CN114656802A - 一种蓝色陶瓷颜料及其制备方法 - Google Patents

一种蓝色陶瓷颜料及其制备方法 Download PDF

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CN114656802A
CN114656802A CN202210261539.7A CN202210261539A CN114656802A CN 114656802 A CN114656802 A CN 114656802A CN 202210261539 A CN202210261539 A CN 202210261539A CN 114656802 A CN114656802 A CN 114656802A
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罗文钦
阿尔法
巫海燕
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Abstract

本发明公开了一种蓝色陶瓷颜料及其制备方法。蓝色陶瓷颜料的化学组成为Mg1+xAl2‑ 2xSixO4:yCo(x=0.05‑0.95,y=0‑0.9),将Mg、Al、Si、Co原料及矿化剂混合均匀,在1100‑1500℃之间煅烧1‑10小时得到最终产品。本发明通过在Co掺杂MgAl2O4中共掺杂Si,以调控Co2+离子周围的晶体场环境,从而在低钴含量的条件下实现颜料高的蓝色度。本发明制备的蓝色陶瓷颜料在钴组分含量为5wt%时其蓝色坐标就接近于CoAl2O4,具有呈色性好、价格低、毒性低的优点,可以取代CoAl2O4颜料用于不同行业。

Description

一种蓝色陶瓷颜料及其制备方法
技术领域
本发明属于耐高温颜料技术领域,具体涉及一种蓝色陶瓷颜料及其制备方法。
背景技术
耐高温颜料是有色玻璃、陶瓷、塑料的重要组成部分。相比于普通的颜料,高温颜料在使用过程中需要经过高温煅烧的阶段,这进一步缩小了高温颜料可选择的范围。目前,市面上使用的高温颜料大部分都是十九世纪到上世纪六十年代发展起来的。随着社会的发展,人们对颜色的要求也越来越高。但是,近年来高温颜料的研究却严重滞后,各种新型高温颜料的开发屈指可数。蓝色是日常生活中常见的主色之一,它是红绿蓝光的三原色中的一元,在这三种原色中它的波长最短,为440~475nm,属于短波长。陶瓷颜料中常见的蓝色有钴蓝,海军蓝,孔雀蓝,宝石蓝等品种,其中尤以钴蓝的市场需求最大,而且钴蓝的色调也呈现出鲜艳明亮的大蓝色。钴蓝的化学式为CoAl2O4,属于尖晶石相,其显著特点是具有很好的耐热性、耐光性、耐候性和耐化学品性。但是随着锂电池的发展,工业上对于Co原料的需求量急剧增长,导致Co原料价格也随之增长。CoAl2O4作为现今最重要的蓝色颜料,其应用也受到限制。很多研究者也在尝试开发新型低钴蓝色陶瓷颜料,但总体进展缓慢。为了降低蓝色颜料中Co的含量,很多研究者用部分的Zn2+,Mg2+等二价离子取代Co2+。但是,取代后得到的颜料的蓝色度降低,降低了颜料的着色能力。如何降低颜料中Co2+含量的同时而不降低颜料的蓝色度是目前颜料开发工作者需要解决的问题。
发明内容
本发明的目的在于提供一种蓝色陶瓷颜料及其制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种蓝色陶瓷颜料,化学组成为Mg1+ xAl2-2xSixO4:yCo,其中0.05≤X≤0.95,0≤y≤0.9。
一种蓝色陶瓷颜料的制备方法,包括以下步骤:
S1:按照化学计量比,将Mg、Al、Si、Co原料及矿化剂混合均匀;
S2:将混合粉体煅烧;
S3:得到的产物重新粉碎,用水洗涤;
S4:水洗后的产品干燥得到最终产品。
优选的是,在步骤S1中,所述Mg、Al、Si、Co原料为Mg、Al、Si、Co的氧化物、硝酸盐、碳酸盐、醋酸盐。
上述任一方案中优选的是,在步骤S1中,所述矿化剂为NaCl、KCl、LiCl、碳酸钠、碳酸锂、碳酸钾、氧化钙中的一种或几种的组合。
上述任一方案中优选的是,在步骤S1中,所述矿化剂的加入量为Mg、Al、Si、Co原料总重的0-20%。
上述任一方案中优选的是,所述矿化剂的加入量为Mg、Al、Si、Co原料总重的3%。
上述任一方案中优选的是,在步骤S4中,所述干燥的温度设置为40-150℃。
上述任一方案中优选的是,在步骤S4中,所述洗涤次数1-5次。
上述任一方案中优选的是,在步骤S2中,所述煅烧时间为1-10h。
上述任一方案中优选的是,在步骤S2中,所述煅烧温度设置为1100-1500℃。
本发明的技术效果和优点:1、本发明的蓝色颜料通过MgAl2O4中掺杂Co2+离子,实现颜料蓝色显色,颜料中Co的含量从CoAl2O4的33.3wt%降低为2wt%左右(以Mg1.2Al1.6Si0.2Co0.05O4计算);
2、在掺杂Co中的同时,我们掺杂少量的Si4+可以明显提高颜料的显色度,实验表明,Mg1.2Al1.6Si0.2Co0.05O4具有和CoAl2O4相近的蓝色显色指数。
附图说明
图1为本发明1400℃煅烧的Mg1.2Al1.6Si0.2Co0.05O4陶瓷颜料的X-射线粉末衍射(XRD)图;
图2为本发明1400℃煅烧的Mg1.2Al1.6Si0.2Co0.05O4陶瓷颜料的扫描电镜照片;
图3为本发明为Mg1.2Al1.6Si0.2Co0.05O4陶瓷颜料的漫反射光谱。
如图1所示,获得样品的主要晶相为MgAl2O4尖晶石相。
如图2所示,样品的颗粒尺寸在40微米左右,粒径分布均匀。
如图3所示,样品在420-720nm处有强的吸收,峰值在600nm,同时,样品在720-1000nm近红外区有强的反射,通过柯尼卡分光测色仪(CM-5)测试,样品的色度参数为L=45.21,a=12.11,b=-46.09。
