CN103459349B - Atz熔凝颗粒 - Google Patents

Atz熔凝颗粒 Download PDF

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Publication number
CN103459349B
CN103459349B CN201280015174.4A CN201280015174A CN103459349B CN 103459349 B CN103459349 B CN 103459349B CN 201280015174 A CN201280015174 A CN 201280015174A CN 103459349 B CN103459349 B CN 103459349B
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oxide
less
consolidation
granule
percentage
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CN103459349A (zh
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史蒂芬·拉斐尔
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Saint Gobain Centre de Recherche et dEtudes Europeen SAS
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Saint Gobain Centre de Recherche et dEtudes Europeen SAS
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Abstract

本发明公开了具有下列化学组成的熔凝颗粒：‑大于10%且小于50%的氧化铝Al2O3；‑大于10%且小于50%的氧化钛TiO2；‑大于21%且小于50%的氧化锆；‑大于1%且小于10%的选自MgO、CaO、Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3的化合物、及其混合物；‑小于20%的二氧化硅SiO2；‑小于10%的选自碱金属氧化物、碱土金属氧化物的化合物、及其混合物；‑小于2%的其他的氧化物种类，其中，所述百分比为基于氧化物的重量百分比。本发明还公开了所述熔凝颗粒在熔化金属中的用途。

