火瓷砖。
不像原位烧结(即在已被放置在它们工作位置后烧结,例如已被喷射在将被保护的墙上后烧结)的产品,根据本发明的产品优选在被放置在其工作位置之前在窑中烧结,以使其各面基本以相同的方式加热。因此阻止了所述温度梯度对在对块体外表面考虑下的点的依赖。不像原位烧结的产品,根据本发明的产品因此具有贯穿整个产品均匀的密度和微观结构,这使有可能在运行中限制局部热机械应力和腐蚀、侵蚀或凹处的点,并因此增加产品的使用寿命。
应用
燃气轮机的侧壁通常包含多个被组装的块体,优选以瓷砖的形式。
为了形成该侧壁,可直接使用根据本发明的产品或可根据本领域技术人员周知的技术通过适当的伸缩接头组装根据本发明的产品。
实施例
提供下面的实施例用于说明的目的且不限制本发明。根据上述步骤a)至e)制备它们。更具体地,将原料在Eirich型混合器中混合。单向按压由此得到的原料以得到大小为210×200×40mm3的预制品,其相对干密度大于95%。在空气中在1630℃下实施烧结。
对于实施例2-4,所述聚集体由板状氧化铝(由Almatis提供,T60/T64等级,Na2O含量为1800-3000ppm,即0.18重量%至0.3重量%)和由WashingtonMills提供的电熔莫来石10F组成。在实施例1中,由Almatis提供的板状氧化铝聚集体等级被对应的由Aluchem公司提供的C99LS等级(其Na2O含量为350-520ppm,即0.035重量%-0.052重量%)取代。
对比实施例3不同于实施例2之处在于其通过在成形前在混合物中使用钠溶液(苏打)而包含具有较高Na2O负载的基质。
对比实施例4不同于实施例2之处在于其包含由RTA(RioTintoAlcan)提供的非常纯的细氧化铝(PFR40/P122B)源,特别地,所述氧化铝源包含比来自实施例2的细氧化铝源(A10/A15SG)更少的Na2O。
对比实施例5不同于实施例1之处在于由于其使用的细氧化铝源与对比实施例4中使用的相同的事实而具有非常纯的基质。
对于所述实施例,聚集体占57%的产品重量,至100%的余量按照定义由基质组成。
下面的表格示出原料,得到的产品的特性和得到的结果。
根据ISO5017标准在大小为20×20×80mm3取自块体核心的试样上测试样品的密度和开孔率。
通过电感耦合等离子体(ICP)发射光谱测量氧化物Na2O、CaO、K2O、MgO、ZrO2、Fe2O3和其他次要氧化物的重量含量,通过X射线荧光(XRF)光谱测量SiO2含量和Al2O3含量。
在空气中对大小为80×20×20mm3的试样测量其20℃下的断裂模量(MOR20℃)。三点弯曲夹具被装配为两个较低支撑物之间的距离为60mm且冲压机的下降速率等于0.5mm/min。值为三次连续测试的平均值。
在空气中对大小为80×20×20mm3的试样测量其1200℃或1400℃下的断裂模量(MOR1200℃和MOR1400℃)。三点弯曲夹具被装配为两个较低支撑物之间的距离为70mm且冲压机的下降速率等于0.5mm/min。值为三次连续测试的平均值。
根据标准化的PREIII.26/PRE/R.1.78测试测量挠曲强度相对损失(MOR损失)。该测试使有可能通过在一个或多个循环后的挠曲强度相对损失(MOR)确定热冲击行为,所述循环包括将试样从环境温度加热至1200℃的温度,将试样在该温度下保持30分钟,然后将所述试样浸入冷水淬火槽中。根据上述方案测量热冲击前后的MOR值。挠曲强度相对损失是这些MOR值间的差异与在应用热冲击之前的MOR值的比率。
蒸汽氧化测试使有可能内在评估在燃气轮机应用条件下产品的行为。所述氧化测试在1400℃下在蒸汽中以32kg/m3/h的恒定生产量实施500h。通过测试健全样品(soundsample)和已经经受氧化测试的样品间的挠曲强度相对损失得到耐腐蚀性。
根据本发明的实施例1在20℃下的MOR大于10MPa且提供对于三次热冲击后残余MOR和1400℃下MOR的最好结果,同时保持良好的耐腐蚀性。在该实施例中,基于产品的重量,聚集体中的Na2O含量小于0.09重量%,基于聚集体的重量,板状氧化铝聚集体中的Na2O含量小于0.05重量%。在一方面实施例1和另一方面实施例2和3的比较显示降低Na2O含量是优选的。
具有非常低Na2O含量的基质的实施例4在三次热冲击后具有比来自根据本发明实施例1的产品(其具有较纯的聚集体)显著更低的残余MOR。实施例1和4的比较因此显示了优选纯化聚集体而不是基质。
