CN1649805A - 钛酸铝烧结坯的制造方法 - Google Patents
钛酸铝烧结坯的制造方法 Download PDFInfo
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- CN1649805A CN1649805A CNA038094002A CN03809400A CN1649805A CN 1649805 A CN1649805 A CN 1649805A CN A038094002 A CNA038094002 A CN A038094002A CN 03809400 A CN03809400 A CN 03809400A CN 1649805 A CN1649805 A CN 1649805A
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Abstract
本发明提供了一种用于制备钛酸铝烧结体的原料组合物,该组合物包括:(i)100重量份的混合物,该混合物包括40-50mol%的TiO2和60-50mol%的Al2O3,(ii)1-10重量份的由通式(NaxK1-x)AlSi3O8 (0≤X≤1)代表的碱性长石,以及(iii)1-10重量份的至少一种选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO的含Mg组分,也提供了一种用于制备钛酸铝烧结体的方法,该方法包括在1300-1700℃的温度下烧结由原料组合物制成的成型制品。根据本发明的方法,可得到机械强度高并且可在高温下稳定使用的钛酸铝烧结体,该烧结体也具有钛酸铝所固有的低热膨胀系数和高耐腐蚀性。
Description
发明领域
本发明涉及一种用于制备钛酸铝烧结体的原料组合物、制备钛酸铝烧结体的方法以及钛酸铝烧结体。
发明背景
钛酸铝烧结体具有低的热膨胀系数和高的耐腐蚀性。它们被称为是耐热材料,当将该材料用作例如铝、铝合金、铁合金等熔融金属的容器、抬包或槽时,该材料具有与熔渣的低润湿性、优良的耐腐蚀性、优良的抗散裂强度和其它优良性质。但是,构成钛酸铝烧结体的晶粒是各向异性,该烧结体趋于具有以下缺点:当被加热或冷却时,热膨胀系数的各向异性产生的应力导致了晶粒晶界的位移;并且形成了微裂纹和孔,这会导致低的机械强度。
因此,常规的钛酸铝烧结体所具有的强度不足,并且特别是当施用于高温并且被施加重的载荷时,不能表现出足够的耐用性。
另外,钛酸铝在1280℃或以下的温度下不稳定。当将其用于约800-1280℃的温度范围时,该化合物具有分解成TiO2和Al2O3的趋势,因此,很难在该高温下持续使用该材料。
为了改进钛酸铝的可烧结性并且阻止其热分解,在烧结之前,将添加剂比如二氧化硅加入原材料中。但是,此时,所得到的烧结体的耐熔性趋于降低。为此,不可能得到可在高达约1400℃的温度下使用并且也具有高机械强度的耐熔性钛酸铝烧结体。
发明概述
本发明的主要目的是提供一种新的钛酸铝烧结体,该烧结体的机械强度被改进到可实际应用的水平,并且可在高温下使用,而且具有钛酸铝所固有的性质,即低的热膨胀系数和高的耐腐蚀性。
为了克服以上的问题,本发明人进行了广泛的研究。结果是,本发明人发现,当在存在特定的碱性长石和至少一种选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO的组分的条件下,将含有二氧化钛和氧化铝的原材料粉末进行烧结时,可得到机械强度被极大地改进的钛酸铝烧结体,该烧结体耐热分解并且具有高的耐熔性,而且不会损失钛酸铝所固有的低的热膨胀,原因是含Mg组分与碱性长石具有协同效果。基于该发现而完成了本发明。
具体的说,本发明提供了以下所述的用于制备钛酸铝烧结体的原料组合物、制备钛酸铝烧结体的方法以及钛酸铝烧结体。
1.用于制备钛酸铝烧结体的原料组合物,该组合物包括:
(i)100重量份的混合物,该混合物包括40-50mol%的TiO2和60-50mol%的Al2O3,
(ii)1-10重量份的由式(NaxK1-x)AlSi3O8(0≤X≤1)代表的碱性长石,以及
(iii)1-10重量份的至少一种选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO的含Mg组分。
