CN111848159A - 一种黄色导电氧化锆陶瓷的制备方法 - Google Patents

一种黄色导电氧化锆陶瓷的制备方法 Download PDF

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CN111848159A
CN111848159A CN202010750790.0A CN202010750790A CN111848159A CN 111848159 A CN111848159 A CN 111848159A CN 202010750790 A CN202010750790 A CN 202010750790A CN 111848159 A CN111848159 A CN 111848159A
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powder
conductive
yellow
zirconia
zirconia ceramic
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常鑫烽
王春华
茹红强
王晓
孙卫康
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Weifang Dongda Electronic Materials Co ltd
Shandong Dongda New Materials Research Institute Co ltd
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Weifang Dongda Electronic Materials Co ltd
Shandong Dongda New Materials Research Institute Co ltd
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Abstract

本发明公开一种黄色导电氧化锆陶瓷的制备方法，包括如下步骤：将氧化锆粉、导电粉、钛源、碳源、添加剂混合，得到混合料；混合料与结合剂、液体介质一起混合成浆料，在球磨罐中球磨或在砂磨机中研磨；所述氧化锆粉、导电粉、钛源、碳源、添加剂的质量配比为(25‑75):(0‑60):(5‑30):(5‑20):(0‑5)。所述氧化锆陶瓷的颜色为土豪金、玫瑰金、卡其色或渐变色，电阻率为0.3μΩ·m‑10Ω·m。本发明制备方法，工艺简单、便于批量化生产；可使氧化锆陶瓷不仅导电，还可以拥有多种黄色色彩，具有金属电学特性和陶瓷结构特性于一体的高性能功能复合导电陶瓷材料，具有卓越的导电性能且电阻率可调。