Description

ATZ熔凝颗粒
技术领域
本发明涉及一种基于氧化铝、氧化钛和氧化锆的熔凝颗粒、涉及一种用于生产这种颗粒的方法、涉及一种包含这种颗粒的烧结制品、和涉及一种用于将这种烧结制品与熔融金属接触的用途。
背景技术
为了能够在这种用途中使用，陶瓷烧结制品必须具有与熔凝金属接触时优良的机械强度、优良的抗热冲击性和优良的抗腐蚀性。为了该目的，选择用于生产该制品的颗粒是决定性因素。
特别地，在钢铁的连续浇铸中尤其使用滑动闸门，以便通过连铸水口或滑动水口，打开或关闭与铸锭模具流体连通的钢水包的浇铸盘或排放孔。
通常，通过烧结刚玉、熔凝的氧化锆-莫来石颗粒和可选的熔凝的氧化铝-氧化锆颗粒的混合物来获得滑动闸门。
EP 1 820 785描述了一种通过烧结包括熔凝颗粒的混合物来制造的滑动闸门，该熔凝颗粒具有重量百分比在10％和50％之间的氧化铝Al2O3、重量百分比在10％和40％之间的TiO2和重量百分比大于50％的氧化锆。
经常需要能够在与熔融的金属接触的烧结制品中、尤其在滑动闸门中使用的新的颗粒，该颗粒具有改进的机械性能以及优良的抗热冲击性。本发明的一个目的是满足该需要。
发明内容
根据本发明，通过一种熔凝颗粒实现了该目的，以总量为100％计，百分比为基于氧化物的重量百分比，该熔凝颗粒包括：
-大于10％，优选大于15％，且小于50％，优选小于35％的氧化铝Al2O3；
-大于10％，优选大于15％，且小于50％，或小于45％，或小于40％，或小于35％的氧化钛TiO2；
-大于21％，优选大于25％，且小于50％，优选小于45％的氧化锆(ZrO2+痕量HfO2)；
-大于1％，优选大于1.5％，优选大于2％，优选大于2.5％，且小于10％，小于9％，优选小于8％的选自由MgO、CaO、Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3及其混合物组成的组的化合物；
-小于20％的二氧化硅SiO2；
-小于10％，优选小于5％，小于4％，或小于3％的选自由碱金属氧化物、碱土金属氧化物及其混合物组成的组的化合物，尤其是选自由元素Sr的氧化物、元素Na的氧化物、元素K的氧化物、元素Ba的氧化物及其混合物组成的组的化合物；
-小于2％的其他的氧化物种类。
根据本发明的熔凝颗粒也可具有下列特征中的一个或多个特征：
-MgO的重量百分比含量为大于1％，优选大于1.5％，和/或小于9％，优选小于8％；
-CaO的重量百分比含量为大于0.5％，或大于0.7％，大于1％，大于1.5％，和/或小于9％，或小于8％，或小于5％，或小于3％；
-Y2O3的重量百分比含量为大于0.5％，或大于0.7％，大于1％，大于1.5％，和/或小于8％，或小于5％，或小于3％；
-同时存在MgO、CaO和Y2O3；
-Cr2O3+MnO2+La2O3+Ga2O3的含量为小于1％，或小于0.5％；
-属于铁、钒、和铬的氧化物、氮化物、氮氧化物、碳化物、碳氧化物、碳氮化物、和金属种类的化合物为杂质；
-每种所述碱金属氧化物和/或碱土金属氧化物的含量为小于4％，或小于3％，或小于1％；
-属于钠和其它碱金属的氧化物、氮化物、氮氧化物、碳化物、碳氧化物、碳氮化物、和金属种类的化合物为杂质；
-二氧化硅的含量为大于0.1％，大于1％，大于2％，和/或小于18％，小于15％，小于12％，小于10％。
本发明还涉及一种包含根据本发明的颗粒或甚至由根据本发明的颗粒组成的粉末，且涉及这种粉末的用于生产滑动闸门或熔炉(如，感应炉)的衬套的用途，尤其是用于熔化金属的用途。特别地，该粉末可以是干式捣打料类型或“DVC”类型、干式振动料类型或干式耐火材料类型。
根据本发明的颗粒的粉末可以具有大于2μm，大于5μm，或大于10μm，或大于50μm，和/或小于8mm，小于7mm，小于5mm，小于3mm，小于2mm，小于1mm，或小于500μm的中值粒径(d50)。
本发明还涉及一种通过烧结根据本发明的粉末或烧结包含至少一种根据本发明的粉末且具有不同的中值粒径的粉末的混合物而获得的烧结制品，该烧结制品尤其是衬套或滑动闸门的形式。
优选地，根据本发明的烧结制品具有小于30％，小于20％，或小于15％的开孔孔隙度。
本发明也涉及一种用于生产根据本发明的熔凝颗粒的粉末的方法，该方法包含下列连续的步骤：
a)混合原材料，以便形成给料，
b)熔化所述给料，直到获得熔融的材料，
c)固化所述熔融的材料，
d)可选地，尤其是如果步骤c)未产生所获得的颗粒，则研磨所述固体，以便获得颗粒的粉末。
根据本发明，在步骤a)中选择原材料，使得在步骤c)结束时获得的固体具有与根据本发明的颗粒一致的组成。
最后，本发明涉及根据本发明的烧结制品的用途，或根据本发明的方法获得的烧结制品的用途，尤其是以衬套或滑动闸门的形式的烧结制品的用途，在该用途中，烧结制品经受热冲击、和/或与熔融的金属接触。特别地，本发明涉及一种选自包含烧结制品的熔炉和包含烧结制品的滑动闸门的装置，该烧结制品通过烧结根据本发明的颗粒的粉末而获得，尤其是在一个区域中，所述烧结制品用于与熔融的金属接触。
定义
-在本说明书和权利要求书中，除非另有说明，所有的百分比为重量百分比。尤其是，颗粒的所有组分按照基于颗粒的氧化物的重量百分比给出。
-“熔融的材料”为液体，为了保持其形状，该液体必须被保留在容器内。熔融的材料可以包含一些固体微粒，但这些固体微粒的含量不足以能够构成所述相。
-“其他的氧化物种类”表示所有的未被提及的氧化物，即，除了Al2O3、TiO2、ZrO2、HfO2、MgO、CaO、Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3、SiO2、和碱金属氧化物、和/或碱土金属氧化物之外的氧化物。
