CN117623745A - 色彩鲜艳的陶瓷制品及其制造方法 - Google Patents

色彩鲜艳的陶瓷制品及其制造方法 Download PDF

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Publication number
CN117623745A
CN117623745A CN202311072092.XA CN202311072092A CN117623745A CN 117623745 A CN117623745 A CN 117623745A CN 202311072092 A CN202311072092 A CN 202311072092A CN 117623745 A CN117623745 A CN 117623745A
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doped
article according
component
ceramic
aluminium garnet
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M·福尔纳巴约
L·塔巴尔德
S·博尔本
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Swatch Group Research and Development SA
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Swatch Group Research and Development SA
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Abstract

本发明涉及由包含基于氧化物的基质和掺杂或共掺杂的铝石榴石族组分的陶瓷制成的彩色制品。本发明还涉及制造所述制品的方法。

Description

色彩鲜艳的陶瓷制品及其制造方法
技术领域
本发明涉及色彩鲜艳的陶瓷制品，特别涉及基于氧化物的材料如氧化铝制成的钟表外壳或机芯组件。其还涉及制造所述制品的方法。
背景技术
彩色陶瓷在工业上通常通过将基于金属氧化物的基质，例如Al2O3、ZrO2及其复合材料与着色颜料混合来制造。在一些情况下，陶瓷可以通过掺杂进入晶体结构的不同原子来着色。以这种方式获得的颜色通常是浅色的。例如，陶瓷的黄色着色通常通过掺杂镨或通过添加基于氧化钨和/或氧化钒的颜料来实现。获得的颜色通常是浅黄色或变成橙色。
文献WO 2018/172428在钟表领域提出了一种替代方案，其公开了通过并入包封在适于允许光通过的金属氧化物基质中的颜料来制造色彩鲜艳的陶瓷部件。更确切而言，该方法设想了使用非常规的加压烧结以使材料致密化，这是一种工业上实施起来复杂的方法。
发明内容
本发明的目的是提供一种新的色彩鲜艳的陶瓷组合物，其允许使用便宜的方法生产制品。
更确切而言，本发明涉及由陶瓷制成的彩色制品，所述陶瓷包含基于氧化物的基质和掺杂或共掺杂的铝石榴石族组分。
更详细地，该掺杂或共掺杂的铝石榴石族组分，如铈掺杂的钇铝石榴石(YAG：Ce)赋予基于氧化物的陶瓷明亮绚丽的色彩。此类着色元素不仅代表了常规着色颜料的替代品，还能够获得更强烈的色调和显著扩展可能的颜色范围。此外，通过添加基于氧化物的基质来开发复合材料可以省去使用纯YAG，这意味着显著降低成本并显著改善韧性与机械加工性。
当用铬或镧系家族的元素(如铈、钕、铒、钬和镱)掺杂铝石榴石族组分时，获得强烈和生动的颜色。特别地，当其掺杂有铈时，获得黄色。这种明亮的颜色不能通过与商业颜料混合或通过掺杂不同原子来获得。当其掺杂有钕时，获得紫色，而当其掺杂有铬时，根据其氧化态获得由绿至红的颜色。当其掺杂有铒时，获得粉红色。当其掺杂有镱时，获得绿色。用选自铬和镧系家族的元素如铈、铒、镱、钬和钕的一种或多种附加元素共掺杂能够调制这些颜色，并由此拓宽了可以获得的颜色范围。使用掺杂或共掺杂的铝石榴石族组分由此能够获得具有再发射性质的明亮绚丽的颜色。
采用这些不同的掺杂剂以这种方式获得的制品具有明亮的颜色，其中Lab颜色空间中的L分量大于或等于80、优选大于或等于85、更优选大于或等于90。