具体实施方式
下面结合附图对本发明的具体实施方式作进一步说明。在此需要说明的是,对于这些实施方式的说明用于帮助理解本发明,但并不构成对本发明的限定。此外,下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
在本发明的描述中,需要理解的是,术语“中心”、“纵向”、“横向”、“长度”、“宽度”、“厚度”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”“内”、“外”、“顺时针”、“逆时针”、“轴向”、“径向”、“周向”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。
此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括至少一个该特征。
本发明提供了如图1-3所示的一种蓝色陶瓷颜料,化学组成为Mg1+xAl2-2xSixO4:yCo,其中0.05≤X≤0.95,0≤y≤0.9。
一种蓝色陶瓷颜料的制备方法,包括以下步骤:
S1:按照化学计量比,将Mg、Al、Si、Co原料及矿化剂混合均匀,Mg、Al、Si、Co原料为Mg、Al、Si、Co的氧化物、硝酸盐、碳酸盐、醋酸盐,矿化剂为NaCl、KCl、LiCl、碳酸钠、碳酸锂、碳酸钾、氧化钙中的一种或几种的组合,矿化剂的加入量为Mg、Al、Si、Co原料总重的0-20%;
S2:将混合粉体煅烧,煅烧温度设置为1100-1500℃,煅烧时间为1-10h;
S3:得到的产物重新粉碎,用水洗涤,洗涤次数1-5次;
S4:水洗后的产品干燥得到最终产品,干燥的温度设置为40-150℃。
实施例1:Mg1.2Al1.6Si0.2Co0.05O4的制备
准确称取2.358g MgO,3.976g Al2O3,0.586g SiO2,1.091g Co(NO3)2,放入研砵中,加入适量的无水乙醇研磨混合均匀。研磨好的混合粉体放入刚玉坩埚中,在80℃干燥2小时。干燥好的样品转移到放入马弗炉中,在800℃煅烧3小时,冷却到常温后再次研磨混合均匀。再次在1400℃煅烧5小时。冷却后研磨成细粉,用水洗涤遍,在80℃干燥12小时得到最终产品。
图1为1400℃煅烧的Mg1.2Al1.6Si0.2Co0.05O4陶瓷颜料的X-射线粉末衍射(XRD)图,如图1所示,获得样品的主要晶相为MgAl2O4尖晶石相。图2为1400℃煅烧的Mg1.2Al1.6Si0.2Co0.05O4陶瓷颜料的扫描电镜照片,如图2所示,样品的颗粒尺寸在40微米左右,粒径分布均匀。图3为Mg1.2Al1.6Si0.2Co0.05O4陶瓷颜料的漫反射光谱,如图3所示,样品在420-720nm处有强的吸收,峰值在600nm。同时,样品在720-1000nm近红外区有强的反射。通过柯尼卡分光测色仪(CM-5)测试,样品的色度参数为L=45.21,a=12.11,b=-46.09。
实施例2:Mg1.4Al1.2Si0.4Co0.05O4的制备
准确称取2.751g MgO,2.982g Al2O3,1.172g SiO2,1.091g Co(NO3)2,放入研砵中,加入适量的无水乙醇研磨混合均匀。研磨好的混合粉体放入刚玉坩埚中,在80℃干燥2小时。干燥好的样品转移到放入马弗炉中,在800℃煅烧3小时,冷却到常温后再次研磨混合均匀。再次在1400℃煅烧5小时。冷却后研磨成细粉,用水洗涤遍,在60℃干燥24小时得到最终产品。通过柯尼卡分光测色仪(CM-5)测试,样品的色度参数为L=44.78,a=4.43,b=-30.62。
实施例3:Mg1.2Al1.6Si0.2Co0.01O4的制备
准确称取2.394g MgO,3.997g Al2O3,0.589g SiO2,0.437g Co(NO3)2,放入研砵中,加入适量的无水乙醇研磨混合均匀。研磨好的混合粉体放入刚玉坩埚中,在80℃干燥2小时。干燥好的样品转移到放入马弗炉中,在800℃煅烧3小时,冷却到常温后再次研磨混合均匀。再次在1400℃煅烧5小时。冷却后研磨成细粉,用水洗涤遍,在80℃干燥12小时得到最终产品。通过柯尼卡分光测色仪(CM-5)测试,样品的色度参数为L=60.56,a=5.36,b=-23.22。
实施例4:Mg1.2Al1.6Si0.2Co0.05O4的制备
准确称取2.358g MgO,3.976g Al2O3,0.586g SiO2,1.091g Co(NO3)2,0.24g NaCl放入研砵中,加入适量的无水乙醇研磨混合均匀。研磨好的混合粉体放入刚玉坩埚中,在80℃干燥2小时。干燥好的样品转移到放入马弗炉中,在800℃煅烧3小时,冷却到常温后再次研磨混合均匀。再次在1200℃煅烧8小时。冷却后研磨成细粉,用水洗涤遍,在100℃干燥8小时得到最终产品。通过柯尼卡分光测色仪(CM-5)测试,样品的色度参数为L=58.77,a=1.43,b=-45.53。
实施例5:Mg1.2Al1.6Si0.2Co0.05O4的制备
准确称取2.358g MgO,3.976g Al2O3,0.586g SiO2,1.091g Co(NO3)2,0.40gNa2CO3放入研砵中,加入适量的无水乙醇研磨混合均匀。研磨好的混合粉体放入刚玉坩埚中,在80℃干燥2小时。干燥好的样品转移到放入马弗炉中,在800℃煅烧3小时,冷却到常温后再次研磨混合均匀。再次在1300℃煅烧4小时。冷却后研磨成细粉,用水洗涤遍,在150℃干燥5小时得到最终产品。通过柯尼卡分光测色仪(CM-5)测试,样品的色度参数为L=61.43,a=6.32,b=-40.15。
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。

