CN111848162A - 一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法 - Google Patents

一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法 Download PDF

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CN111848162A
CN111848162A CN202010752431.9A CN202010752431A CN111848162A CN 111848162 A CN111848162 A CN 111848162A CN 202010752431 A CN202010752431 A CN 202010752431A CN 111848162 A CN111848162 A CN 111848162A
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preparation
porosity
powder
steps
zirconia ceramic
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王春华
茹红强
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

本发明提供一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，所述制备方法，包括混料；烘干、造粒，模压成型，干燥，烧结。本发明工艺简单、便于批量化生产；可使氧化锆陶瓷不仅导电，还拥有多孔的特性，具备结构与功能一体化优势，在电子烟雾化芯、催化剂载体、传感器方面具有非常大的实用前景。氧化锆陶瓷孔隙率具有可调性，通过控制成型压力和石蜡的配比，可以获得大范围的孔隙率5.0~70.0%。

Description

一种电阻率、气孔率可调多孔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，特别涉及一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法。
背景技术
氧化锆陶瓷具有强度高、硬度高、耐磨损、耐化学腐蚀、高导热等优良的特性，已被广泛应用在电子烟雾化芯、催化剂载体、传感器领域，展现出巨大的市场商机。在用作电子烟雾化芯时，通常情况下，氧化锆陶瓷是不导电的，其表面必须印刷导电线路，电路产生的热量传导给氧化锆陶瓷片后，再将烟油雾化，这种热量多次传递过程，热能的利用率较低，容易使电池发热；不仅有安全隐患，还降低了使用者的体验感。
CN106938930A公开了高致密高强度氧化锆导电陶瓷及其制备方法，氧化锆粉中加入碳化硼粉、粘结剂、分散剂、水进行球磨、造粒、静压处理、烧结处理等。
该专利存在以下不足或缺陷：
电阻率低，导电性能差。此专利是靠真空烧结或氩气保护的方式，使氧化锆晶体结构产生氧缺位，导电模式为空穴导电或离子导电，导电性能差。碳化硼本身不导电。
热压烧结工艺缺陷非常明显：耗能高、产量极低、产品形状尺寸受限，不适合规模化大批量工业生产。
热压烧结获得陶瓷致密度非常高，但是不能制备出多孔陶瓷，孔隙率不能在大范围调控，因此陶瓷无法发挥多孔的特性，如过滤、催化剂载体、吸附等功能，导致热压烧结获得陶瓷的应用领域非常狭窄。
CN104876611B公开了一种石墨烯增强陶瓷及其制备方法，氧化锆粉中加入导电材料石墨烯，制备导电氧化锆陶瓷。
该专利存在以下不足或缺陷：
（1）虽然有导电功能的介绍，但是实施例中未发现任何导电指标，如电阻率值或导电率值，其真实导电性能有待考证。
（2）即使此陶瓷能导电，但是导电性能并不稳定，陶瓷导电过程也是一个发热、温度升高的过程，众所周知，石墨烯本质是碳，结构并不稳定，温度过高易氧化，石墨烯氧化，必会降低陶瓷的导电性能，其它性能也会下降。
（3）陶瓷不具备多孔特性，孔隙率不能在大范围调控，因此陶瓷无法发挥多孔的特性，如过滤、催化剂载体、吸附等功能，导致应用领域不能拓宽。
（4）石墨烯成本高昂，且存在分散不均的难题，石墨烯的研究还处于实验室阶段，商业化道路任重道远，因此石墨烯增强陶瓷并不具备大规模批量化生产的条件。
发明内容
针对现有技术存在的不足，本发明提供一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，实现以下发明目的：
（1）导电性能好；
（2）电阻率、孔隙率可以调控；
（3）提高氧化锆陶瓷的硬度和强度。
为解决上述技术问题，本发明取得以下技术方案：