2.根据第1项的用于制备钛酸铝烧结体的原料组合物,其中,碱性长石的组成(NaxK1-x)AlSi3O8中,x的范围是0.1≤X≤1。
3.根据第1或2项的用于制备钛酸铝烧结体的原料组合物,其中,碱性长石中的Si与含Mg组分中的Mg的摩尔比范围是Si∶Mg=0.9∶1-1.1∶1。
4.用于制备钛酸铝烧结体的方法,该方法包括在1300-1700℃的温度下烧结成型制品,
成型制品由用于制备钛酸铝烧结体的原料组合物制成,该组合物包括:
(i)100重量份的混合物,该混合物包括40-50mol%的TiO2和60-50mol%的Al2O3,
(ii)1-10重量份的由式(NaxK1-x)AlSi3O8(0≤X≤1)代表的碱性长石,以及
(iii)1-10重量份的至少一种选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO的含Mg组分。
5.根据第4项的方法制备的钛酸铝烧结体。
用于制备本发明钛酸铝烧结体的方法是这样一种方法,其中,通过将含有TiO2和Al2O3的混合物、与式(NaxK1-x)AlSi3O8(0≤X≤1)所代表的碱性长石、以及选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO的至少一种含Mg组分混合,制备出用作原材料的组合物;并且将由该组合物制备的成型制品在1300-1700℃的温度下烧结。
对作为原材料的TiO2和Al2O3没有特别的限制,只要通过烧结由这些物质可合成钛酸铝即可。它们通常选自用于制造各种陶瓷比如氧化铝陶瓷、二氧化钛陶瓷、氧化铝陶瓷等的原材料。
TiO2和Al2O3的混合比范围可以是40-50mol%的TiO2和60-50mol%的Al2O3,优选45-50mol%的TiO2和55-50mol%的Al2O3。特别是,在上述混合比范围内,将Al2O3/TiO2的摩尔比调节为1或更高可阻止液相的共存。
作为添加剂的碱性长石可由式(NaxK1-x)AlSi3O8表示,其中0≤X≤1。特别是,在上式中,优选x的范围是0.1≤X≤1,并且更优选x的范围是0.15≤X≤0.85。具有该x值范围的碱性长石具有低的熔点,并且因此特别有利于促进钛酸铝的烧结。
当Al2O3和TiO2的总量是100重量份时,使用的碱性长石量可以是约1-10重量份,优选约3-4重量份。
在本发明中,可以单独使用尖晶石结构的含Mg氧化物、MgCO3和MgO,或将它们中的两种或多种组合使用。其中,可使用的具有尖晶石结构的含Mg氧化物的实例包括MgAl2O4和MgTi2O4等。也可使用通过烧结含有MgO和Al2O3的原材料或含有MgO和TiO2的原材料而制备的尖晶石氧化物。在本发明中,可结合使用两种或多种具有尖晶石结构的氧化物。
当Al2O3和TiO2的总量是100重量份时,选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO中的至少一种含Mg组分的使用量范围是约1-10重量份,优选约3-6重量份。
在本发明的方法中,碱性长石中的Si与含Mg组分中的Mg的摩尔比范围优选是Si∶Mg=约0.9∶1-约1.1∶1,更优选的范围是Si∶Mg=约0.95∶1-约1.05∶1。
根据本发明的方法,通过将上述含Mg组分、作为添加剂的碱性长石以及含有TiO2和Al2O3的混合物混合、使该混合物成型为所需要的形状并且该烧结成型制品,可提供机械强度高、耐热分解性好并且耐熔性高的钛酸铝烧结体。
通过本发明可提供机械强度高并且耐热分解性好的钛酸铝烧结体的原因尚不清楚,但是原因可能如下:
当通过烧结合成钛酸铝时,碱性长石中的Si溶解于晶格中并且置换了Al。由于Si的半径小于Al,因此,缩短了其与临近氧原子的键合长度。因此,得到的晶体的晶格常数比纯的钛酸铝小。因此,得到的烧结体具有稳定的晶体结构,改进的机械强度和非常高的热稳定性,由此导致了耐熔性的极大改进。
另外,利用含Mg组分作为添加剂可得到致密的烧结体。因此,可形成机械强度比纯的钛酸铝高的烧结体。