Description

一种黄色导电氧化锆陶瓷的制备方法
技术领域
本发明属于导电陶瓷材料的技术领域，特别涉及一种黄色导电氧化锆陶瓷的制备方法。
技术背景
氧化锆陶瓷具有强度高、硬度高、耐磨损、耐化学腐蚀等优良的特性，已被广泛应用在珠宝装饰、智能手机后盖和手表表壳等领域，展现出巨大的市场商机。彩色氧化锆陶瓷通常是添加色釉、在氧化气氛中烧结获得，不仅导电性能较差，且色度波动较大，只能作为结构件。氧化锆陶瓷结构与功能不能兼得的问题导致其在智能穿戴、电子消费产品领域的深层次价值得不到充分的发掘利用。
现有专利CN201810437739.7公开了一种黄色氧化锆陶瓷的制备方法，具体按照以下步骤实施：步骤1，将经钇稳定的氧化锆粉料和氧化钒或钒酸铵在球磨机中进行混合，并加入分散剂进行球磨，混合均匀干燥后研磨，获得黄色氧化锆陶瓷粉体；步骤2，将制得的黄色氧化锆粉体在马弗炉中于1180℃进行预煅烧2-5h，随后随炉冷却至室温，得到钒锆固溶体；步骤3，将制得的钒锆固溶体研磨粉碎，造粒后，采用干压或冷等静压成型获得黄色氧化锆素坯；步骤4，将制得的氧化锆陶瓷素坯经高温烧结得到黄色氧化锆陶瓷。本发明的黄色氧化锆陶瓷的制备方法，通过着色剂氧化钒或钒酸铵与钇稳定氧化锆预烧形成钒锆固溶体，提高氧化钒的高温稳定性，实现黄色氧化锆陶瓷的成功制备。
现有专利CN201911213134.0涉及一种黄色氧化锆陶瓷用粉体的制备方法，特征是:包括S1:取如下质量份物料：0.28～0.32份MgO、0.19～0.25份Al2O3、0.33～0.37份SiO2、2.9～3.2份Y2O3、0.48～0.52份Pr6O11、95～96份ZrO2，搅拌形成混合料；S2：取如下质量份物料：10～14份研磨介质、1.2～1.5份去离子水及0.8～1.2份S1中混合料，放入球磨罐，加氨水调节pH至9～12，加入0.01～0.02份分散剂，将浆料球磨至D50≤0.4μm；S3：将S2中浆料在80～150℃下烘干，再研磨到D50≤0.2mm，得到产物粉体。其工艺极其简单、原料成本低。还提供一种通过上述制备方法制得的黄色氧化锆陶瓷用粉体，此粉体为紫灰色，烧结后形成黄色氧化锆陶瓷，不用染色；一种黄色氧化锆陶瓷，其力学性能优越，抗弯强度高、硬度高，断裂韧性好，工艺简单、可操作性强。
现有技术的黄色氧化锆陶瓷的制备方法，黄色氧化锆陶瓷结构与功能不能兼得，电阻率可调性差，化学稳定性低，力学性能不理想。
发明内容
本发明的目的是针对现有的问题，提供了一种黄色导电氧化锆陶瓷的制备方法，并达到以下发明目的：制备的黄色氧化锆陶瓷，颜色可以为土豪金、玫瑰金、卡其色、渐变色等多种时尚流行黄色色彩，电阻率可调性高且化学稳定性高、抗高温氧化、耐磨损、力学性能优异。
为实现上述目的，本发明采取的技术方案如下：
一种黄色导电氧化锆陶瓷的制备方法，步骤如下：
（1）将氧化锆粉、导电粉、钛源、碳源、添加剂混合，得到混合料；
混合料与结合剂、液体介质一起混合成浆料，在球磨罐中球磨或在砂磨机中研磨。
所述氧化锆粉、导电粉、钛源、碳源、添加剂的质量配比为(25-75):(0-60):(5-30):(5-20):(0-5)。
所述氧化锆粉：平均粒度为0.5nm-5μm，氧化锆含量大于90%，还含有稳定剂，稳定剂含量为1-10%；稳定剂为CaO、MgO、Y2O3、CeO2中的一种。
所述导电粉可以是氮化钛、氮化锆、碳氮化钛、碳化钛、碳化锆、碳化铊、碳化铪、硼化钛、硼化锆、硼化铊、硼化铪、硅化钼、碳化钨中的一种。
所述钛源可以是Ti粉、TiCl4、TiO2粉、钛酸丁酯中的一种。
所述碳源可以是酚醛树脂、绵白糖、碳黑、石墨烯、碳化硼中的一种。
所述添加剂可以是氧化锰、氧化锌、氧化硅、氧化镍、氧化铝、氧化钴、氧化铬、氧化钒、氧化镧、氧化铪中的一种。
所述结合剂可以是酚醛树脂、PVA、PVB或其它有机胶。
所述液体介质可以是水、乙醇或汽油。
所述结合剂的用量为混合料质量的5-15%，液体介质的用量为混合料质量的80-200%。
（2）将混合浆料进行喷雾造粒或在40-100℃干燥箱中烘干后摇摆造粒机过筛造粒，得到造粒粉；造粒粉粒径为50-150目。
（3）将造粒粉放入模具中，经过模压成型制成陶瓷生坯；模压成型的压力为50-250MPa。
（4）将压制好的陶瓷生坯放入60-200℃干燥箱中干燥；
（5）将干燥后的生坯烧结，1550-1850℃反应烧结获得黄色导电氧化锆陶瓷。烧结气氛可以是氮气、氨气、氯化铵。
所述氧化锆陶瓷的颜色可以为土豪金、玫瑰金、卡其色、渐变色等多种黄色色彩，电阻率为0.3μΩ·m-10Ω·m。
与现有技术相比，本发明的优点在于：
（1）本发明黄色导电氧化锆陶瓷是具有金属电学特性和陶瓷结构特性于一体的高性能功能复合导电陶瓷材料，具有卓越的导电性能且电阻率可调，颜色可以为土豪金、玫瑰金、卡其色、渐变色等多种时尚流行黄色色彩。本发明制备的黄色导电氧化锆陶瓷，电阻率在0.3μΩ·m-10Ω·m范围内可调。
（2）本发明制备的黄色导电氧化锆陶瓷，具有化学稳定性高、抗高温氧化、耐磨损、综合力学性能优异的优势；弯曲强度为582-746MPa，断裂韧性为7.43-8.75MPa·m1/2，维氏硬度为15.76-17.43GPa，相对密度为98.81-99.53%，气孔率为0.14-0.62%。
（3）本发明特定的制备工艺，可以制备出电阻率可调、形状可塑、色彩多样的产品，工艺简单，对设备要求度低，便于大规模自动化生产，产品成本低，具有巨大的市场实用价值。
