CN113582686A - 一种蓝色氧化锆陶瓷的制备方法 - Google Patents

一种蓝色氧化锆陶瓷的制备方法 Download PDF

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CN113582686A
CN113582686A CN202110859970.7A CN202110859970A CN113582686A CN 113582686 A CN113582686 A CN 113582686A CN 202110859970 A CN202110859970 A CN 202110859970A CN 113582686 A CN113582686 A CN 113582686A
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蒋朋
程秋雨
陈新
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University of Science and Technology Beijing USTB
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Abstract

本发明公开了一种蓝色氧化锆陶瓷的制备方法，属于无机颜料和彩色氧化锆陶瓷技术领域。蓝色陶瓷的制备步骤为：先以BaCO3，MgO，Al2O3，NiO或Co3O4为原料，按照Ba0.956Mg0.912Al10.088‑xNixO17(0≤x≤0.3)和Ba0.956Mg0.912Al10.088‑xCoxO17(0≤x≤0.3)的化学计量比进行混料、研磨、压块、烧结制备蓝色颜料；再按照颜料相与氧化锆相质量配比1：9进行混料。用行星式球磨机在200‑500r/min的转速下干磨4‑12h，在200‑500r/min的转速下湿磨20‑80min。将混合均匀的原料混料放入烘箱中，在50‑80℃下干燥6‑12h。烘干后的原料在10‑30MPa压力下压片并保压1‑5min。随后在箱式炉中进行高温烧结，烧结温度为1200‑1650℃，烧结时间为2‑12h，升温速率为5‑10℃/min，降温速率为5‑10℃/min。本发明合成的蓝色氧化锆陶瓷，环保无毒，色泽明亮，制备工艺简单，硬度稳定并且具有良好的结构稳定性。