本发明通过将原料与液体介质混成均一浆料，经与石蜡混合、造粒、模压成型，高温烧结获得具有卓越的导电性能且电阻率、气孔率可调、化学稳定性高、抗高温氧化、耐磨损、综合力学性能优异的氧化锆陶瓷。
一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，包括混料；烘干、造粒，模压成型，干燥，烧结。
以下是对上述技术方案的进一步改进：
具体步骤如下：
（1）混料
将氧化锆粉、导电粉、烧结助剂、结合剂混合，得到混合料，然后与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）烘干、造粒
将混合浆料在40~100℃干燥箱中烘干后破碎成混合粉，再与石蜡加热混合均匀，冷却成块体后经摇摆造粒机80目过筛造粒；
所述烘干，优选为60-100℃，烘干6-15h；
（3）模压成型
将造粒粉放入模具中，经过模压成型制成陶瓷生坯；
（4）干燥
将压制好的陶瓷生坯放入40~150℃干燥箱中干燥脱蜡；
优选为100-150℃中干燥12-24h；
（5）烧结
将生坯放入烧结中，1250~1650℃反应烧结获得电阻率、气孔率可调氧化锆陶瓷。
所述的步骤(1)中，氧化锆粉平均粒度为0.5nm~5μm，纯度大于90%，稳定剂为CaO、MgO、Y2O3、CeO2中的一种；
上述步骤(1)中，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、碳化钨其中的至少一种。
上述步骤(1)中，烧结助剂为滑石粉、钾长石、钠长石、玻璃粉、氧化镁、锂辉石、黏土、十二烷基苯磺酸钠、氧化硼、氧化钙、氧化铝其中的至少一种。
所述导电粉和烧结助剂的平均粒径都在5μm以下；
上述步骤(1)中，结合剂为PVA、PVB、PVP或其它有机胶；所述结合剂的有效成分含量为3-10wt%；
上述步骤(1)中，液体介质可以是水、乙醇或汽油等其它有机溶剂；所述液体介质与混合料的质量比为1.1-1.3:1。
上述步骤(1)中，氧化锆粉、导电粉、烧结助剂、结合剂的质量配比为(40-70):(5-45):(5-15):(5-30)；优选为（55-70）:（20-40）:（8-15）:（5-25）；
上述步骤(2)中，混合粉与石蜡的质量配比为100：(0-30)；
上述步骤(3)中，模压成型的压力为30~200MPa；优选为50-200 MPa；
上述步骤(5)中，烧结气氛可以是真空、氩气、氮气；所述烧结，将生坯在590-610℃保温60-120min，1250~1650℃反应烧结90-120min。
上述步骤(5)中，氧化锆陶瓷电阻率为1μΩ·m~10Ω·m，气孔率为5.0~70.0%。
与现有技术相比，本发明的有益效果在于：
（1）在氧化锆基体中引入导电相，可以使氧化锆陶瓷具备导电性能，用作电子烟雾化芯时，导电发热，直接将热量传递给烟油，实现热能高效利用的同时提高电池的安全性；本发明制备的氧化锆陶瓷，电阻率为2.5×10-6～1.3×10-3Ω·m。
（2）氧化锆陶瓷孔隙率具有可调性。通过控制成型压力和石蜡的配比，可以获得大范围的孔隙率5.0~70.0%，优选为5-56%；孔隙率较低时，高致密化的氧化锆陶瓷具有优异的力学性能和较低的电阻率，可以直接加工成导电薄片雾化烟油，或作为电极片用在智能穿戴结构部件以检测人体弱电流信号；当孔隙率较高时，显著增大与烟油接触面积，提升雾化效率，或作为气敏传感器件提高灵敏度。
本发明制备的氧化锆陶瓷，相对密度为45-95%。
（3）本发明工艺简单，对设备要求度低，可以制备出电阻率、气孔率可调，形状可塑的产品，便于大规模自动化生产，产品成本低且性能高，具有巨大的市场实用价值。
（4）本发明开发的电阻率、气孔率可调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，除具有卓越的导电性能(电阻率低至10-6Ω·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外，还拥有气孔率可调的特点；在智能穿戴、传感器件、电子烟雾化芯领域具有巨大的应用前景。
本发明制备的氧化锆陶瓷的弯曲强度为85-320MPa，断裂韧性为1.35-3.18MPa·m1/2，维氏硬度为4.5-12.68GPa。
附图说明
图1为本发明实施例1中制备的片式导电氧化锆陶瓷雾化芯实物图片；
图2为本发明实施例2中制备的空心圆柱式多孔导电氧化锆陶瓷雾化芯实物图片；
图3为本发明实施例3中制备的圆柱式多孔导电氧化锆陶瓷雾化芯实物图片。
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
