CN101133002B - 基于氧化锆和氧化铈的烧结珠 - Google Patents
基于氧化锆和氧化铈的烧结珠 Download PDFInfo
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Abstract
本发明涉及一种烧结珠,其表现为下述化学分析,其在总量100%中按重量百分数计为:ZrO2+HfO2:78%-85%;CeO2:≥15%;Al2O3:>0.1%;添加剂:>0.1%;杂质:<1%;所述添加剂选自MnO、MnO2、Fe2O3、CuO、TiO2、Y2O3、Sb2O3、ZnO和它们的混合物。本发明还涉及所述烧结珠在微研磨和微分散中的应用。
Description
技术领域
本发明涉及一种基于氧化锆和氧化铈的烧结珠,以及其在研磨机中的应用。
背景技术
在微研磨和微分散的应用中,例如,和涂料用的颜料一起的微研磨和微分散,烧结珠所需要的特性是其耐磨损性。
已知密度是一项重要的参数,并且已知可以通过提高烧结温度来增加烧结产品的密度。然而,提高温度是非常昂贵的,并且也会导致产品微结构的改变,而这可以损害其性能。
发明内容
因此,需要一种表现出良好耐磨损性和能够在相对低温下,通过烧结被制造的烧结珠。
本发明的目的在于满足这一需要。
根据本发明,这一目的是通过一种烧结珠来实现的,该烧结珠表现出下述化学分析,按重量百分数计,在总100%中为:
·ZrO2+HfO2:78%-85%;
·CeO2: ≥15%;
·Al2O3: >0.1%;
·添加剂: >0.1%;
·杂质: <1%;
所述添加剂选自MnO、MnO2、Fe2O3、CuO、TiO2、Y2O3、Sb2O3、ZnO和它们的混合物。
如下述说明书中更详细的说明,氧化铝和添加剂的组合物具有一协同效应,并且使得耐磨损性显著提高。因此,可以在低至1300℃的烧结温度下获得良好的耐磨损性。
优选地,本发明的烧结珠也可选择地呈现出下述特性中的一种或多种:
·按重量百分数计,所述氧化铝(Al2O3)的含量大于0.2%和/或小于1%;
·按重量百分数计,所述添加剂的含量大于0.3%和/或小于0.8%;
·按重量百分数计,所述Al2O3和所述添加剂的总量大于0.6%,优选大于0.7%;
·所述添加剂是MnO和/或Fe2O3;
·按重量计,所述CeO2的含量小于或等于20%;
·所述添加剂百分数和所述氧化铝百分数的比值大于0.5和/或小于2。优选大于0.7和/或小于1.5,和更优选该比值基本上等于1。
本发明还提供了发明所述烧结珠混合物在研磨机中的应用,尤其是用于颜料的微研磨或微分散。
在本说明书中,除非指明为相反内容,烧结珠的所有组成均按照基于烧结珠总重量的重量百分数给出。
术语“杂质”意指原料中提供的所有其它成分,例如CaO。考虑到杂质总含量小于1%并不显著改变所得到的结果。
在本说明书中,术语“添加剂”可以不仅指MnO、MnO2、Fe2O3、CuO、TiO2、Y2O3、Sb2O3或者ZnO,也可以指这些成分的混合物。
确定氧化铈CeO2的量以便本发明的烧结珠基本上不含单斜晶形氧化锆。相对于烧结珠的其它氧化物的重量,CeO2的最小值为15%被认为是必需的。然而,由于CeO2非常昂贵,其含量优选不大于20%。
为了制造本发明的烧结珠,可以按如下进行。
在室温下,首先制备一水悬浮液,其包括ZrO2+HfO2、CeO2、Al2O3的粉末和,在适宜的时候,包括下述一种或多种氧化物:MnO、MnO2、Fe2O3、CuO、TiO2、Y2O3、Sb2O3和ZnO。这些成分的来源是按照这样的方式选择,使得按重量百分数计,在本发明烧结珠的成分的干物质的重量中,杂质的总含量小于1%。
所述的水悬浮液表现为干物质含量在50%~70%的范围内。
正如本领域技术人员公知,该悬浮液也可以含有下述成分:
·一分散剂,按重量计,其浓度为相对于干物质重量占0~10%;
·一粘度稳定剂或反絮凝剂,按重量百分数计,其浓度为相对于干物质重量占0~3%;和
·一表面张力改性剂,按重量百分数计,其浓度为相对于干物质重量占0~3%;
·一胶凝剂,按重量百分数计,其浓度为相对于干物质重量占0~2%。
分散剂或反絮凝剂、表面张力改性剂和胶凝剂是本领域技术人员公知的。将其应用于电解液,该电解液适合与一确定的胶凝剂反应。
作为实例,可以提及以下:
·作为分散剂或反絮凝剂的,聚甲基丙烯酸钠或聚甲基丙烯酸铵系列,聚丙烯酸钠或聚丙烯酸铵系列,聚丙烯酸(钠盐或铵盐)系列,或者其它聚电解质,柠檬酸盐系列,例如柠檬酸铵,磷酸钠系列和碳酸酯系列;
