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CN105541322A - 生产氧化锆基有色，特别是灰色，制品的方法，和使用该方法得到的氧化锆基有色装饰制品 - Google Patents

生产氧化锆基有色，特别是灰色，制品的方法，和使用该方法得到的氧化锆基有色装饰制品 Download PDF

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CN105541322A
CN105541322A CN201510688850.XA CN201510688850A CN105541322A CN 105541322 A CN105541322 A CN 105541322A CN 201510688850 A CN201510688850 A CN 201510688850A CN 105541322 A CN105541322 A CN 105541322A
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CN105541322B (zh
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A·阿克蒂斯-达塔
D·卡蒂尔
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Comadur SA
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Abstract

本发明涉及制备灰色氧化锆基制品的方法，其特征在于它包括以下连续步骤：a)制备包含以下组分的第一混合物：●形成基本成分的氧化锆粉末，●4-15重量％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，●0.1-1重量％氧化钒粉末(V2O5)，●0.1-1重量％氧化铬粉末(Cr2O3)和，●0.1-1重量％二氧化硅粉末(SiO2)；b)制备包含所述第一混合物和粘合剂的第二混合物；c)通过进行所述第二混合物的粒化而制备颗粒混合物；d)通过赋予该第二颗粒混合物所述制品的形状而形成坯；d)将所述坯在空气中在1250-1550℃的温度下烧结至少30分钟。