一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，步骤如下：
（1）混料
按质量比，将氧化锆粉、硼化钛、滑石粉、5.0%PVA结合剂按照质量配比为55:40:8:5进行混合，得到混合料；和无水乙醇一起混合成浆料，在球磨罐中球磨12h；
所述氧化锆粉，氧化锆的含量为90wt%，稳定剂CeO2的含量为10wt%，平均粒径1μm；
所述无水乙醇与混合料的质量比为1.2：1。
（2）烘干、造粒
将混合浆料在60℃干燥箱中干燥15小时，烘干后破碎再经摇摆造粒机过筛（80目筛网）造粒（此过程没加石蜡，即石蜡的配比为0）。
（3）模压成型
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）干燥
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）烧结
将生坯放入烧结中，氩气气氛下，在600℃保温60min，达到烧结温度1650℃时，保温90min，获得氧化锆陶瓷。
经测试，该氧化锆陶瓷的弯曲强度为320MPa，断裂韧性为3.18MPa·m1/2，维氏硬度为12.68GPa，相对密度为94.34%，气孔率为5.26%，电阻率为2.5×10-6Ω·m。
实施例2
一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，步骤如下：
（1）混料
按质量比，将氧化锆粉(纯度90%，平均粒径1μm、稳定剂CeO2)、碳化钛粉、钾长石粉、3.0%PVB结合剂的质量配比为60:20:15:25混合，得到混合料，和去离子水一起混合成浆料，在砂磨机中研磨2h；
所述氧化锆粉，氧化锆的含量为90wt%，稳定剂CeO2的含量为10wt%，平均粒径1μm；
所述去离子水与混合料的质量比为1.2：1。
（2）烘干、造粒
将混合浆料在80℃干燥箱中干燥8小时，烘干破碎成混合粉，过100目筛，再与石蜡按质量比100:25加热混合均匀，冷却成块体后经摇摆造粒机过筛（80目筛网）造粒。
（3）模压成型
将造粒粉放入模具中，经压力机模压成型，压力50MPa，获得生坯。
（4）干燥
将压制好的陶瓷生坯放入120℃干燥箱中脱蜡、干燥15h排出体内水分。
（5）烧结
将生坯放入烧结中，氩气气氛下，在600℃保温90min，达到烧结温度1600℃时，保温120min，获得氧化锆陶瓷。
经测试，该氧化锆陶瓷的弯曲强度为85MPa，断裂韧性为1.35MPa·m1/2，维氏硬度为4.68GPa，相对密度为46.26%，气孔率为55.34%，电阻率为1.3×10-3Ω·m。
实施例3
一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，步骤如下：
（1）混料
按质量比，将氧化锆粉(纯度98%，平均粒径5μm、稳定剂MgO)、氮化钛粉、玻璃粉、10.0%PVA结合剂的质量配比为70:30:10:12，和蒸馏水一起混合成浆料，在砂磨机中研磨4h；
所述氧化锆粉，氧化锆的含量为98wt%，稳定剂MgO的含量为2wt%，平均粒径5μm；
所述蒸馏水与混合料的质量比为1.2：1。
（2）烘干、造粒
将混合浆料在100℃干燥箱中干燥6小时，烘干破碎成混合粉，，过100目筛，再与石蜡按质量比100:10加热混合均匀，冷却成块体后经摇摆造粒机过筛（80目筛网）造粒。
（3）模压成型
将造粒粉放入模具中，经压力机模压成型，压力100MPa，获得生坯。
（4）干燥
将压制好的陶瓷生坯放入100℃干燥箱中干燥24h排出体内水分。
（5）烧结
将生坯放入烧结中，氮气气氛下，在600℃保温120min，达到烧结温度1550℃时，保温120min，获得氧化锆陶瓷。
经测试，该氧化锆陶瓷的弯曲强度为135MPa，断裂韧性为2.24MPa·m1/2，维氏硬度为6.34GPa，相对密度为67.21%，气孔率为30.50%，电阻率为5.3×10-4Ω·m。
实施例2和实施例3制备的高气孔率氧化锆陶瓷，由实施例2和实施例3概括得出以下技术方案：
一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，包括混料；烘干、造粒，模压成型，干燥，烧结。
具体步骤如下：
（1）混料
将氧化锆粉、导电粉、烧结助剂、结合剂混合，得到混合料，然后与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2-4h；
（2）烘干、造粒
将混合浆料在80~100℃干燥箱中烘干6-8h后破碎成混合粉，再与石蜡加热混合均匀，冷却成块体后经摇摆造粒机80目过筛造粒；
（3）模压成型
将造粒粉放入模具中，经过模压成型制成陶瓷生坯；
（4）干燥
