CN110128135A - 制造鲜橙色氧化锆基制品的方法；和根据该方法得到的装饰性鲜橙色氧化锆基制品 - Google Patents

制造鲜橙色氧化锆基制品的方法；和根据该方法得到的装饰性鲜橙色氧化锆基制品 Download PDF

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CN110128135A
CN110128135A CN201910439602.XA CN201910439602A CN110128135A CN 110128135 A CN110128135 A CN 110128135A CN 201910439602 A CN201910439602 A CN 201910439602A CN 110128135 A CN110128135 A CN 110128135A
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oxide
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zirconium oxide
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A·阿克蒂斯-达塔
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Comadur SA
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Abstract

本发明涉及制造橙色氧化锆基制品的方法，其特征在于它包括一系列步骤，在于：包含以下组分的第一混合物：氧化锆粉末，3‑20重量％的至少一种选自包含单独或组合的氧化钇、氧化镁和氧化钙的氧化物组的稳定剂，0.1％至5重量％的至少一种预期形成玻璃相且选自包含单独或组合的二氧化硅、氧化铝、氧化锂和氧化钇的组的元素，1％至6重量％氧化铈粉末；产生包含所述第一混合物和粘合剂的第二混合物；通过将所述第二混合物造粒而产生粒状混合物；通过赋予所述第二粒状混合物所需制品的形状而形成生坯；在1,250‑1,500℃的温度下空气烧结至少30分钟并将所需制品在还原气氛中在700℃至1,350℃的温度下退火30分钟至20小时，和将所述烧结生坯抛光。