Description

生产氧化锆基有色，特别是灰色，制品的方法，和使用该方法得到的氧化锆基有色装饰制品
技术领域
本发明涉及生产氧化锆基有色制品，特别是具有灰色范围内的颜色并通过烧结制备的这类制品的方法。为了方便，该制品在以下描述中称为“灰色制品”。
本发明还涉及特别是通过以上方法得到的灰色氧化锆基装饰制品。
背景技术
由文件CN102659401中已知通过将氧化锆材料在石墨真空炉中热处理而由灰色陶瓷材料制备制品，这产生制品的黑色/灰色表面氧化。该方法的缺点特别是不能将制品稳固地着色使得它妨碍在处理以后制品的任何随后加工以得到其最后的形状。此外，所得表面颜色不是均匀的且具有不理想的条纹和大理石花纹。
因此，本发明的主要目的是提供生产基于烧结的有色氧化锆的灰色制品的方法，以及提供特别是使用该方法得到的该制品，该制品具有与未着色氧化锆的那些相当的机械性能，同时还具有稳固着色(solidcoloration)。
发明内容
因此，本发明涉及生产灰色氧化锆基制品的方法，其特征在于它包括以下连续步骤：
a)制备包含以下组分的第一混合物：
●形成基本成分的氧化锆粉末，
●4-15重量％至少一种稳定剂，所述稳定剂选自包括单独或组合的氧化钇、氧化镁和氧化钙的氧化物，
●0.1-1重量％氧化钒粉末(V2O5)，
●0.1-1重量％二氧化硅粉末(SiO2)和
●0.1-1重量％氧化铬粉末(Cr2O3)；
b)制备包含所述第一混合物和粘合剂的第二混合物；
c)通过进行所述第二混合物的粒化而制备颗粒混合物；
d)通过赋予该第二颗粒混合物所需制品的形状而形成坯；
e)将所述坯在空气中在1250-1550℃范围内的温度下烧结至少30分钟。
通过将氧化钒、氧化铬和二氧化硅粉末的混合物并入稳定化的氧化锆粉末中，本发明方法能够在成型和烧结以后形成具有灰色范围内的均匀颜色的稳固着色陶瓷制品。本发明方法能够形成具有特别有吸引力的美学外观的灰色陶瓷制品而不削弱未着色氧化锆的固有机械性能。
根据本发明一个实施方案，第一混合物包含：
●0.4-0.7重量％氧化钒粉末(V2O5)，
●0.2-0.3重量％氧化铬粉末(Cr2O3)，
●0.2-0.3重量％二氧化硅粉末(SiO2)。
有利的是，第一混合物还包含0.1-1重量％，优选0.2-0.3重量％氧化锰粉末(MnO2)。在一个变化方案中，第一混合物还包含0.1-1重量％氧化铁粉末(Fe2O3)，优选第一混合物还包含0.1-5重量％氧化铝粉末(Al2O3)。
本发明还涉及意欲用于生产装饰和/或功能制品的注射模塑或压缩模塑组合物，英文术语通常称为原料，其包含75-96重量％无机粉末混合物和4-25重量％粘合剂，其中所述粉末混合物包含：
●82-95.7重量％氧化锆粉末，
●4-15重量％至少一种稳定剂，所述稳定剂选自包括单独或组合的氧化钇、氧化镁和氧化钙的氧化物，
●0.1-1重量％氧化钒粉末(V2O5)
●0.1-1重量％氧化铬粉末(Cr2O3)，和
●0.1-1重量％二氧化硅粉末(SiO2)。
根据一个优选实施方案，粘合剂和无机粉末混合物以适用作注入模具中的原料的颗粒的形式或者以容易压入模具中的粉末的形式存在。有利地，无机粉末混合物还包含0.1-1重量％，优选0.2-0.3重量％氧化锰粉末(MnO2)。进一步优选无机粉末混合物还包含0.1-5重量％氧化铝粉末(Al2O3)。根据一个变化方案，无机粉末混合物还包含0.1-1重量％氧化铁粉末(Fe2O3)。
本发明还涉及灰色氧化锆基装饰和/或功能制品，其特征在于它由模塑部件烧结的部件形成，所述模塑部件基本包含氧化锆基体、4-15重量％至少一种选自包括氧化钇、氧化镁和氧化钙及其混合物的氧化物的稳定剂、0.1-1重量％氧化钒(V2O5)、0.1-1重量％氧化铬(Cr2O3)和0.1-1重量％二氧化硅(SiO2)。
这类制品的优点是在磨光以后显示出高光泽，因此适于制备装饰制品，例如表壳、珠宝、手镯、胸针、领带别针、项链、手提包、电话机、家具或家用器具的组成元件。
根据一个有利的实施方案，制品包含0.4-0.7重量％氧化钒(V2O5)、0.2-0.3重量％氧化铬(Cr2O3)和0.2-0.3重量％二氧化硅(SiO2)。
在第一变化方案中，制品还包含0.1-1重量％，优选0.2-0.3重量％氧化锰(MnO2)、0.1-5重量％氧化铝(Al2O3)和0.1-1重量％氧化铁(Fe2O3)。
具体实施方式
本发明的其它特征和优点鉴于以下描述变得清晰，以下描述解释为了说明而给出的本发明的非限定性实践实例。
现在详细描述的本发明生产方法的第一实例能够形成灰色烧结氧化锆基制品，其外观和机械性能特别好地适于形成手表的组成部件或者形成任何其它装饰和/或功能制品。
根据该第一实例得到的灰色氧化锆制品包含98.8重量％稳定化氧化锆以及其余重量为0.5重量％氧化钒粉末(V2O5)、0.2重量％二氧化硅粉末(SiO2)和0.5重量％氧化铬粉末(Cr2O3)。
氧化锆以传统方式通过至少一种稳定剂稳定化在四方相中，所述稳定剂选自包括单独或组合的氧化钇、氧化镁和氧化钙的氧化物，该稳定剂的量相对于氧化锆合计为5重量％。
为形成该制品，使用本发明方法的该实践实例的程序如下：
称出2470g的用5重量％氧化钇稳定化的氧化锆粉末。所用粉末具有通常0.5μm的微米或亚微米范围的平均粒度。该粉末以参考号TZ-3Y由theTosohCorporation，日本出售。
然后称出30g的二氧化硅、氧化钒和氧化铬粉末的混合物。
所用硅粉末具有2μmAPS的粒度，并且以参考号13024由AlfaAesar，德国出售。所用氧化钒粉末具有通常22目的微米或亚微米级平均粒度并且以参考号10904由AlfaAesar，德国出售。
所用氧化铬粉末具有通常2.4μm的微米或亚微米级平均粒度，并且以参考号374725由SigmaAldrichChemie，瑞士出售。如果需要的话，将粉末研磨以得到所需粒度。
应当指出所有这些粉末必须优选具有95％以上的纯度。
当粉末的称重结束时，将所有这些粉末混合并混入湿介质中。在最终混合阶段中加入约50g粘合剂，例如聚乙烯醇。
然后将混合物干燥，例如在传统雾化器中干燥。
将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所需制品的构型的模具中以形成后者的坯。
以其几乎最终一般形式，将制品放入烧结炉中。就这点而言，应当指出烧结可以在空气中进行。然后将制品在第一阶段中以30度每小时的速率加热至约1000℃，然后在第二阶段中以50度每小时的速率加热至1450℃的温度。将制品在该温度下保持至少30分钟，优选1小时。
应当指出烧结当然可在高于或等于1100°且低于1600℃的任何其它温度下进行。
在烧结操作以后所得制品的颜色为纯灰色。
然后将制品冷却，然后加工以得到适于其最终用途的形状。应当指出实现的颜色为稳固着色使得在制品上的加工操作不会以任何方式削弱其颜色。
然后将制品磨光，例如使用金刚石研膏，且因此所得制品具有浅灰色光泽外观，使得它显示出有吸引力且有意义的美学特征，特别是对在制表业范畴中的应用而言。
根据本发明方法的另一实施方案，遵循上述操作模式以制备45mm直径且4mm厚的圆形表圈。在该实例中，使用V2O5(0.63％)、Cr2O3(0.25％)、SiO2(0.25％)、MnO2(0.25％)和Al2O3(0.25％)的组合形成配混物，其在总组合物中的重量计含量为1.63％，且余量为98.37重量％稳定化ZrO2。当以其所需最终形式构造时，将表圈和表壳在空气中在1450℃下烧结2小时。将表圈和表壳冷却，然后镜面磨光。所得表圈和表壳具有深灰色光泽外观。在表壳破坏以后还发现着色为稳固的。
根据本发明方法的又一实施方案，遵循上述操作模式以制备45mm直径且4mm厚的圆形表圈。在该实例中，使用V2O5(0.75％)、Cr2O3(0.5％)、SiO2(0.30％)、MnO2(0.10％)、Al2O3(0.25％)和Fe2O3(0.25％)的组合形成配混物，其在总组合物中的重量计含量为2.15％，且余量为97.85重量％稳定化ZrO2。当以其所需最终形式构造时，将表圈在空气中在1450℃下烧结2小时。将表圈冷却，然后镜面磨光。所得表圈具有浅棕灰色光泽外观。在表圈破坏以后还发现着色为稳固的。
下表显示根据本发明制备的制品的其它实例和根据其组成得到的颜色。