其具有大于或等于1000HV10、优选大于或等于1200HV10、更优选大于或等于1550HV10的硬度。
其具有1.7至6MPa√m、通常为2至4.5MPa√m的韧度KiC。
本发明还涉及制造所述制品的方法，包括以下步骤：
-用氧化物和掺杂或共掺杂的铝石榴石族组分产生基础混合物，也称为第一混合物，并且该步骤任选在液体介质中进行，
-形成包含第一混合物和有机粘合剂体系的第二混合物，
-将所述第二混合物造粒，
-形成具有该制品的形状的坯料，
-在空气中在1500至1800℃、优选1600至1700℃的保持温度下烧结该坯料20分钟至20小时、优选1小时至5小时的时间。
通过混合粉末和常规烧结，提出的方法可以容易地工业化，并且与涉及通过SPS(放电等离子体烧结)或用包含纯YAG的组合物制造的现有方法相比具有更低的经济影响。
在参考附图阅读以下详述之后，本发明的其它特征和优点将变得更加显而易见。
附图说明
图1显示了包括由根据本发明的陶瓷材料制成的表身(middle)的钟表。
具体实施方式
本发明涉及由基于氧化物的陶瓷材料制成的制品。该制品可以是装饰性制品，如手表、珠宝、手镯等的组成元件，或者更一般地为便携式元件的外部部分，如移动电话的外壳。在钟表制造领域中，该制品可以是外部部件如表身、底盖、表壳前圈、表冠、夹板、按钮、腕带连接件、表盘、指针、表盘快慢针(dial index)等。为了说明，图1中显示了由根据本发明的陶瓷材料制成的表身。其还可以包括机芯组件例如主夹板或摆锤。
陶瓷材料包含基于氧化物的基质。该氧化物可以是ZrO2、Al2O3、TiO2、SiO2、MgAl2O4和ZnO或这些氧化物的混合物，如Al2O3+ZrO2。在氧化锆(ZrO2)的存在下，后者通常由钇、铈、钙或镁来稳定。优选地，该基质基于Al2O3。该陶瓷材料进一步包含掺杂或共掺杂的铝石榴石族的磷光染料组分。掺杂或共掺杂的铝石榴石族组分的重量百分比相对于陶瓷材料的总重量为5至85％、优选5至70％、更优选10至60％。由此，该陶瓷材料按重量计包含15至95％、优选30至95％、更优选40至90％的氧化物，和5至85％、优选5至70％、更优选10至60％的掺杂或共掺杂的铝石榴石族组分。
该铝石榴石可以是钇铝石榴石(YAG)或镥铝石榴石(LuAG)。优选钇铝石榴石。这些石榴石分别掺杂或共掺杂有镧系家族的一种或多种元素：铈、钕、钬、铒和镱，或掺杂有铬。优选地，该石榴石掺杂有铈。更优选地，其是掺杂有铈的钇铝石榴石。甚至更优选地，该制品包含基于氧化铝的基质(Al2O3)和掺杂有铈的钇铝石榴石(YAG：Ce)。这种陶瓷还可包含含量小于或等于0.2重量％、或0.1重量％的可能杂质。
有利地，该陶瓷由基于氧化物的基质、掺杂或共掺杂的石榴石族组分和可能的杂质组成。优选地，该陶瓷由基于氧化铝的基质(Al2O3)和掺杂铈的钇铝石榴石(YAG：Ce)和可能的杂质组成。
根据本发明，石榴石族组分掺杂有上述元素中的一种，并且可能共掺杂有上述元素中的一种或多种，掺杂剂和可能的一种或多种共掺杂剂相对于该组分的总原子百分比为0.1至50％。当需要黄色时，用铈掺杂。优选地，对于用铈掺杂，相对于石榴石族组分的原子百分比为0.5至10％、更优选1至5％。当需要绿色至红色的颜色时，根据铬的氧化程度，用铬掺杂。对于铬掺杂，相对于石榴石族组分的原子百分比为0.1至50％。当需要紫色时，用钕掺杂。优选地，相对于该组分的原子百分比为0.9至11％。当需要粉红色着色时，用铒掺杂，其中相对于该组分的原子百分比为0.1至50％。当需要绿色着色时，用镱掺杂，其中相对于该组分的原子百分比为0.1至50％。添加共掺杂剂使得可以改变颜色。例如，其可以是掺杂有铈并共掺杂有钕的石榴石族组分。