根据本发明的方法,由于结合使用了具有该效果的碱性长石和含Mg组分作为添加剂,因此,认为碱性长石中的Si和含Mg组分中的Mg取代了钛酸铝中的主要的Al位置。另一方面,当单独添加这些组分中的每一种时,原来保持在它们的电荷平衡位置处的三价Al被二价元素(Mg)或四价(Si)元素取代,并且由此导致烧结体需要保持电平衡。因此,当添加Mg时,为了保持电荷平衡,使得氧似乎被从该体系中挤出,从而导致烧结体中的氧缺陷。当添加本身为四价的四价Si或Ti时,认为为了保持电荷平衡而被还原为三价。在本发明中,认为通过结合使用碱性长石和含Mg组分,可保持电荷平衡,因为Mg的电荷数比Al少1,并且Si的电荷数比Al多1,因此,这些元素可溶解在烧结体中而不会影响构成烧结体的其它元素。特别是,当这两种添加剂的量接近等摩尔时,与单独添加这些添加剂相比,预计该组合添加剂的存在更稳定。为此认为,与单独添加这些添加剂相比,由于这两种添加剂的协同作用而极大地改进了烧结体的机械强度,因此,形成的钛酸铝烧结体的高机械强度超过了实践应用水平,并且由于极大地提高了耐热分解性而具有非常高的耐熔性,同时不会损失钛酸铝所固有的低的热膨胀。
可将含有TiO2、Al2O3、碱性长石和含Mg组分的原料混合物充分混合、研磨成合适的颗粒尺寸并且接着将其成型为所需要的形状。
对原料混合物的混合和研磨工艺没有特别的限制,可以是任何已知的工艺,比如球磨、搅拌的介质研磨等方式来混合和研磨。
原料混合物的研磨程度不是关键。通常将材料研磨成约1μm或更小的颗粒尺寸,优选是尽可能小的颗粒尺寸,只要不形成二次颗粒即可。
如果需要,可将成型助剂加入原料混合物中。可根据成型方法从迄今为止所使用的成型助剂中选择这一物质。
该成型助剂的实例包括聚乙烯醇、微蜡乳液、羧甲级纤维素以及类似的黏结剂、硬脂酸乳液和类似的脱模剂、邻-辛基醇、辛基苯氧基乙醇以及类似的起泡抑制剂、二甲胺、三乙胺以及类似的抗絮凝剂。
所使用的成型助剂量并不关键,可以根据成型方法在目前的使用量范围中选择合适的成型助剂使用量。例如,当将成型助剂用于流铸时,可使用的粘结剂的量是约0.2-0.6重量份,絮凝剂的量是约0.5-1.5重量份,脱模剂(固体量)的量是约0.2-0.7重量份,并且起泡抑制剂的量是约0.5-1.5重量份,该计量基于Al2O3和TiO2的总量是100重量份。
对原料混合物的成型方法没有特别的限制,可以从比如压制成型、片铸、流铸、挤压成型、喷射成型、CIP成型等已知的成型方法中选择。
烧结温度可以是约1300-1700℃,优选约1350-1450℃。
对烧结气氛没有特别的限制,可以是迄今为止所使用的任何含氧气氛比如空气、还原气氛和惰性气氛。
对烧结时间没有特别的限制,只要制品被充分的烧结即可,这取决于成型制品的形状等。通常进行约1-10小时的烧结,在此期间维持上述温度。对烧结过程中的加热速度和冷却速度没有特别的限制,可以选择合适的速度,以使得烧结体中没有形成裂纹。
本发明方法得到的烧结体具有上述特征,例如同时具备高的机械强度和低的热膨胀系数。另外,由于烧结体稳定的晶体结构而导致其具有优良的耐热分解性以及高的耐熔性。因此,抑制了钛酸铝的分解反应,并且即使在高温比如几百到约1600℃的温度下,制品也可以被稳定的使用。对于抗弯强度而言,可得到超过约90MPa的抗弯强度,而该值是已知的钛酸铝烧结体的6倍。另外,根据本发明的方法,烧结时不产生裂纹是可行的,因此,得到的烧结体致密并且具有高的抗热冲击性。
本发明方法制备的烧结体显示出非常高的对于熔融金属的非润湿性和耐腐蚀性。因此,其显示出如此优异的对于熔融金属流的耐腐蚀性,这样的性能从熟知的材料中是不可预期的。
由本发明方法制备的具有上述优良特性的钛酸铝烧结体可用于各种应用中,例如,高熔点金属的容器比如熔化金属用的坩埚、抬包和槽;飞机的喷气式发动机的高温部分的组件;喷嘴;各种内燃式发动机的高温部分比如电热塞、气缸和活塞头;太空船外壁所使用的绝缘板或屏蔽板等。另外,在LSI制造工艺中,可将其低膨胀性用于印刷过程用表面板中。
由以上可以看出,由本发明方法制备的钛酸铝烧结体具有高的机械强度和抗热冲击性,同时保持钛酸铝所固有的低的热膨胀系数。另外,钛酸铝烧结体具有其优良的耐热分解性,显示出高的耐熔性并且可在高温下稳定的使用。
附图说明
图1表示在1000℃的气氛中,本发明钛酸铝烧结体中的剩余钛酸铝百分数随着时间的变化曲线。
实施本发明的最好方式