Description

一种蓝色氧化锆陶瓷的制备方法
技术领域
本发明涉及无机颜料和彩色氧化锆陶瓷技术领域，公开了一种环保无毒，色泽明亮，制备工艺简单，具有良好的结构稳定性和较高硬度的蓝色氧化锆陶瓷的制备方法。
背景技术
氧化锆陶瓷同时具有优异的物理和化学性能，广泛用于牙齿种植、手机背板等领域。彩色氧化锆陶瓷的合成可以通过向氧化锆分体中添加颜料粉体实现，但是由于氧化锆陶瓷的烧结温度高(1500-1600℃)，大部分颜料粉体在高温下存在高挥发性、有毒前体或分解的问题，导致颜色消失，因此满足要求的颜料非常有限。目前工业上应用最广泛的蓝色氧化锆陶瓷块体制备方法是利用氧化钴(Co2O3)合成钴蓝(CoAl2O4)之后进一步合成蓝色氧化锆陶瓷。由于钴蓝(CoAl2O4)含有大量的钴，钴的储量少且有毒，因此探索一种新的钴含量较低的蓝色颜料及其作为蓝色发色团制备新型蓝色氧化锆陶瓷显得尤为重要。
发明内容
为了解决目前蓝色氧化锆陶瓷着色剂可选范围小的问题，本发明的内容是以合成的Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)或Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)蓝色颜料粉体为着色剂，选择Y-ZrO2粉体，按照颜料相与氧化锆相1：9的质量配比，制备得到蓝色氧化锆陶瓷块体。
一种蓝色氧化锆陶瓷的制备方法，其特征在于蓝色陶瓷的制备步骤为：先以BaCO3，MgO，Al2O3，NiO或Co3O4为原料，按照Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)或Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)的化学计量比进行混料、研磨、压块、烧结制备蓝色颜料；再按照颜料相与氧化锆相质量配比1：9进行混料、干燥、压块、烧结制备合成蓝色氧化锆陶瓷。
如上所述的一种蓝色氧化锆陶瓷的制备方法，其特征在于包括以下步骤：
(1)以蓝色颜料Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)或Ba0.956Mg0.912Al10.088- xCoxO17(0≤x≤0.3)与Y-ZrO2为原料，按照蓝色颜料与氧化锆相1：9的质量配比，用电子天平精确称取原料；
(2)将称量好的粉末原料放入球磨罐中，用行星式球磨机在室温下进行干磨和湿磨，使原料充分混合；
(3)球磨结束后，将混合好的原料放入烘箱静置烘干；
(4)将烘干的原料放入压片模具中，用压片机干压成型；
(5)将压制成型的块体放到刚玉坩埚中，按照升温曲线在箱式炉中进行高温烧结。
进一步地，步骤(1)中所述原料质量误差为±0.0005g。
进一步地，步骤(2)中所述的干磨条件为200-500r/min，4-12h；湿磨条件为200-500r/min，20-80min。
进一步地，步骤(3)中所述的在电热鼓风干燥箱中50-80℃条件下干燥6-12h。
进一步地，步骤(4)中所述的压片模具的直径为10-20mm，压样压力为10-30MPa，保压时间为1-5min。
进一步地，步骤(5)中样品的烧结温度为1200-1650℃，烧结时间为2-12h，升温速率为5-10℃/min，降温速率为5-10℃/min。
进一步地，所述蓝色颜料的制备步骤如下：
(1)以BaCO3，MgO，Al2O3，NiO或Co3O4为原料，按照颜料相的化学计量比，用电子天平精确称取原料；
(2)将称量好的粉末原料放入玛瑙研钵中研磨，使原料充分混合；
(3)研磨结束后，将混合好的原料放入压片模具中，用压片机干压成型；
(4)将压制成型的块体放到刚玉坩埚中，按照升温曲线在箱式炉中进行高温烧结，得到Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)或Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)。
进一步地，步骤(1)中所述原料质量误差为±0.0005g；步骤(2)中所述的研磨时间为20-30min；步骤(3)中所述的压片模具的直径为10-20mm，压样压力为10-30MPa，保压时间为1-5min。
进一步地，步骤(4)中样品的烧结温度为1200-1650℃，烧结时间为2-12h，烧结气氛为N2，升温速率为5-10℃/min，降温速率为5-10℃/min。
本发明的技术难点及优点：
(1)本发明制备的蓝色颜料粉体，环保无毒，色泽饱满，制备工艺简单，具有良好的结构稳定性和化学稳定性。
(2)本发明制备的蓝色颜料粉体可以用作着色剂制备蓝色氧化锆陶瓷块体。
(3)本发明的蓝色氧化锆陶瓷块体环保无毒，色泽明亮，制备工艺简单，硬度稳定并且具有良好的结构稳定性。
附图说明
图1(a)为Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)蓝色颜料粉末的XRD图谱，(b)为Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)蓝色颜料粉末的XRD图谱
图2(a)为Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)蓝色颜料粉末的UV-VIS-NIR图谱，(b)为Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)蓝色颜料粉末的UV-VIS-NIR图谱
图3为ZrO2陶瓷，10wt％Ba0.956Mg0.912Al9.988Ni0.1O17或10wt％Ba0.956Mg0.912Al9.888Co0.2O17与90wt％Y-ZrO2复合后得到的蓝色氧化锆陶瓷块体的XRD图。
图4(a)为10wt％Ba0.956Mg0.912Al9.988Ni0.1O17+90wt％Y-ZrO2蓝色氧化锆陶瓷块体的UV-VIS-NIR图谱，(b)为10wt％Ba0.956Mg0.912Al9.888Co0.2O17+90wt％Y-ZrO2蓝色氧化锆陶瓷块体的UV-VIS-NIR图谱。
表1
Figure BDA0003185345380000031
表1为ZrO2陶瓷，10wt％Ba0.956Mg0.912Al9.988Ni0.1O17或10wt％Ba0.956Mg0.912Al9.888Co0.2O17与90wt％Y-ZrO2复合后得到的蓝色氧化锆陶瓷块体的维氏硬度(单位：GPa)(打点数：12)
具体实施方式
下面结合具体实施例及附图进一步详细描述本发明。实施例仅为本发明的范例，而非限制本发明。本领域技术人员应该理解的是，在不偏离本发明的精神和范围下可以对本发明实施例的技术方案进行修改或者等同替换，但这些修改和替换均在本发明的保护范围内。
实施例1：
Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)和Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)蓝色颜料粉体的制备：以BaCO3，MgO，Al2O3，NiO或Co3O4为原料，按照颜料相的化学计量比，用电子天平精确称取原料，允许质量误差为±0.0005g。将称取好的原料放入球玛瑙研钵中，研磨20min。将混合好的原料放入压片模具中，加压至10MPa保压3min。将干压成型的块体放入管式中，在N2气氛中，以5℃/min的升温速率升温至1600℃，在1600℃下保温4h，再以5℃/min的降温速率降到室温，研磨后得到蓝色颜料粉体。
实施例2：
以Ba0.956Mg0.912Al9.988Ni0.1O17和Ba0.956Mg0.912Al9.888Co0.2O17为着色剂制备蓝色氧化锆陶瓷块体：根据10wt％Ba0.956Mg0.912Al9.988Ni0.1O17+90wt％Y-ZrO2和10wt％Ba0.956Mg0.912Al9.888Co0.2O17+90wt％Y-ZrO2的配比，用电子天平称取蓝色颜料粉体和氧化锆粉体，允许质量误差为±0.0005g。将称取好的原料放入球磨罐中，用行星式球磨机在300r/min条件下干磨10h，随后向球磨罐中加入酒精，在300r/min下湿磨30min。将球磨好的样品放入电热鼓风干燥箱中在60℃下干燥12h。将干燥好的原料放入压片模具中，加压至10MPa保压3min。将干压成型的块体放入箱式炉中，以5℃/min的升温速率升温至1400℃，在1400℃下保温6h，再以5℃/min的降温速率降到室温，最后得到蓝色氧化锆陶瓷块体。