将压制好的陶瓷生坯放入100-120℃干燥箱中干燥脱蜡15-24h；
（5）烧结
将生坯放入烧结炉中，反应烧结获得电阻率、气孔率可调氧化锆陶瓷。
所述的步骤(1)中，氧化锆粉平均粒度为1μm~5μm，纯度大于90%，稳定剂为CaO、MgO、Y2O3、CeO2中的一种；
上述步骤(1)中，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、碳化钨其中的至少一种。
上述步骤(1)中，烧结助剂为滑石粉、钾长石、钠长石、玻璃粉、氧化镁、锂辉石、黏土、十二烷基苯磺酸钠、氧化硼、氧化钙、氧化铝其中的至少一种。
所述导电粉和烧结助剂的平均粒径都在5μm以下；
上述步骤(1)中，结合剂为PVA、PVB、PVP；所述结合剂的有效成分含量为3-10wt%；
上述步骤(1)中，液体介质可以是水、乙醇或汽油；所述液体介质与混合料的质量比为1.1-1.3:1。
上述步骤(1)中，氧化锆粉、导电粉、烧结助剂、结合剂的质量配比为(60-70):(20-30):(10-15):(12-25)；
上述步骤(2)中，混合粉与石蜡的质量配比为100：(10-25)；
上述步骤(3)中，模压成型的压力为50~100MP；
上述步骤(5)中，烧结气氛可以是真空、氩气、氮气；所述烧结，将生坯在590-610℃保温90-120min，1550~1600℃反应烧结115-125min。
上述技术方案可以实现以下技术效果：
制备的氧化锆陶瓷的弯曲强度为85-135MPa，断裂韧性为1.35-2.24MPa·m1/2，维氏硬度为4.68-6.34GPa，相对密度为46.26-67.21%，气孔率为30.50-55.34%，电阻率为5.3×10-4~1.3×10-3Ω·m。
除非特殊说明，本发明采用的百分比均为质量百分比，采用的比例均为质量比例。
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)

1.一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述制备方法，包括混料；烘干、造粒，模压成型，干燥，烧结。
2.根据权利要求1所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述混料，将氧化锆粉、导电粉、烧结助剂、结合剂混合，得到混合料，然后与液体介质混合，得到混合浆料，进行球磨或研磨。
3.根据权利要求2所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述氧化锆粉的平均粒度为0.5nm~5μm，纯度大于90%，稳定剂的添加量为2-10%；所述稳定剂为CaO、MgO、Y2O3、CeO2中的一种。
4.根据权利要求2所述的一种电阻率、气孔率可调多孔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、碳化钨其中的至少一种。
5.根据权利要求2所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述烧结助剂为滑石粉、钾长石、钠长石、玻璃粉、氧化镁、锂辉石、黏土、十二烷基苯磺酸钠、氧化硼、氧化钙、氧化铝其中的至少一种。
6.根据权利要求2所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述结合剂为PVA、PVB、PVP或其它有机胶；所述结合剂的有效成分含量为3-10wt%；所述液体介质为水、乙醇或汽油；所述液体介质与混合料的质量比为1.1-1.3:1。
7.根据权利要求2所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述氧化锆粉、导电粉、烧结助剂、结合剂的质量配比为(40-70):(5-45):(5-15):(5-30)。
8.根据权利要求1所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述烘干、造粒，混合浆料经过烘干破碎成混合粉，再与石蜡加热混合均匀，冷却成块体后过筛造粒；所述混合粉与石蜡的质量比为100：(0-30)。
9.根据权利要求1所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述模压成型，压力为30~200MPa。
10.根据权利要求1所述的一种电阻率、气孔率可调多孔氧化锆陶瓷的制备方法，其特征在于：所述烧结，将生坯在590-610℃保温60-120min，1250~1650℃反应烧结90-120min。
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