Claims (10)

1.一种蓝色陶瓷颜料,其特征在于:化学组成为Mg1+xAl2-2xSixO4:yCo,其中0.05≤X≤0.95,0≤y≤0.9。
2.一种根据权利要求1所述的蓝色陶瓷颜料的制备方法,其特征在于:包括以下步骤:
S1:按照化学计量比,将Mg、Al、Si、Co原料及矿化剂混合均匀;
S2:将混合粉体煅烧;
S3:得到的产物重新粉碎,用水洗涤;
S4:水洗后的产品干燥得到最终产品。
3.根据权利要求2所述的一种蓝色陶瓷颜料的制备方法,其特征在于:在步骤S1中,所述Mg、Al、Si、Co原料为Mg、Al、Si、Co的氧化物、硝酸盐、碳酸盐、醋酸盐。
4.根据权利要求2所述的一种蓝色陶瓷颜料的制备方法,其特征在于:在步骤S1中,所述矿化剂为NaCl、KCl、LiCl、碳酸钠、碳酸锂、碳酸钾、氧化钙中的一种或几种的组合。
5.根据权利要求3所述的一种蓝色陶瓷颜料的制备方法,其特征在于:在步骤S1中,所述矿化剂的加入量为Mg、Al、Si、Co原料总重的0-20%。
6.根据权利要求5所述的一种蓝色陶瓷颜料的制备方法,其特征在于:所述矿化剂的加入量为Mg、Al、Si、Co原料总重的3%。
7.根据权利要求2所述的一种蓝色陶瓷颜料的制备方法,其特征在于:在步骤S4中,所述干燥的温度设置为40-150℃。
8.根据权利要求2所述的一种蓝色陶瓷颜料的制备方法,其特征在于:在步骤S4中,所述洗涤次数1-5次。
9.根据权利要求2所述的一种蓝色陶瓷颜料的制备方法,其特征在于:在步骤S2中,所述煅烧时间为1-10h。
10.根据权利要求2所述的一种蓝色陶瓷颜料的制备方法,其特征在于:在步骤S2中,所述煅烧温度设置为1100-1500℃。
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