Claims (18)

1.制备灰色氧化锆基制品的方法，其特征在于它包括以下连续步骤：
a)制备包含以下组分的第一混合物：
●形成基本成分的氧化锆粉末，
●4-15重量％至少一种稳定剂，所述稳定剂选自包括单独或组合的氧化钇、氧化镁和氧化钙的氧化物，
●0.1-1重量％氧化钒粉末(V2O5)，
●0.1-1重量％氧化铬粉末(Cr2O3)和
●0.1-1重量％二氧化硅粉末(SiO2)；
b)制备包含所述第一混合物和粘合剂的第二混合物；
c)通过进行所述第二混合物的粒化而制备颗粒混合物；
d)通过赋予该第二颗粒混合物所需制品的形状而形成坯；
e)将所述坯在空气中在1250-1550℃范围内的温度下烧结至少30分钟。
2.根据权利要求1的方法，其特征在于第一混合物包含：
●0.4-0.7重量％氧化钒粉末(V2O5)
●0.2-0.3重量％氧化铬粉末(Cr2O3)和
●0.2-0.3重量％二氧化硅粉末(SiO2)。
3.根据权利要求1的方法，其中第一混合物还包含0.1-1重量％，优选0.2-0.3重量％氧化锰粉末(MnO2)。
4.根据权利要求1的方法，其中第一混合物还包含0.1-5重量％氧化铝粉末(Al2O3)。
5.根据权利要求1的方法，其中第一混合物还包含0.1-1重量％氧化铁粉末(Fe2O3)。
6.根据权利要求1的方法，其特征在于稳定剂为氧化钇。
7.根据权利要求1的方法，其特征在于它还包括在步骤e)以后将制品磨光的步骤。
8.意欲用于生产装饰和/或功能制品的注射模塑或压缩模塑组合物，其包含75-96重量％无机粉末混合物和4-25重量％粘合剂，其中所述粉末混合物包含：
●82-95.7重量％氧化锆粉末，
●4-15重量％至少一种稳定剂，所述稳定剂选自包括单独或组合的氧化钇、氧化镁和氧化钙的氧化物，
●0.1-1重量％氧化钒粉末(V2O5)
●0.1-1重量％氧化铬粉末(Cr2O3)和
●0.1-1重量％二氧化硅粉末(SiO2)。
9.根据权利要求8的模塑组合物，其特征在于所述无机粉末混合物包含：
●0.4-0.7重量％氧化钒粉末(V2O5)
●0.2-0.3重量％氧化铬粉末(Cr2O3)和
●0.2-0.3重量％二氧化硅粉末(SiO2)。
10.根据权利要求8或9的模塑组合物，其中无机粉末混合物还包含0.1-1重量％，优选0.2-0.3重量％氧化锰粉末(MnO2)。
11.根据权利要求8的模塑组合物，其中无机粉末混合物还包含0.1-5重量％氧化铝粉末(Al2O3)。
12.根据权利要求8的模塑组合物，其中混合物还包含0.1-1重量％氧化铁粉末(Fe2O3)。
13.特别使用根据权利要求1的方法得到的灰色氧化锆基装饰和/或功能制品，其特征在于它由模塑部件烧结的部件形成，所述模塑部件基本包含氧化锆基体、4-15重量％至少一种选自包括氧化钇、氧化镁和氧化钙及其混合物的氧化物的稳定剂、0.1-1重量％氧化钒(V2O5)、0.1-1重量％氧化铬(Cr2O3)和0.1-1重量％二氧化硅(SiO2)。
14.根据权利要求13的制品，其特征在于它包含0.4-0.7重量％氧化钒(V2O5)、0.2-0.3重量％氧化铬(Cr2O3)和0.2-0.3重量％二氧化硅(SiO2)。
15.根据权利要求13或14的制品，其特征在于它还包含0.1-1重量％，优选0.2-0.3重量％氧化锰(MnO2)。
16.根据权利要求13的制品，其特征在于它还包含0.1-5重量％氧化铝(Al2O3)。
17.根据权利要求13的制品，其特征在于它还包含0.1-1重量％氧化铁(Fe2O3)。
18.根据权利要求13的制品，其特征在于它形成计时器的组成元件。
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PT3012239T (pt) 2020-01-20
US20160115082A1 (en) 2016-04-28
KR20160047408A (ko) 2016-05-02
JP6310435B2 (ja) 2018-04-11
US10059629B2 (en) 2018-08-28
JP2016084270A (ja) 2016-05-19
EP3012239B1 (fr) 2019-10-09
EP3012239A1 (fr) 2016-04-27

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