Description

制造鲜橙色氧化锆基制品的方法；和根据该方法得到的装饰 性鲜橙色氧化锆基制品
本申请是申请号为201480035281.2的发明专利申请的分案申请，原申请的申请日为2014年5月5日，发明名称为：生产由氧化锆制造的有色制品，特别是橙色制品的方法；和根据该方法得到的由氧化锆制造的有色装饰性制品。
本发明涉及制造有色氧化锆基制品，特别是显示出包含在从鲜橙色至铜棕色范围内的颜色并借助烧结实现的这种制品。为了方便，该制品在以下描述中称为“橙色制品”。
本发明还涉及特别根据下文所述方法得到的装饰性氧化锆基橙色制品。
已知将着色剂或颜料如硫化镉(CdSe)、硒化镉和硫硒化镉结合到陶瓷材料中以得到例如用于产生家用或地板用珐琅、釉料和容器的橙色/红色陶瓷制品。
当需要将这类着色剂结合到工业陶瓷，特别是烧结氧化锆基陶瓷中时，这类着色剂的使用具有大量缺点。
实际上，这些着色剂在高温下是不稳定的，并且在达1,000或2,000℃下显示其着色特性。这极大地限制了这类着色剂的用途，特别是，不容许用于产生烧结氧化锆制品，因为氧化锆的烧结温度在任何情况下都高于1,100℃。
另外，包含重金属的这类着色剂在意欲与使用者皮肤接触的物体如表壳中的使用如果法律不禁止的话，至少受到强烈阻拦。
另外，市售的这类着色剂具有大粒度，这与得到与氧化锆粉末的均匀混合物不相容。
因此，本发明的主要目的是一方面提供制造鲜橙色烧结氧化锆基制品的方法，另一方面提供根据该方法得到的这种制品，该制品具有满意的机械性能，同时在从表面上起至少5mm的深度显示出鲜橙色颜色。
为此，本发明涉及制造鲜橙色氧化锆基制品的方法，其特征在于它包括一系列步骤，在于：
产生包含以下组分的第一混合物：
·氧化锆粉末，
·3-20重量％的至少一种稳定剂，所述稳定剂单独或组合地选自包含氧化钇、氧化镁和氧化钙的氧化物组，
·0.1％至5重量％的至少一种意欲产生玻璃相且单独或组合地选自包含二氧化硅、氧化铝、氧化锂和氧化钇的组的元素，
·1％至6重量％的氧化铈粉末；
产生包含所述第一混合物和粘合剂的第二混合物，
通过将所述第二混合物造粒而产生粒状混合物；
通过赋予第二粒状混合物所需制品的形状而形成生坯；
在1,250-1,500℃的温度下空气烧结至少30分钟，和
将所需制品在具有10-6至10-1大气压的氧分压的还原气氛中在700℃至1,350℃的温度下退火30分钟至20小时的时间，和
将所述烧结生坯抛光。
本发明方法使得可通过将氧化铈粉末(CeO2)结合到待烧结混合物中而降低烧结温度。氧化铈还充当赋予制品所需的橙色的决定元素之一。
实际上，在CeO2的存在下的烧结操作以后，制品的颜色是象牙白。然后在本发明方法的随后步骤，所谓的退火步骤期间，利用CeO2(+4氧化态)的存在将它还原成Ce2O3(+3氧化态)。在该退火步骤以后，制品取决于存在于颗粒边界上的+4和+3氧化态的铈各自的量而具有黄橙色至鲜橙色范围内的颜色。+4氧化态的氧化铈(CeO2)的颜色是象牙白，+3氧化态的氧化铈(Ce2O3)的颜色为鲜橙色。
存在于颗粒边界上的+4和+3氧化态的氧化铈各自的量由退火条件决定，更具体而言，通过改变进行退火的烘箱环境中的氧分压而决定。
根据一个实施方案，第一混合物包含0.1-1重量％的用于玻璃相的氧化物粉末，优选4-5重量％的氧化铈粉末(Ce+4O2)。
本发明还涉及根据上述方法得到的装饰性鲜橙色氧化锆基制品，其特征在于它由烧结部件形成，所述烧结部件由模制部件制成，所述模制部件基本包含氧化锆基体，3-20重量％的至少一种稳定剂，所述稳定剂选自包含单独或组合的氧化钇、氧化镁和氧化钙的氧化物组，0.1％至5重量％的玻璃相，所述玻璃相包含至少一种选自包含单独或组合的二氧化硅、氧化铝、氧化锂和氧化钇的组的元素，和1％至6重量％的氧化铈。
所述制品的优点是在抛光以后显示出强光泽度，因此特别适于制备装饰性制品，例如表壳的组成部件、珠宝、手镯、胸针、领带别针、项链、手提包、电话机、家具或家用器具。
本发明的其它特征和优点鉴于对本发明方法的示例执行的以下描述获悉。
现在详细描述的本发明制造方法为容许产生鲜橙色烧结氧化锆基制品的方法，所述制品的外观和机械性能特别适于制备手表的组成部件或者制备任何其它装饰性制品。
根据该方法得到的鲜橙色氧化锆制品包含89％至98.9重量％的稳定化氧化锆和其余重量计，即0.1％至5重量％的由二氧化硅、氧化铝、氧化钇和氧化锂单独或组合地形成的玻璃相，和1％至6重量％的氧化铈。
氧化锆通常通过至少一种选自包含单独或组合的氧化钇、氧化镁和氧化钙的氧化组的稳定剂稳定为四方相，该稳定剂相对于氧化锆为3％至20重量％的量。
为制备该制品，根据本发明方法的示例执行，一种方法如下进行：
称943g具有3重量％氧化钇的稳定化锆粉末。所用粉末具有微米级，通常0.1-0.5μm的平均粒度。该粉末以参考名TZ-3 Y由the Tosoh Corporation，日本出售。
然后称7g二氧化硅、氧化铝和氧化锂粉末的混合物，其预期在随后的烧结期间形成玻璃相。
优选，玻璃相包含以重量计递减次序，分别47％、40％和13％的二氧化硅、氧化铝和氧化锂的混合物或组合。
所用硅粉末具有小于1μm，通常40nm的平均粒度，并且以名称Aerosil OX50由Cerdec，德国出售。
所用铝粉末具有微米或亚微米级，通常0.5μm的平均粒度，并且以名称CR30由Baikowski，法国出售。
所用锂粉末具有微米或亚微米级，通常2.4μm的平均粒度，并且以参考号374725由Sigma-Aldrich Chemicals，瑞士出售。如果需要的话，将粉末研磨以实现所需粒度。
最后，称50g氧化铈(Ce4+O)；所用粉末具有微米或亚微米级，通常0.5μm的粒度，并且以参考号202975由Sigma-Aldrich Chemicals，瑞士出售。
应当指出这些粉末应优选都具有多于95％的纯度。
当将粉末称重时，将所有所述粉末在湿介质中混合并均化。在均化的最后阶段中，加入约50g粘合剂，例如聚乙烯醇。
然后将混合物例如在常规雾化器中干燥。
将因此所得颗粒筛分以保持具有小于200μm的粒度的颗粒。
然后将筛分的颗粒压入具有技术人员想要得到的制品形状的模具中以形成其生坯。
将为其几乎最终通常形状的制品放入烧结炉中。就这点而言，应当指出烧结可在空气中进行。然后将制品在第一阶段中以30°/小时的速度加热至约1,000℃，然后在第二阶段中以50°/小时的速度加热至1,250℃的温度。将制品保持在该温度下至少30分钟，优选1小时。
应当指出烧结当然可在高于或等于1,100°且低于1,600℃的任何其它温度下进行。
在烧结期间，二氧化硅、氧化铝、氧化钇和氧化锂与颗粒边界上的+4氧化态的氧化铈形成浓缩的玻璃相，这在烧结以后赋予制品象牙颜色。
应当指出氧化锂的存在有利地降低烧结温度并限制氧化铈颜色的转变，由此容许得到鲜橙色。
在该烧结步骤以后，将制品放入可选择气氛的退火炉中。将所需制品在氢气气氛(H2)中，或者在包含氮气和氢气的混合物(N2/H2)或氩气和氢气的混合物的气氛中退火。
在该退火操作期间，炉中的氧分压为10-6至10-1大气压，退火温度为700℃至1250℃，且退火时间通常为30分钟至20小时。
根据本发明方法的优选执行，退火炉中的气氛为氢气，氧分压为10-4至10-1大气压，退火温度为900-1,150℃且退火时间为4-6小时。应当理解制品内部的颜色深度与退火时间成比例地变化。
取决于退火条件，在退火操作以后得到的制品的颜色为鲜橙色或者橙色与铜棕色之间的色调。
然后将制品冷却并机器加工以得到适于其最终用途的形状。应当指出在制品内部深处着色，使得机器加工制品决不改变其颜色。
最后，将制品例如使用金刚石研磨膏抛光，因此所得制品根据退火条件具有为鲜橙色或者包含在上述颜色之间的色调的光泽外观，使得它具有有吸引力且有意义的美学特征，特别是对制表业领域中的应用而言。
根据本发明方法的另一示例执行，进行上述操作方法以产生直径45mm且4mm厚的圆形表圈(watch bezel)。该实例使用SiO2(47％)、Al2O3(40％)和Li2O(13％)的组合，从而形成总组合物的重量比例为0.7％的化合物，所述混合物形成玻璃相，6重量％CeO2，和其余，即93.3重量％稳定化ZrO2。当以其所需最终形状构造时，将表圈在空气中在1,450℃下烧结2小时。然后将这些表圈在包含5％氢气和95％氩气的气氛中在1,000℃下退火12小时。然后将表圈冷却并镜面抛光。所得表圈具有鲜橙色光泽外观。在将表圈打破以后，还观察到着色在制品深处实现。