Claims (10)

1.一种蓝色氧化锆陶瓷的制备方法，其特征在于蓝色陶瓷的制备步骤为：先以BaCO3，MgO，Al2O3，NiO或Co3O4为原料，按照Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)或Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)的化学计量比进行混料、研磨、压块、烧结制备蓝色颜料；再按照颜料相与氧化锆相质量配比1：9进行混料、干燥、压块、烧结制备合成蓝色氧化锆陶瓷。
2.如权利要求1所述的一种蓝色氧化锆陶瓷的制备方法，其特征在于包括以下步骤：
(1)以蓝色颜料Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)或Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)与Y-ZrO2为原料，按照蓝色颜料与氧化锆相1：9的质量配比，用电子天平精确称取原料；
(2)将称量好的粉末原料放入球磨罐中，用行星式球磨机在室温下进行干磨和湿磨，使原料充分混合；
(3)球磨结束后，将混合好的原料放入烘箱静置烘干；
(4)将烘干的原料放入压片模具中，用压片机干压成型；
(5)将压制成型的块体放到刚玉坩埚中，按照升温曲线在箱式炉中进行高温烧结。
3.如权利要求2所述一种蓝色氧化锆陶瓷的制备方法，其特征在于，步骤(1)中所述原料质量误差为±0.0005g。
4.如权利要求2所述一种蓝色氧化锆陶瓷的制备方法，其特征在于，步骤(2)中所述的干磨条件为200-500r/min，4-12h；湿磨条件为200-500r/min，20-80min。
5.如权利要求2所述一种蓝色氧化锆陶瓷的制备方法，其特征在于，步骤(3)中所述的在电热鼓风干燥箱中50-80℃条件下干燥6-12h。
6.如权利要求2所述一种蓝色氧化锆陶瓷的制备方法，其特征在于，步骤(4)中所述的压片模具的直径为10-20mm，压样压力为10-30MPa，保压时间为1-5min。
7.如权利要求2所述一种蓝色氧化锆陶瓷的制备方法，其特征在于，步骤(5)中样品的烧结温度为1200-1650℃，烧结时间为2-12h，升温速率为5-10℃/min，降温速率为5-10℃/min。
8.如权利要求1或2所述的蓝色氧化锆陶瓷的制备方法，其特征在于所述蓝色颜料的制备步骤如下：
(1)以BaCO3，MgO，Al2O3，NiO或Co3O4为原料，按照颜料相的化学计量比，用电子天平精确称取原料；
(2)将称量好的粉末原料放入玛瑙研钵中研磨，使原料充分混合；
(3)研磨结束后，将混合好的原料放入压片模具中，用压片机干压成型；
(4)将压制成型的块体放到刚玉坩埚中，按照升温曲线在箱式炉中进行高温烧结，得到Ba0.956Mg0.912Al10.088-xNixO17(0≤x≤0.3)或Ba0.956Mg0.912Al10.088-xCoxO17(0≤x≤0.3)。
9.如权利要求8所述的蓝色氧化锆陶瓷的制备方法，其特征在于步骤(1)中所述原料质量误差为±0.0005g；步骤(2)中所述的研磨时间为20-30min；步骤(3)中所述的压片模具的直径为10-20mm，压样压力为10-30MPa，保压时间为1-5min。
10.如权利要求8所述的蓝色氧化锆陶瓷的制备方法，其特征在于，步骤(4)中样品的烧结温度为1200-1650℃，烧结时间为2-12h，烧结气氛为N2，升温速率为5-10℃/min，降温速率为5-10℃/min。
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