在原料中，引入原位合成源，通过反应烧结，在氧化锆陶瓷基体中原位反应生成导电相与原料中导电相结合，显著降低氧化锆陶瓷的电阻率从而具有卓越的导电性能。原位反应生成导电相的引入，起到颗粒强化作用，可明显改善氧化锆陶瓷的抗弯强度、断裂韧性和维氏硬度。原料中引入添加剂，在氮气、氨气、氯化铵气氛中烧结，获得土豪金、玫瑰金、卡其色、渐变色等多种黄色色彩。本发明黄色导电氧化锆陶瓷是具有金属电学特性和陶瓷结构特性于一体的高性能功能复合导电陶瓷材料，具有卓越的导电性能(电阻率低至10-7Ω·m)且电阻率可调、化学稳定性高、抗高温氧化、耐磨损、综合力学性能优异的优势，颜色可以为多种时尚流行黄色色彩。黄色导电氧化锆陶瓷在智能穿戴、电子消费产品领域具有巨大的应用前景。
附图说明
图1为本发明实施例1中制备的玫瑰金导电氧化锆陶瓷金相图片；
图2为本发明实施例1中制备的玫瑰金导电氧化锆陶瓷色差仪测量参数；
图3为本发明实施例2中制备的土豪金导电氧化锆陶瓷金相图片；
图4为本发明实施例2中制备的土豪金导电氧化锆陶瓷色差仪测量参数；
图5为本发明实施例3中制备的渐变色导电氧化锆陶瓷金相图片；
图6为本发明实施例3中制备的渐变色导电氧化锆陶瓷色差仪测量参数。
具体实施方式
以下结合具体实施例，对本发明做进一步说明。应理解，以下实施例仅用于说明本发明而非用于限制本发明的范围。
实施例1
一种黄色导电氧化锆陶瓷的制备方法，步骤如下：
（1）将氧化锆粉、碳化钛粉、Ti粉、石墨烯、氧化铪按质量比60:32:15:5:3混合，得到混合料；
所述氧化锆粉: 氧化锆含量为95%，平均粒径0.5nm，含有稳定剂Y2O3，含量为5%；
混合料与与结合剂、去离子水一起混合成浆料，在球磨罐中球磨12h。
所述结合剂：为PVA，质量百分浓度为5.0%，结合剂用量为混合料质量的6%；
所述水的用量为混合料质量的120%。
（2）将球磨后的浆料在80℃干燥，通过摇摆造粒机过筛造粒；得到造粒粉；所述过筛：过筛筛网为80目。
（3）将造粒粉放入模具中，经压力机模压成型，压力150MPa，获得生坯；
（4）将压制好的陶瓷生坯放入150℃干燥箱中干燥12h排出体内水分；
（5）将生坯在氮气气氛下进行烧结，在1100℃保温120min，达到烧结温度1650℃时，保温90min，获得玫瑰金色导电氧化锆陶瓷。
经测试，该玫瑰金色导电氧化锆陶瓷的弯曲强度为651MPa，断裂韧性为8.75MPa·m1/2，维氏硬度为16.52GPa，相对密度为98.81%，气孔率为0.62%，电阻率为8.2×10-6Ω·m；色差仪测量色度参数值分别为：L=61.18，a=10.98，b=15.56，c=19.05，h=54.78。
实施例2
一种黄色导电氧化锆陶瓷的制备方法，步骤如下：
（1）将氧化锆粉、氮化钛粉、氧化钛粉、酚醛树脂、氧化铝按质量比35:55:25:15:5混合，得到混合料；
所述氧化锆粉: 氧化锆含量为90%，平均粒径1μm，含有稳定剂CeO2，含量为10%；
混合料与结合剂、水一起混合成浆料，在砂磨机中研磨3h。
所述结合剂：为PVB，质量百分浓度为5.0%，结合剂用量为混合料质量的10%；
所述水的用量为混合料质量的150%。
（2）将球磨后的浆料进行喷雾造粒，过筛得到60-100目粒径造粒粉。
（3）将造粒粉放入模具中，经压力机模压成型，压力250MPa，获得生坯。
（4）将压制好的陶瓷生坯放入200℃干燥箱中干燥15h排出体内水分。
（5）将生坯在氨气气氛下进行烧结， 1150℃保温150min，达到烧结温度1750℃时，保温150min，获得土豪金色导电氧化锆陶瓷。
经测试，该土豪金色导电氧化锆陶瓷的弯曲强度为582MPa，断裂韧性为7.43MPa·m1/2，维氏硬度为17.43GPa，相对密度为99.14%，气孔率为0.38%，电阻率为6.9×10-7Ω·m；色差仪测量色度参数值分别为：L=65.17，a=5.96，b=18.15，c=19.11，h=71.82。
实施例3
一种黄色导电氧化锆陶瓷的制备方法，步骤如下：
（1）将氧化锆粉、碳氮化钛粉、钛酸丁酯、炭黑、氧化镧按质量比70:25:30:10:2混合，得到混合料；
所述氧化锆粉: 氧化锆含量为98%，平均粒径5μm，含有稳定剂MgO，含量为2%；
混合料与结合剂、无水乙醇一起混合成浆料，在球磨罐中球磨3h。
所述结合剂：为酚醛树脂，质量百分浓度为10.0%；结合剂用量为混合料质量的15%；
所述无水乙醇用量为混合料质量的200%。
（2）将球磨后的浆料进行喷雾造粒；
（3）将造粒粉放入模具中，经压力机模压成型，压力200MPa，获得生坯；
（4）将压制好的陶瓷生坯放入120℃干燥箱中干燥24h排出体内水分；
（5）将生坯在氯化铵气氛下进行烧结，在950℃保温60min，达到烧结温度1820℃时，保温120min，获得渐变色（土豪金与玫瑰金混合渐变的一种颜色）导电氧化锆陶瓷。
经测试，该渐变色导电氧化锆陶瓷的弯曲强度为746MPa，断裂韧性为7.78MPa·m1 /2，维氏硬度为15.76GPa，相对密度为99.53%，气孔率为0.14%，电阻率为4.3×10-6Ω·m；色差仪测量色度参数值分别为：L=59.11，a=9.62，b=10.66，c=14.36，h=47.93。
除特殊说明外，本发明所述的百分数均为质量百分数，所述的比值均为质量比。
以上所述，仅为本发明的实施例，并非用以限定本发明的范围，本发明的上述实施例还可以做出各种变化。凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰，皆落入本发明专利的权利要求保护范围。本发明未详尽描述的均为常规技术内容。