Claims (8)

1.制造鲜橙色氧化锆基制品的方法，其特征在于它包括一系列步骤，在于：
产生包含以下组分的第一混合物：
·氧化锆粉末，
·3-20重量％的至少一种稳定剂，所述稳定剂选自包含单独或组合的氧化钇、氧化镁和氧化钙的氧化物组，
·0.1％至5重量％的至少一种预期产生玻璃相且选自包含单独或组合的二氧化硅、氧化铝、氧化锂和氧化钇的组的元素，
·1％至6重量％的氧化铈粉末，
其中第一混合物不包含氧化铜粉末；
产生包含所述第一混合物和粘合剂的第二混合物，
通过将所述第二混合物造粒而产生粒状混合物；
通过赋予第二粒状混合物所需制品的形状而形成生坯；
在1,250-1,500℃的温度下空气烧结至少30分钟，和
将所需制品在还原气氛中在700℃至1,350℃的温度下退火30分钟至20小时，和
将所述烧结生坯抛光。
2.根据权利要求1的方法，其中第一混合物包含0.1％至1重量％的预期形成玻璃相的粉末。
3.根据权利要求1或2的方法，其中预期形成玻璃相的粉末包含以重量计递减次序的量的二氧化硅、氧化铝、氧化锂和氧化钇。
4.根据权利要求3的方法，其中二氧化硅、氧化铝和氧化锂的以重量计递减次序的量分别为47％、40％和13％。
5.根据权利要求1或2的方法，其特征在于第一混合物包含1-6％，优选4-5重量％的氧化铈粉末。
6.根据权利要求1或2的方法，其特征在于稳定剂为氧化钇。
7.根据权利要求1或2的方法，其特征在于退火温度为700-1,350℃且还原气氛具有10-6至10-1大气压的氧分压。
8.根据权利要求1-7中任一项所述方法得到的装饰性鲜橙色氧化锆基制品，其特征在于制品由烧结部件形成，所述烧结部件由模制部件制成，所述模制部件基本包含氧化锆基体，3-20重量％的至少一种稳定剂，所述稳定剂选自包含氧化钇、氧化镁、氧化铈和氧化钙及其混合物的氧化物组，0.1％至5重量％的玻璃相，所述玻璃相包含二氧化硅、氧化铝、氧化锂和氧化钇及其混合物，和1％至6重量％的氧化铈。
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KR20160004382A (ko) 2016-01-12
US9676671B2 (en) 2017-06-13
KR101821876B1 (ko) 2018-01-24
EP2799411A1 (fr) 2014-11-05
CA2910905A1 (fr) 2014-11-06
PT2991950T (pt) 2017-06-29
WO2014177714A1 (fr) 2014-11-06

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