不像实施例1,对比实施例5具有含小于0.010%的Na2O的基质。这导致较高的开孔率和较低的20℃下的MOR。20℃下的MOR和三次热冲击后残余的MOR对于目标应用是太低的。
正如现在清楚显示的,本发明提供非常好地适合目标应用且特别地适合燃气轮机的产品。
然而本发明不限于该应用。
Claims (15)
1.一种烧结的耐火产品,其具有块体形状且由如下物质组成:
-聚集体,其由尺寸大于100μm称为“粗粒”的所有粒子形成,和
-基质,其粘合所述粗粒且由尺寸小于或等于100μm的粒子组成,所述聚集体占所述产品的45重量%至90重量%,
所述产品具有基于氧化物的如下重量百分数的组成:
-Al2O3>80%,
-SiO2<15%,
-Na2O<0.15%,
-Fe2O3<0.05%,
-CaO<0.1%,
-其他氧化物,其构成至100%的余量,
基于所述产品的重量,基质中Na2O的含量大于0.010重量%。
2.根据前述权利要求所述的产品,其中:
-Na2O+K2O<0.20%。
3.根据前述权利要求任一项所述的产品,其中:
-Al2O3>85%和/或
-3%<SiO2<10%和/或
-Na2O+K2O<0.15%和/或
-Fe2O3<0.03%和/或
-CaO<0.05%和/或
-ZrO2<5%和/或
-TiO2<5%。
4.根据前述权利要求任一项所述的产品,其中:
-Al2O3>90%和/或
-SiO2>7%和/或
-Na2O<0.12%和/或
-ZrO2<1%和/或
-TiO2<1%。
5.根据前述权利要求任一项所述的产品,其中基于聚集体的重量,氧化铝聚集体中Na2O的含量小于0.070重量%。
6.根据前述权利要求任一项所述的产品,其中基于结晶相的重量,在一方面氧化铝的总量和另一方面莫来石和/或尖晶石和/或莫来石-氧化锆的总量大于95重量%。
7.根据前述权利要求任一项所述的产品,其中基于结晶相的重量,莫来石的量大于10重量%且小于50重量%。
8.根据前述权利要求任一项所述的产品,其开孔率大于10体积%且小于30体积%。
9.根据前述权利要求任一项所述的产品,其开孔率小于20体积%。
10.根据前述权利要求任一项所述的产品,其中使用水银测孔计测得的孔径分布是如此以使:
-P50大于1μm并小于20μm,和/或
-P80大于10μm并小于50μm,和/或
-P90大于30μm并小于70μm。
11.根据前述权利要求任一项所述的产品,其中所述聚集体,对于大于90重量%,由粗莫来石粒子组成和/或由粗氧化铝粒子组成和/或由粗尖晶石粒子组成和/或由粗莫来石-氧化锆粒子组成。
12.根据前述权利要求任一项所述的产品,其中所述基质,对于大于90重量%,由氧化铝组成。
13.根据前述权利要求任一项所述的产品,其中尺寸小于或等于100μm且大于10μm的所述粒子占大于10%且小于30%的所述产品重量和/或尺寸小于或等于10μm的所述粒子占大于10%且小于30%的所述产品重量。
14.一种装置,其选自由燃气轮机、化学反应器、烧制支撑物和和玻璃熔炉上部结构形成的组,所述装置包括至少部分由根据前述权利要求任一项的产品形成的一个壁。
15.根据前一个权利要求所述的装置,所述化学反应器为用于制备氨或甲烷的二次重整反应器,且所述烧制支撑物为用于陶瓷部件的烧制支撑物。
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CN110475760A (zh) * | 2017-01-31 | 2019-11-19 | 法商圣高拜欧洲实验及研究中心 | 致密烧结产品 |
CN111868005A (zh) * | 2019-02-28 | 2020-10-30 | 圣戈班Tm股份有限公司 | 高氧化铝熔融铸造耐火物及其制造方法 |
CN112789256A (zh) * | 2018-12-06 | 2021-05-11 | 日本碍子株式会社 | 陶瓷烧结体以及半导体装置用基板 |
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US9758434B2 (en) * | 2015-06-01 | 2017-09-12 | Saint-Gobain Ceramics & Plastics, Inc. | Refractory articles and methods for forming same |