Claims (10)

1.一种黄色导电氧化锆陶瓷的制备方法，其特征在于，包括如下步骤：
将氧化锆粉、导电粉、钛源、碳源、添加剂混合，得到混合料；混合料与结合剂、液体介质一起混合成浆料，在球磨罐中球磨或在砂磨机中研磨；所述氧化锆粉、导电粉、钛源、碳源、添加剂的质量配比为(25-75):(0-60):(5-30):(5-20):(0-5)。
2.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：所述氧化锆陶瓷的颜色为土豪金、玫瑰金、卡其色或渐变色，电阻率为0.3μΩ·m-10Ω·m。
3.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：还包括：将研磨后的混合浆料进行造粒；造粒粉粒径为50-150目。
4.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：还包括：将造粒粉放入模具中，经过模压成型制成陶瓷生坯；模压成型的压力为50-250MPa。
5.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：还包括：将陶瓷生坯干燥，干燥温度为60-200℃。
6.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：还包括：将干燥后的生坯反应烧结获得黄色导电氧化锆陶瓷；所述反应烧结：温度为1550-1850℃，烧结气氛为氮气、氨气或氯化铵。
7.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：
所述氧化锆粉：平均粒度为0.5nm-5μm，氧化锆含量大于90%，还含有稳定剂，稳定剂含量为1-10%；稳定剂为CaO、MgO、Y2O3、CeO2中的一种。
8.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：
所述导电粉为氮化钛、氮化锆、碳氮化钛、碳化钛、碳化锆、碳化铊、碳化铪、硼化钛、硼化锆、硼化铊、硼化铪、硅化钼、碳化钨中的一种。
9.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：
所述钛源为Ti粉、TiCl4、TiO2粉、钛酸丁酯中的一种；所述碳源可以是酚醛树脂、绵白糖、碳黑、石墨烯、碳化硼中的一种。
10.根据权利要求1所述的一种黄色导电氧化锆陶瓷的制备方法，其特征在于：
所述添加剂为氧化锰、氧化锌、氧化硅、氧化镍、氧化铝、氧化钴、氧化铬、氧化钒、氧化镧、氧化铪中的一种；
所述结合剂为酚醛树脂、PVA、PVB或其它有机胶。
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