具有一种或多种掺杂剂的制品具有明亮的颜色，其中Lab颜色空间中的L分量为大于或等于80、优选大于或等于85、更优选大于或等于90。其具有大于或等于1000HV10、优选大于或等于1200HV10、更优选大于或等于1550HV10的硬度。对于具有掺杂铈的钇铝石榴石的氧化铝基质，其具有大于或等于1400HV10、优选大于或等于1550HV10的硬度。对于具有铈掺杂的钇铝石榴石的氧化锆基质，其具有大于或等于1250HV10、优选大于或等于1400HV10的硬度。类似地，对于具有铈掺杂的钇铝石榴石的氧化铝和氧化锆基质，其具有大于或等于1250HV10、优选1400HV10的硬度。该制品具有1.7至6MPa√m、优选2至4.5MPa√m的韧度KiC。对于具有铈掺杂的钇铝石榴石的氧化铝基质，其具有大于或等于2MPa√m的韧度KiC。对于具有铈掺杂的钇铝石榴石的氧化铝和氧化锆基质，其具有大于或等于2.5MPa√m的韧度KiC。对于具有铈掺杂的钇铝石榴石的氧化锆基质，其也具有大于或等于2.5MPa√m的韧度KiC。该制品具有大于或等于95％、优选大于或等于97％、更优选大于或等于98％的密度。
具有氧化铝基质和铈掺杂的钇铝石榴石的陶瓷制品具有黄色，在CIELAB颜色空间(根据标准CIE No.15、lSO 7724/1、DIN 5033部分7、ASTM E-1164)中，分量L*大于或等于85、优选大于或等于90，分量a*为-5至15、优选-5至12，分量b*为65至110、优选70至97。
具有氧化铝与氧化锆基质和铈掺杂的钇铝石榴石的陶瓷制品也具有黄色，在CIELAB颜色空间(根据标准CIE No.15、1SO 7724/1、DIN 5033部分7、ASTME-1164)中，分量L*大于或等于85、优选大于或等于90，分量a*为-5至5、优选-5至2，分量b*为45至80、优选50至70。
该制品通过用由以下步骤组成的方法烧结来制造：
-用上文提及的不同组分并可能在液体介质中产生基础混合物，也称为第一混合物，
-形成包含第一混合物和有机粘合剂体系(石蜡、聚乙烯、聚乙酸乙烯酯等)的第二混合物，
-将所述第二混合物造粒，并在需要的情况下干燥所述第二混合物，例如在雾化器中。优选地，颗粒具有10至100μm、优选40至60μm的尺寸d50，
-通过使第二粒状混合物具有所需物品的形状，例如通过注射或压制来形成坯料。优选地，通过单轴压制和/或冷等静压(CIP)来进行成形，
-在空气中在1500至1800℃、优选1600至1700℃的保持温度下烧结该坯料20分钟至20小时、优选1至5小时。该步骤使得可以实现与理论密度相比大于97％的致密化。在该步骤之前可以进行在200至1200℃的温度范围内的热脱脂步骤，在注塑的情况下其也可以是溶剂脱脂，
-任选地，在比烧结温度低50℃至150℃的温度下用热等静压(HIP)压制该坯料以改善该坯料的最终密度。
冷却以这种方式获得的坯料。如果需要的话，可以随后对其进行机械加工、抛光和装饰，以获得所需制品。由于颜色存在于坯料的主体内，这些精加工操作不改变制品的最终颜色。
对包含氧化铝和铈掺杂的钇铝石榴石的陶瓷进行测试，其中铈掺杂的钇铝石榴石(YAG：3Ce)的百分比为10至60重量％。还对包含用铈掺杂的钇铝石榴石稳定的氧化铝和氧化锆基质的陶瓷进行测试，其中铈掺杂的钇铝石榴石(YAG：3Ce)的百分比为50重量％。还对包含氧化锆基质和20重量％的铈掺杂的钇铝石榴石的陶瓷进行测试。在所有这些测试中，该掺杂相对于石榴石为3原子％，并且氧化锆是稳定的。结果显示在下表1中。硬度测量值为HV10硬度。韧度基于在硬度压痕的对角线的四个末端处的裂纹长度测量结果根据下式来确定：
其中P是施加的载荷(N)，a是半对角线(m)，且l是测得的裂纹长度(m)。
在下列条件下用CM-3610A分光光度计在抛光样品上测量Lab比色值：测量SCI(包括镜面反射率)和SCE(不包括镜面反射率)，8°的倾斜度，4毫米直径的测量区域MAV。
在空气中在1600℃至1700℃的温度下烧结样品2至4小时。获得的所有样品均具有黄色。与通过添加氧化镨着色的氧化锆的情况下大约80的L*值相比，比色法测量显示了L*值高于90的极高亮度。此外，与通过添加氧化镨着色的氧化锆的情况下大约30的b*值相比，比色法测量显示氧化铝基质的b*值高于75的极高黄色色调。这种黄色分量随着铈掺杂的钇铝石榴石含量的提高而增强。另一方面，韧度和硬度随着含量的提高而降低。随着铈掺杂的铝钇石榴石含量而变，可以由此根据应用的需要来调制性质和颜色。
对于包含氧化锆的基质，黄色不那么强烈，其b*值为50左右，但仍高于通过添加氧化镨着色的氧化锆的情况下30的值。在硬度方面，获得高于1250HV10的值。对于韧度，获得高于2.5MPa√m的值。