·作为表面张力改性剂的,有机溶剂,例如,某些脂肪族醇;和
·作为胶凝剂的,某些天然多糖系列中的某些成分。
上述所有成分在下述制造步骤中不复存在。因此,它们并不影响本发明的烧结珠的组成。
所使用的粉末,尤其是ZrO2和CeO2的粉末,优选地表现为中位直径小于1微米(μm),优选小于0.5μm。
然后,通过将悬浮液流经一个校准孔获得悬浮液的液滴。该液滴离开该孔落入到一凝胶溶液(与胶凝剂反应的电解液)池中,在池中,该液滴在被变成基本上是球面的形状后变硬。然后,从该池中提取出由此所获得的空心烧结珠,干燥,然后在常压下,在空气中烧结。
优选地,烧结时间持续2~5小时。
通常,所获得的烧结珠直径为0.5~2.5毫米(mm)。
具体实施方式
为了说明本发明的目的给出下述非限制性实施例。
通过氧化锆(中位直径小于5μm)源、CeO2(中位直径小于10μm)源和氧化铝(中位直径(d50)为0.4μm)源制备烧结珠。氧化锆和CeO2源的纯度大于98%。将粉末混合然后在一湿介质中共同研磨直到获得一表现出良好粒径的混合物(中位直径<1μm,优选<0.5μm)。然后干燥该混合物。
然后将该混合物用于制备水悬浮液,按干物质的重量百分数计,所述水悬浮液包括:7.5%的聚丙烯酸型分散剂;1.95%正丁醇(表面张力改性剂);1%碳酸酯型的反絮凝剂(粘度稳定剂);和1%胶凝剂,即藻酸盐系列的一种多糖。
在制备中使用一台球磨机以便获得具有良好均一性的悬浮液。首先制备含有胶凝剂的溶液。此后,向其中添加下述:添加剂和氧化铝;然后是ZrO2/HfO2和CeO2粉末;然后是分散剂,然后是表面张力改性剂;和最后是足量水以保证实现良好的混合。将所获得的混合物搅拌8小时。然后添加反絮凝剂,并搅拌混合物0.5小时。最后,加入定量的水以便获得具有65%干物质和粘度小于8500厘泊(cP)的水悬浮液,该粘度由布鲁克费尔德粘度计测定。然后悬浮液的pH值大约是9。
在本文的实施例中,对悬浮液施加压力使其以一定速率通过一个校准孔,其使得所获得的烧结珠在经烧结后能够具有约为1.2mm的粒度。悬浮液的液滴落入到一基于电解液的凝胶浴中,该电解液是由与胶凝剂反应的、二价或三价的阳离子盐组成的。然后收集粗烧结珠,清洗以除去过量的反应物,然后在90℃干燥以除去水分。然后将烧结珠转移到一烧结炉中,在那里连续4小时以5℃/h的速率被升高到所期望的温度。
对表现为不同组成和使用上述方法获得的烧结珠进行两套试验。在第一套试验中,将烧结温度在1300℃保持不变,并观察与烧结温度无关时,烧结珠组成对烧结珠密度的影响。在第二套试验中,以所有被测试的烧结珠表现为密度基本上相同的方式设置烧结温度。因此,可以观察到与密度无关时,烧结珠的组成对磨损率的影响。
通过将在水悬浮液中的770克(g)烧结珠加载到一个1升(L)的磨损型圆盘研磨机上来评估耐磨损性,所述的水悬浮液含有按重量计10%的、适于模拟该操作的陶瓷粉末。此后,调节转动速度并以线速度为10米/秒(m/s)的方式保持80h。此后测量烧结珠的重量损失。所述磨损率,以百分数给出,对应于烧结珠在研磨前和研磨后的重量差值除以研磨前烧结珠重量的比值。
下述表1总结了所获得的结果。
表1
NA:″没有得到″
表1中的组合物还包括16.5%的CeO2,含量小于1%的杂质,和总计100%的余量的ZrO2+HfO2,。
表1中第一套试验显示本发明烧结珠中氧化铝的存在导致在一给定烧结温度下密度增加。当在组合物中进一步含有选自MnO、MnO2、Fe2O3和CuO的添加剂时,该密度更大。添加剂是CuO和Fe2O3时得到密度最大值。
表1中第二套试验中显示,对于具有基本上相同密度的、由不同组合物组成的烧结珠,当组合物不仅包括氧化铝,还包括至少一种选自MnO、MnO2、Fe2O3和CuO的添加剂时,所测量的磨损率显著提高。令人惊讶地,同时使用氧化铝和至少一种选自MnO、MnO2、Fe2O3和CuO的添加剂时,可以获得比平均值更好的结果,该平均值通过只加入氧化铝或只加入添加剂获得。因此氧化铝和添加剂是协同作用的。
MnO和Fe2O3是优选的添加剂,使用它们获得最佳耐磨损性,最优选的是组合物4。
优选地,按重量百分数计,添加剂的总含量大于或等于0.2%,优选0.3%,更优选0.5%。
优选地,添加剂百分数和氧化铝百分数的比值在0.5~2之间,优选0.7~1.5。该比值优选基本上等于1。