EP3612287A4 (en) * | 2017-04-17 | 2020-10-21 | Vesuvius USA Corporation | POROUS FIRE-RESISTANT CASTING MATERIAL, ITS USE AND MANUFACTURING |
EP3453689B1 (en) * | 2017-09-08 | 2020-08-26 | AGC Ceramics Co., Ltd. | High-zirconia electrocast refractory and method for manufacturing the same |
MX2020008329A (es) | 2018-02-09 | 2020-09-21 | Vesuvius Usa Corp | Composiciones refractarias y capas de barrera antioxidante in situ. |
WO2020006068A1 (en) * | 2018-06-29 | 2020-01-02 | Saint-Gobain Ceramics & Plastics, Inc. | Porous acid-resistant ceramic media |
CN109721343B (zh) * | 2019-01-17 | 2022-05-24 | 东莞信柏结构陶瓷股份有限公司 | 多孔陶瓷原料、多孔陶瓷及其制备方法与应用 |
FR3104713A1 (fr) | 2019-12-11 | 2021-06-18 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Capteur ceramique |
FR3107895B1 (fr) * | 2020-03-03 | 2022-12-23 | Saint Gobain Ct Recherches | Procede de protection thermique |
JP7336626B2 (ja) | 2021-08-03 | 2023-08-31 | 京セラ株式会社 | セラミック焼結体、セラミック基板、実装用基板、電子装置及びセラミック焼結体の製造方法 |
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CN110475760A (zh) * | 2017-01-31 | 2019-11-19 | 法商圣高拜欧洲实验及研究中心 | 致密烧结产品 |
CN112789256A (zh) * | 2018-12-06 | 2021-05-11 | 日本碍子株式会社 | 陶瓷烧结体以及半导体装置用基板 |
CN112789256B (zh) * | 2018-12-06 | 2022-11-08 | 日本碍子株式会社 | 陶瓷烧结体以及半导体装置用基板 |
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CN111868005B (zh) * | 2019-02-28 | 2022-05-31 | 圣戈班Tm股份有限公司 | 高氧化铝熔融铸造耐火物及其制造方法 |
Also Published As
Publication number | Publication date |
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FR3008967A1 (fr) | 2015-01-30 |
US20160185666A1 (en) | 2016-06-30 |
EP3024799B1 (fr) | 2018-10-03 |
JP6607575B2 (ja) | 2019-11-20 |
WO2015011623A1 (fr) | 2015-01-29 |
US10167233B2 (en) | 2019-01-01 |
JP2016532623A (ja) | 2016-10-20 |
EP3024799A1 (fr) | 2016-06-01 |
CN105683124B (zh) | 2017-10-27 |
FR3008967B1 (fr) | 2016-12-30 |
MX2016001140A (es) | 2016-04-29 |
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