Claims (18)

1.由陶瓷制成的彩色制品，所述陶瓷包含基于氧化物的基质和掺杂或共掺杂的铝石榴石族组分。
2.根据权利要求1的制品，其特征在于所述陶瓷包含含量为15至95重量％的基于氧化物的基质和含量为5至85重量％的掺杂或共掺杂的铝石榴石族组分。
3.根据权利要求1或2的制品，其特征在于所述陶瓷包含含量为30至95重量％的基于氧化物的基质和含量为5至70重量％的掺杂或共掺杂的铝石榴石族组分。
4.根据权利要求1或2的制品，其特征在于铝石榴石族组分掺杂或共掺杂有一种或多种元素，其中所有元素相对于铝石榴石族组分的总原子百分比为0.1至50％。
5.根据权利要求1或2的制品，其特征在于掺杂或共掺杂的铝石榴石族组分包含镥铝石榴石和钇铝石榴石，并且其特征在于掺杂或共掺杂元素选自铬或镧系家族的元素。
6.根据权利要求5的制品，其特征在于镧系家族的元素选自铈、钕、铒、钬和镱。
7.根据权利要求6的制品，其特征在于对于钕掺杂，相对于铝石榴石族组分的原子百分比为0.5至10％。
8.根据权利要求6的制品，其特征在于对于钕掺杂，相对于铝石榴石族组分的原子百分比为0.9至11％。
9.根据权利要求1或2的制品，其特征在于所述陶瓷包含基于氧化铝、氧化锆或稳定的氧化锆或这些氧化物的混合物的基质。
10.根据权利要求6的制品，其特征在于所述陶瓷包含基于氧化铝的基质和任选含有共掺杂元素的铈掺杂的钇铝石榴石。
11.根据权利要求1或2的制品，其特征在于所述陶瓷由基于氧化物的基质和掺杂或共掺杂的铝石榴石族组分和可能的杂质组成。
12.根据权利要求1或2的制品，其特征在于所述陶瓷在CIELAB颜色空间中具有大于或等于80的分量L*。
13.根据权利要求10的制品，其特征在于所述陶瓷在CIELAB颜色空间中具有-5至15的分量b*。
14.根据权利要求1或2的制品，其特征在于所述陶瓷具有大于或等于1000HV10的硬度。
15.根据权利要求1或2的制品，其特征在于所述陶瓷具有1.7至6MPa√m的韧度KiC。
16.根据权利要求1或2的制品，其特征在于其包括钟表外壳或机芯的组件或珠宝的组件。
17.制造根据权利要求1至16任一项的制品的方法，包括以下步骤：
-用权利要求1至11任一项的氧化物和掺杂或共掺杂的铝石榴石族组分产生基础混合物，也称为第一混合物，并且所述步骤任选在液体介质中进行，
-形成包含第一混合物和有机粘合剂体系的第二混合物，
-将所述第二混合物造粒，
-形成具有所述制品的形状的坯料，
-在空气中在1500至1800℃的保持温度下烧结所述坯料20分钟至20小时的时间。
18.根据权利要求17的方法，其特征在于其在烧结步骤之后包括在比烧结温度低50℃至150℃的温度下的热等静压(HIP)步骤。
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