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CN111747742A - 一种黑色导电氧化锆陶瓷的制备方法 - Google Patents

一种黑色导电氧化锆陶瓷的制备方法 Download PDF

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CN111747742A
CN111747742A CN202010752448.4A CN202010752448A CN111747742A CN 111747742 A CN111747742 A CN 111747742A CN 202010752448 A CN202010752448 A CN 202010752448A CN 111747742 A CN111747742 A CN 111747742A
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powder
black conductive
zirconia
oxide
zirconia ceramic
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茹红强
王春华
常鑫烽
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

本发明公开一种黑色导电氧化锆陶瓷的制备方法一种黑色导电氧化锆陶瓷的制备方法，包括如下步骤：（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；（2）将研磨后的浆料进行烘干后过筛造粒，得到造粒粉；（3）将造粒粉放入模具中，经过模压成型制成陶瓷生坯；（4）将陶瓷生坯干燥；（5）将干燥后的生坯烧结，高温反应烧结获得黑色导电氧化锆陶瓷。本发明氧化锆陶瓷具有出色的导电能力，具备结构与功能一体化特性，在智能穿戴、电子产品领域具有非常大的实用前景。

Description

一种黑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，特别涉及一种黑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。普通黑色氧化锆陶瓷通常是添加金属氧化物，在氧化气氛中或者在真空气氛下获得烧结，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。
专利CN201210077363.6公开了一种石墨烯和氧化物陶瓷复合材料及制备方法，是以氧化石墨为石墨烯前驱体，与氧化锆陶瓷粉按照一定比例混合，成型和烧结形成石墨烯和氧化锆陶瓷复合材料。由本发明制备的石墨烯和氧化锆陶瓷复合材料具有纳米片层石墨烯均匀分布于陶瓷基体构成网络连接的纳米复合结构，该纳米复合结构有利于增强陶瓷，赋予陶瓷半导体、导电、导热和电化学等功能特性，该复合材料可用于发展传感器、电磁屏蔽、电加热器件、导热材料和储能电极等，用于航空航天、电子、化工和能源领域。该石墨烯和氧化物陶瓷复合材料在烧结过程中一步形成，不需功能化和混合等过程。
专利CN201710143683.X，提供了一种高纯钇稳定氧化锆与高纯碳化硼复合的导电陶瓷制备方法，采用纳米级钇稳定氧化锆粉与纳米级碳化硼粉用高能球磨的办法对粉末进行混合并制成浆料，然后通过离心喷雾造粒的方法进行造粒，通过冷等静压压制成型，最后通过热等静压烧结的方法制成。本发明具有高致密高强度导电性好的优点，本发明不仅工艺和设备简单，成本低，收率高，能耗低，生产效率高，适合工业化生产，而且能够获得质量稳定、晶粒细小可控的氧化锆导电陶瓷，本发明过程无坏境污染，是一种新型的低成本、质量稳定的高致密高强度氧化锆导电陶瓷的制备方法。
现有技术的氧化锆导电陶瓷的制备方法，得到的氧化锆陶瓷结构与功能不能兼得，导电性能不理想，化学稳定性、抗高温氧化、耐磨损以及力学性能不佳。
发明内容
本发明的目的是针对现有技术问题，提供了一种黑色导电氧化锆陶瓷的制备方法，并达到以下发明目的：提高导电性能且电阻率可调，化学稳定性高、抗高温氧化、耐磨损、综合力学性能优异。
为实现上述目的，本发明采取的技术方案如下：
一种黑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(20-80):(0-65):(0-30):(0-15):(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或其它有机胶中的一种。结合剂用量为混合料质量的8-12%；
所述液体介质可以是水、乙醇或汽油；液体介质用量为混合料质量的80-120%。
（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）将干燥后的生坯放入烧结气氛中烧结，1500-1800℃反应烧结，获得氧化锆陶瓷。烧结气氛可以是真空、氩气、氢气。
所述氧化锆陶瓷的颜色为黑色，电阻率为0.1μΩ·m-100Ω·m。
与现有技术相比，本发明的优点在于：
（1）本发明黑色导电氧化锆陶瓷，具有卓越的导电性能，电阻率0.1μΩ·m-100Ω·m范围内可调、化学稳定性高、抗高温氧化、耐磨损、综合力学性能优异；弯曲强度为540-789MPa，断裂韧性为5.52-9.35MPa·m1/2，维氏硬度为14.34-17.35GPa，相对密度为98.12-99.54%，气孔率为0.15-1.61%。
（2）本发明黑色导电氧化锆陶瓷，色度均匀且可调，色差仪测量黑度值L=51.91-59.12。
（3）本发明制备方法，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，明显改善氧化锆陶瓷的抗弯强度、断裂韧性和维氏硬度。在原料中引入特定添加剂，在真空、氩气、氢气气氛中烧结，获得色度均匀且可调的黑色氧化锆。本发明氧化锆陶瓷具有出色的导电能力，具备结构与功能一体化特性，在智能穿戴、电子产品领域具有非常大的实用前景。
附图说明
图1为本发明制备的黑色导电氧化锆陶瓷的金相图片；
图2为本发明制备的黑色导电氧化锆陶瓷在扫描电镜下二次电子成像图片；
图3为本发明制备的黑色导电氧化锆陶瓷在扫描电镜下背散射电子成像图片；
图4为本发明实施例1中制备的黑色导电氧化锆陶瓷色差仪测量参数；
图5为本发明实施例2中制备的黑色导电氧化锆陶瓷色差仪测量参数；
图6为本发明实施例3中制备的黑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
一种黑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、TiCl4、氧化钴按质量比70:20:10:5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%；
混合料与结合剂、无水乙醇一起混合成浆料，在球磨罐中球磨12h。
所述结合剂：为酚醛树脂，质量百分浓度为8.0%；结合剂用量为混合料质量的10%；
所述无水乙醇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排出坯内水分。
（5）将干燥后的生坯进行真空烧结，在1100℃保温120min，然后在烧结温度1650℃，保温90min，获得黑色导电氧化锆陶瓷。
经测试，该黑色导电氧化锆陶瓷的弯曲强度为540MPa，断裂韧性为5.52MPa·m1/2，维氏硬度为14.34GPa，相对密度为98.12%，气孔率为1.61%，电阻率为2.5×10-4Ω·m；色差仪测量黑度值L=51.91。
实施例2
一种黑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、石墨烯、氧化铬按质量比60:40:15:10:3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8%；
所述水的用量为混合料质量的80%。
（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）将生坯放入烧结中，氩气气氛下，1150℃保温150min，达到烧结温度1750℃时，保温150min，获黑色导电氧化锆陶瓷。
经测试，该黑色金导电氧化锆陶瓷的弯曲强度为789MPa，断裂韧性为9.35MPa·m1 /2，维氏硬度为15.26GPa，相对密度为99.54%，气孔率为0.15%，电阻率为3.7×10-6Ω·m；色差仪测量黑度值L=57.75。
实施例3
一种黑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、氧化钛粉、酚醛树脂、氧化镍按质量比30:55:30:8:2.5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、水一起混合成浆料，在砂磨机中研磨3h。
所述结合剂：为PVA，质量百分浓度为10.0%，结合剂用量为混合料质量的12%；
所述水的用量为混合料质量的110%。
（2）将球磨后的浆料进行喷雾造粒，过筛得到100-150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）将生坯放入烧结中，氢气气氛下，在950℃保温60min，达到烧结温度1800℃时，保温120min，获得黑色导电氧化锆陶瓷。
经测试，该黑色导电氧化锆陶瓷的弯曲强度为653MPa，断裂韧性为7.71MPa·m1/2，维氏硬度为17.35GPa，相对密度为99.13%，气孔率为0.83%，电阻率为6.4×10-7Ω·m；色差仪测量黑度值L=59.12。
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)