将参考以下的实施例更详细地描述本发明。
实施例1
在含有43.9重量%(50mol%)的锐钛矿型二氧化钛和56.1重量%(50mol%)的可烧结α-氧化铝的100重量份的混合物中,加入4重量份的式(Na0.6K0.4)AlSi3O8所表示的碱性长石、6重量份的式MgAl2O4表示的尖晶石、0.25重量份作为粘结剂的聚乙烯醇、1重量份的作为抗絮凝剂的二乙胺以及0.5重量份的作为发泡抑制剂的聚丙烯醇。利用球磨混合该混合物达3小时,并且接着利用干燥器在120℃下干燥12小时或更长,由此得到原材料粉末。
将得到的原材料粉末研磨至约150目,并且在60MPa的压力下压制成型,由此得到大小为100mm×100mm×10mm的成型制品。
在气氛中按照以下的加热方式对成型制品进行烧结,并且之后放置以冷却,由此得到钛酸铝烧结体。
(加热方式)
经过6小时使温度从0到180℃
在180℃下保持4小时(水蒸发)
经过4小时使温度从180到340℃
在340℃下保持4小时(有机粘结剂的燃烧)
经过4小时使温度从340到700℃
在700℃下保持2小时(残余的碳燃烧)
经过4小时使温度从700到1400℃
在1400℃下保持4小时
从得到的烧结体上切出5mm×5mm×20mm的样品。将样品的表面抛光,并且在20℃/min的加热速度下测量了样品的热膨胀系数。结果示于下表1中。
表1
温度(℃) | 热膨胀百分数(ΔL/L)% | 热膨胀系数平均值(×10-7/K) |
126 | -0.016 | -15.55 |
226 | -0.029 | -14.26 |
326 | -0.036 | -12.13 |
426 | -0.040 | -10.10 |
526 | -0.039 | -7.87 |
626 | -0.033 | -5.47 |
726 | -0.014 | -2.07 |
826 | 0.012 | 1.55 |
926 | 0.035 | 3.85 |
由以上的结果可以看出,本发明方法得到的烧结体具有低的热膨胀系数,并且保持了钛酸铝所固有的低的热膨胀系数。
实施例2
除了按照以下的加热方式进行烧结之外,利用与实施例1相同的原材料和相同的方式得到了钛酸铝烧结体。
(加热方式)
经过6小时使温度从0到180℃
在180℃下保持4小时(水蒸发)
经过4小时使温度从180到340℃
在340℃下保持4小时(有机粘结剂的燃烧)
经过4小时使温度从340到700℃
在700℃下保持2小时(残余的碳燃烧)
经过4小时使温度从700到1350℃
在1350℃下保持4小时
从得到的钛酸铝烧结体上切出3mm×4mm×40mm的样品。将样品的表面抛光,并且测量了样品的三点抗弯强度。
为了比较,制备了两个对比样:除了没有使用尖晶石并且4重量份的碱性长石被用作唯一的添加剂之外,利用与实施例1相同的原材料配方、按照与实施例2相同的烧结方式(烧结温度:1350℃)得到的烧结体(对比实施例1);除了没有使用碱性长石并且6重量份的尖晶石被用作唯一的添加剂之外,利用与实施例1相同的原材料配方、按照与实施例2相同的烧结方式(烧结温度:1350℃)得到的烧结体(对比实施例2)。按照相同的方式测量了烧结体的三点抗弯强度。
表2
样品名称 | 三点抗弯强度(Mpa) |
实施例2(添加了长石和尖晶石 | 85.7 |
对比实施例1(添加了长石) | 56.0 |
对比实施例2(添加了尖晶石) | 30.3 |
由以上的结果可以看出,通过同时添加碱性长石和尖晶石而得到的实施例2的钛酸铝烧结体、比添加碱性长石或尖晶石中的一种时得到的对比实施例1和对比实施例2烧结体的机械强度高。
另外,从实施例2、仅添加了长石而得到的对比实施例1以及仅添加了尖晶石而得到的对比实施例2中的每一个切出10mm×10mm×10mm的测试样品。将样品放置在1000℃的气氛中,通过X-射线衍射来确定剩余的钛酸铝百分数随着时间的变化。通过测量金红石的(110)和(101)面的衍射强度来计算剩余的钛酸铝百分数,并且由其总面积来确定金红石的量,因为钛酸铝分解成了氧化铝和金红石。
另外,除了既不添加尖晶石也不添加碱性长石之外,利用与实施例1相同的原材料配方、按照与实施例1相同的烧结条件(烧结温度:1400℃)得到了一种烧结体,也按照相同的方式测试了该烧结体剩余的钛酸铝百分数随着时间的变化。结果示于图1中。