-术语“杂质”应该被理解成通过原材料无意引入或来源于这些组分的反应的不可避免的组分。杂质为不必要的组分，但仅仅是可容忍的组分。
-术语“氧化锆”指的是氧化锆ZrO2和在化学上与ZrO2不可分离且总是天然地存在于ZrO2源中的痕量氧化铪HfO2。这些痕量的HfO2占氧化锆的重量小于2％。氧化铪既不被认为是杂质，也不被认为是“其它的氧化物种类”。
-通常由d50表示的颗粒的粉末的“中值粒径”词语是指，将这种粉末的颗粒划分成在体积上是相等的第一群体和第二群体的直径，这些第一群体和第二群体仅包含分别具有大于或小于中值粒径的直径的颗粒。词语“颗粒的直径”被理解意味着相同体积的球体的直径。按照惯例，通过利用激光粒度分析仪进行的粒度分布表征来评估粉末的颗粒直径。例如，激光粒度分析仪可以是来自HORIBA公司的Partica LA-950。
术语“颗粒”是指具有小于10mm的直径的微粒。
具体实施方式
出于说明的目的提供以下描述，以下描述不限制本发明。
根据前面提及的步骤a)至步骤d)可以制造根据本发明的熔凝颗粒。
在步骤a)中，按照惯例量出原材料，以便获得所需的组成，然后混合，以便形成给料。
可以以任何形式引入钛，尤其是以氧化物TiO2的形式、或以金属形式、或以氧化锆-氧化钛合金或钛酸铝的形式引入钛。
在一个实施方式中，碱金属氧化物和碱土金属氧化物为杂质。
可以认为，小于2％的“其它的氧化物种类”的含量不抑制由发明提供的技术效果。“其它的氧化物种类”也可以是杂质。
优选地，杂质的含量为小于3％，小于2％，小于1％，或小于0.5％。
在步骤b)中，优选使用电弧炉，但可以构思所有已知的熔炉(例如，感应炉或等离子体炉)，条件是它们可以完全熔化给料。优选地，在中性条件(例如，在氩气下)或氧化条件下，优选在大气压力下，进行烧制。
在步骤c)中，可快速冷却，即，使得在小于3分钟内完全固化熔凝材料。例如，可以由如在US 3,993,119中描述的浇铸到CS(碳钢)模具中或由淬火产生冷却。冷却也可以是缓慢的(露天冷却的铸锭或退火块)。
如果步骤c)不能够获得颗粒的粉末，或如果对于预期用途，这些颗粒没有合适的粒径，则可以根据常规的技术进行研磨(步骤d)。
由根据本发明的颗粒的粉末可以通过任何已知的方法来生产根据本发明的烧结制品。
实施例
以说明的方式提供下列的实施例，这些实施例不限制本发明的范围。
在所有实施例中，由下面的原材料制备样品：
-由Altichem公司出售的含有大于98％的TiO2的锐钛矿，或由EuropeMinerals公司出售的含有大于95％的TiO2且具有大约120μm的中值粒径d50的金红石，
-由Alcan公司出售的含有大于98％的Al2O3且具有大约85μm的中值粒径d50的矾土AR75，
-由Sifraco公司出售的具有大于99.5％的纯度且具有208μm的中值粒径d50的二氧化硅SiO2，
-由Nedmag公司出售的具有大于98％的纯度的氧化镁MgO，大于80％的该微粒具有在0.25mm和1mm之间的直径，
-由Saint-Gobain ZirPro公司出售的标号为“CC10”的具有大于98.5％的纯度且具有3.5μm的中值粒径d50的氧化锆。
量出原材料，将其混合，以便制成具有适当组成的给料。
对于实施例3的样品的制备，给料被挤压，以便制成具有13mm直径和13mm高度的圆盘的形式的预成型体。
对于实施例1、实施例2和实施例4的样品的制备，在电氧化、空气的条件下，在电弧炉中将给料熔化，然后冷却。然后，研磨和筛选所获得的固体，以便获得具有在10μm和15μm之间的中值粒径(d50)的粉末。
熔凝颗粒的粉末被挤压，以便制成类似于实施例3的圆盘的形式的预成型体。
然后，在1450℃的温度下，对所有的圆盘烧结4小时。从而获得实施例1至实施例4的样品。
然后，分析所制备的样品。结果汇总在表1中。
通过X射线荧光法测定按照基于氧化物的质量百分比指出的化学组成。
按照惯例，利用氦比重瓶测定法，通过对经研磨的样品测量几何密度和绝对密度来测定孔隙度(P)。
在50℃和600℃之间测量膨胀系数“a”。
在室温下，以常规方式对样品1至样品4测定抗压强度“b”。
表1
*：比较实施例
表1表明，根据本发明的颗粒(实施例2)导致了具有特别高的机械强度的烧结制品。
实施例2和实施例3的比较显示出通过熔化所获得的的颗粒的优点，该颗粒被称为“熔凝”颗粒。这是因为，给料的熔化导致了更好的机械强度和更低的孔隙度，使得可以限制腐蚀和/或渗透。
表1表明，根据本发明的颗粒具有的膨胀系数“a”低于实施例4*、或低于熔凝的莫来石-氧化锆颗粒(膨胀系数“a”大约为7×10-6C-1)、或低于熔凝的氧化铝-氧化锆颗粒(膨胀系数“a”大约为10×10-6C-1)的膨胀系数“a”。这使得可以获得具有更好的抗热冲击性的制品。
通过X射线衍射法来表征在实施例2的样品中存在的结晶相。观测到主相，该主相由固溶体中的伪板钛矿型的氧化物相构成，伪板钛矿型类型的相包括一定比例的钛、铝、镁和锆使得伪板钛矿型的相基本上符合式(Al2TiO5)x(MgTi2O5)y(MgTiZrO5)z，其中，0.1≤x<1，0<y≤0.9，且z＝1-x-y。也观测到硅酸盐相和基本上由氧化钛和氧化锆组成的另一种相。
此外，利用X射线衍射法，通过在实施例2的样品中初始存在的结晶相与在800℃下经过热处理100小时后在该同一样品中存在的结晶相的比较测试，检验了存在的结晶相的稳定性。
显然，本发明提供了一种适用于与熔凝金属接触的烧结制品中有效使用的颗粒。
当然，本发明不限于出于说明的目的所提供的实施例的实施方式。