1.一种黑色导电氧化锆陶瓷的制备方法，其特征在于：
包括如下步骤：
（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；
（2）将研磨后的浆料进行烘干后过筛造粒，得到造粒粉；
（3）将造粒粉放入模具中，经过模压成型制成陶瓷生坯；
（4）将陶瓷生坯干燥；
（5）将干燥后的生坯烧结，高温反应烧结获得黑色导电氧化锆陶瓷。
2.根据权利要求1所述的一种黑色导电氧化锆陶瓷的制备方法，其特征在于：所述氧化锆粉、导电粉、钛源、碳源、添加剂的质量配比为(20-80):(0-65):(0-30):(0-15):(0-5)。
3.根据权利要求1所述的一种黑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%。
4.根据权利要求3所述的一种黑色导电氧化锆陶瓷的制备方法，其特征在于：所述稳定剂为CaO、MgO、Y2O3、CeO2中的一种。
5.根据权利要求1所述的一种黑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。
6.根据权利要求1所述的一种黑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。
7.根据权利要求1所述的一种黑色导电氧化锆陶瓷的制备方法，其特征在于：所述碳源为酚醛树脂、绵白糖、碳黑、石墨烯、碳化硼中的一种。
8.根据权利要求1所述的一种黑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。
9.根据权利要求1所述的一种黑色导电氧化锆陶瓷的制备方法，其特征在于：所述结合剂为酚醛树脂、PVA、PVB或其它有机胶中的一种；结合剂用量为混合料质量的8-12%；
所述液体介质为水、乙醇或汽油；液体介质用量为混合料质量的80-120%。
10.根据权利要求1所述的一种黑色导电氧化锆陶瓷的制备方法，其特征在于： 所述的反应烧结：温度为1500-1800℃。
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