优选地,所述组合物包括MnO作为单独的添加剂,也优选,按重量百分数计,氧化铝的含量大于或等于0.2%,优选0.3%。
就此可以清楚地看出,本发明提供了一种表现出良好耐磨损性并能在相对低的温度下通过烧结而制造的烧结珠。
当然,本发明并不仅仅限于上述实施例和实施过程。尤其是,其它凝胶体系也适于制造本发明的陶瓷烧结珠。因此US 5 466 400、FR 2 842 438和US 4 063 856描述了可以使用的溶胶-凝胶方法。FR 2 842 438和US 4 063 856使用了一种与上述接近的凝胶体系(基于藻酸钠),而US 5 466 400描述了一种非常不同的体系。
Claims (11)
1.一种烧结珠,该烧结珠表现为下述化学分析,其在总量100%中按重量百分数计为:
·ZrO2+HfO2: 78%-总计100%余量;
·CeO2: ≥15%和≤20%;
·Al2O3: >0.1%和<1%;
·添加剂: >0.1%和<0.8%;
·杂质: <1%;
所述添加剂选自MnO、MnO2、Fe2O3、CuO、TiO2、Y2O3、Sb2O3、ZnO和它们的混合物。
2.根据权利要求1所述的烧结珠,其特征在于,按重量百分数计,氧化铝Al2O3的含量大于0.2%。
3.根据权利要求1所述的烧结珠,其特征在于,按重量百分数计,所述添加剂的含量大于0.3%。
4.根据权利要求1所述的烧结珠,其特征在于,按重量百分数计,所述氧化铝加上所述添加剂的总量大于0.6%。
5.根据权利要求1所述的烧结珠,其特征在于,所述添加剂的百分数和所述氧化铝的百分数的比值大于0.5和小于2。
6.根据权利要求5所述的烧结珠,其特征在于,所述添加剂的百分数和所述氧化铝的百分数的比率大于0.7和小于1.5。
7.根据权利要求1所述的烧结珠,其特征在于,所述添加剂的百分数和所述氧化铝的百分数的比值基本上是1。
8.根据权利要求1所述的烧结珠,其特征在于,所述添加剂是MnO和/或Fe2O3。
9.根据权利要求4所述的烧结珠,其特征在于,所述添加剂的百分数和所述氧化铝的百分数的比率大于0.7和小于1.5。
10.根据权利要求9所述的烧结珠,其特征在于,所述添加剂是MnO和/或Fe2O3。
11.根据前述任一权利要求所述的烧结珠的混合物在研磨机中的应用。
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PCT/FR2006/000437 WO2006092486A1 (fr) | 2005-03-01 | 2006-02-27 | Bille frittee a base de zircone et d'oxyde de cerium |
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EP1853532B1 (fr) | 2010-06-30 |
AU2006219849B2 (en) | 2012-06-28 |
PL1853532T3 (pl) | 2010-12-31 |
DK1853532T3 (da) | 2010-10-18 |
FR2882749A1 (fr) | 2006-09-08 |
KR20070122204A (ko) | 2007-12-28 |
JP2008531455A (ja) | 2008-08-14 |
DE602006015168D1 (de) | 2010-08-12 |
SI1853532T1 (sl) | 2010-10-29 |
ZA200707503B (en) | 2008-12-31 |
EA200701668A1 (ru) | 2008-02-28 |
AU2006219849A1 (en) | 2006-09-08 |
KR101330767B1 (ko) | 2013-11-18 |
CA2599421C (fr) | 2013-10-15 |
JP5112084B2 (ja) | 2013-01-09 |
EA011425B1 (ru) | 2009-02-27 |
WO2006092486A1 (fr) | 2006-09-08 |
CN101133002A (zh) | 2008-02-27 |
US20090120010A1 (en) | 2009-05-14 |
PT1853532E (pt) | 2010-09-22 |
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