Claims (15)

1.一种具有下列化学组成的熔凝颗粒，以总量为100％计，以基于氧化物的重量百分比计：
-大于10％且小于50％的氧化铝Al2O3；
-大于10％且小于50％的氧化钛TiO2；
-大于21％且小于50％的氧化锆；
-大于1％且小于10％的选自由MgO、CaO、Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3及其混合物组成的组的物质；
-小于20％的二氧化硅SiO2；
-小于10％的选自由元素Sr的氧化物、元素Na的氧化物、元素K的氧化物和元素Ba的氧化物及其混合物组成的组的物质；
-小于2％的其他的氧化物种类。
2.根据权利要求1所述的熔凝颗粒，所述熔凝颗粒以基于氧化物的重量百分比计包括：
-大于15％的氧化铝Al2O3；和/或
-大于15％的氧化钛TiO2；和/或
-大于25％的氧化锆；
-大于1.5％的选自由MgO、CaO、Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3及其混合物组成的组的物质；和/或
-小于5％的选自由元素Sr的氧化物、元素Na的氧化物、元素K的氧化物和元素Ba的氧化物及其混合物组成的组的物质。
3.根据权利要求1所述的熔凝颗粒，所述熔凝颗粒以基于氧化物的重量百分比计包括：
-小于35％的氧化铝Al2O3；和/或
-小于45％的氧化钛TiO2；和/或
-小于45％的氧化锆；和/或
-小于9％的选自由MgO、CaO、Fe2O3、Cr2O3、MnO2、La2O3、Y2O3、Ga2O3及其混合物组成的组的物质；和/或
-小于4％的选自由元素Sr的氧化物、元素Na的氧化物、元素K的氧化物和元素Ba的氧化物及其混合物组成的组的物质。
4.根据权利要求3所述的熔凝颗粒，所述熔凝颗粒以基于氧化物的重量百分比计包括：
-小于40％的氧化钛TiO2；和/或
-小于3％的选自由元素Sr的氧化物、元素Na的氧化物、元素K的氧化物和元素Ba的氧化物及其混合物组成的组的物质。
5.根据权利要求1所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，MgO的重量百分比含量为大于1.5％且小于8％。
6.根据权利要求1所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，CaO的重量百分比含量为大于1.5％且小于8％。
7.根据权利要求1所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，Y2O3的重量百分比含量为大于1.5％且小于8％。
8.根据权利要求1所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，(Cr2O3+MnO2+La2O3+Ga2O3)的含量为小于1％。
9.根据权利要求1所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，所述的元素Sr的氧化物、元素Na的氧化物、元素K的氧化物和元素Ba的氧化物中的每一种的含量为小于4％。
10.根据权利要求9所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，所述元素Sr的氧化物、元素Na的氧化物、元素K的氧化物和元素Ba的氧化物及其混合物的含量为小于1％。
11.根据权利要求1所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，二氧化硅的含量为大于0.1％。
12.根据权利要求11所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，二氧化硅的含量为大于1％。
13.根据权利要求1所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，二氧化硅的含量为小于15％。
14.根据权利要求13所述的熔凝颗粒，其中，以基于氧化物的重量百分比计，二氧化硅的含量为大于2％且小于10％。
15.一种烧结制品，所述烧结制品通过烧结粉末混合物而获得，所述粉末混合物包含至少一种根据权利要求1至14中任一项所述的颗粒的粉末。
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