由图1可以看出,当实施例2的钛酸铝烧结体被放置在高温下达长的时间段之后,该烧结体很难分解成Al2O3和TiO2。这证实了该烧结体具有优良的耐热分解性。
Claims (5)
1.一种用于制备钛酸铝烧结体的原料组合物,该组合物包括:
(i)100重量份的混合物,该混合物包括40-50mol%的TiO2和60-50mol%的Al2O3,
(ii)1-10重量份的由通式(NaxK1-x)AlSi3O8(0≤X≤1)代表的碱性长石,以及
(iii)1-10重量份的至少一种选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO的含Mg组分。
2.根据权利要求1的用于制备钛酸铝烧结体的原料组合物,其中碱性长石具有这样的组成,在通式(NaxK1-x)AlSi3O8中x的范围是0.1≤X≤1。
3.根据权利要求1或2的用于制备钛酸铝烧结体的原料组合物,其中碱性长石中的Si与含Mg组分中的Mg的摩尔比范围是Si∶Mg=0.9∶1-1.1∶1。
4.一种用于制备钛酸铝烧结体的方法,该方法包括在1300-1700℃的温度下烧结成型制品,
成型制品由用于制备钛酸铝烧结体的原料组合物制成,该组合物包括:
(i)100重量份的混合物,该混合物包括40-50mol%的TiO2和60-50mol%的Al2O3,
(ii)1-10重量份的由通式(NaxK1-x)AlSi3O8(0≤X≤1)代表的碱性长石,以及
(iii)1-10重量份的至少一种选自具有尖晶石结构的含Mg氧化物、MgCO3和MgO的含Mg组分。
5.一种根据权利要求4的方法制备的钛酸铝烧结体。
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JP2002126553A JP3489030B1 (ja) | 2002-04-26 | 2002-04-26 | チタン酸アルミニウム系焼結体の製造方法 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100339307C (zh) * | 2006-01-12 | 2007-09-26 | 景德镇陶瓷学院 | 一种合成钛酸铝超细粉的方法 |
CN100371246C (zh) * | 2006-01-27 | 2008-02-27 | 王洪增 | 一种钛酸铝陶瓷材料 |
CN100402436C (zh) * | 2006-01-27 | 2008-07-16 | 王洪增 | 一种高熔聚合材料的生产工艺 |
CN102471170A (zh) * | 2009-07-15 | 2012-05-23 | 纳幕尔杜邦公司 | 钛酸铝镁复合陶瓷 |
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US20050181929A1 (en) | 2005-08-18 |
TWI276619B (en) | 2007-03-21 |
CA2482679A1 (en) | 2003-11-06 |
CN1280235C (zh) | 2006-10-18 |
US7148168B2 (en) | 2006-12-12 |
WO2003091183A1 (fr) | 2003-11-06 |
KR100956690B1 (ko) | 2010-05-10 |
EP1514857A4 (en) | 2007-05-23 |
TW200400163A (en) | 2004-01-01 |
EP1514857A1 (en) | 2005-03-16 |
USRE42646E1 (en) | 2011-08-23 |
KR20050007338A (ko) | 2005-01-17 |
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EP1514857B1 (en) | 2014-08-13 |
JP2004026508A (ja) | 2004-01-29 |
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