CN115010482B - 一种大功率用高导电氧化锌基陶瓷的制备方法 - Google Patents

一种大功率用高导电氧化锌基陶瓷的制备方法 Download PDF

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CN115010482B
CN115010482B CN202210678142.8A CN202210678142A CN115010482B CN 115010482 B CN115010482 B CN 115010482B CN 202210678142 A CN202210678142 A CN 202210678142A CN 115010482 B CN115010482 B CN 115010482B
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张代兵
王俊
张晨然
吕辰
钦达
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Abstract

一种大功率用高导电氧化锌基陶瓷的制备方法。本发明以Zn(CH3COO)2·2H2O、Ga(NO3)3·xH2O和Ni(NO3)2·6H2O为原料，以氨水、三乙醇胺和去离子水混合液作为溶剂，通过二次水热反应制备了Zn1‑x‑yNixGayO(0≤x≤0.005，0≤y≤0.2)粉体，所得粉体经真空热压法烧结后，制备出载流子浓度≥2×1020cm‑3、载流子迁移率≥50cm2V‑1S‑1、电阻率为ρ≤3.0×10‑6Ω·m、电阻温度系数为k≤+2.0×10‑3/℃、使用温度范围为‑100～500℃的Zn1‑x‑yNixGayO(0≤x≤0.005，0≤y≤0.2)导电陶瓷。本发明工艺具有环境友好、节能、高效等特点。

Description

一种大功率用高导电氧化锌基陶瓷的制备方法
技术领域
本发明属于导电材料技术领域，特别涉及一种制备大功率用高导电氧化锌基陶瓷的方法，涉及到水热合成法和真空热压烧结工艺。
背景技术
在脉冲大功率供电系统中，通常采用金属导电体，但它在升温150℃后性能失效，因此需增加金属体积和串并联数量，导致其体积较大且因电感量大而使控制电路复杂。为了克服金属材料的不足，采用“水电阻”技术可克服上述问题，但“水电阻”体积仍然庞大、温度范围窄、实战性差。近年来，国内外采用高导电的非金属陶瓷方案，解决以上问题，但存在抗氧化特性差、使用温度窄等问题(陶瓷需浸泡在油里)。目前这些非金属陶瓷全部依赖进口，需求量大，价格昂贵。
导电氧化物陶瓷可解决上述问题，但国内外此类产品甚少，目前已有氧化物陶瓷产品一般其导电性能低、且电阻温度系数为负，无法满足实际要求。氧化物陶瓷因其具有高温服役稳定、抗氧化、环境友好等特点，近几年颇受国内外研究者关注。已发展众多氧化物陶瓷：ZnO、NaxCoO2、Ca3Co4O9、SrTiO3、CaMnO3等，相比于其它氧化物陶瓷，NaxCoO2和ZnO均具有较优异的导电能力。NaxCoO2陶瓷凭借其[CoO2]层可为电子提供快速通道，结合有效的掺杂改性及结构调控，常温电阻率低至1×10-4Ω·m，已具备了较优异的导电性[Tak JY，etal.Journal of Electronic Materials，2015，44：1408-1412.]。但因在高温下，Na容易挥发导致其结构和性能不稳定，进而限制了其应用。相比于NaxCoO2陶瓷，ZnO陶瓷的电学性能及热稳定性都极佳，而且原料丰富、价格低廉，是一种极富应用潜力的导电陶瓷。ZnO由于天然存在着O空位和Zn间隙等多种缺陷，因此不掺杂的ZnO表现为n型导电特性，可通过高价离子的n型掺杂实现更优异的导电性。早在1996年，M.ohtaki等利用传统球磨工艺结合固相烧结法制备的Al掺杂ZnO陶瓷，其室温电阻率可低至～1×10-5Ω·m[Ohtaki M，etal.Journal of Applied Physics，1996，79：1816-1818.]。继此之后，各国学者通过不同的制备工艺和掺杂改性，对ZnO陶瓷的电输运性质进行了大量的研究和探索。但随后的研究发现，ZnO-Al2O3体系的相图中没有Al2O3在ZnO中的固溶区，固溶度仅～0.3％mol，这就给Al掺杂ZnO的研究带来了困难，因此限制了ZnO陶瓷电导率的进一步提升。研究者们也曾尝试利用其它Ti4+、Sn4+、Bi3+、Ga3+、Sb5+等高价离子单掺或者共掺提高ZnO的导电性，但结果并不理想，该系列掺杂离子的固溶度依然很低，当离子掺杂量高于2％mol时容易出现高电阻率的第二相，限制了ZnO电导率的提升。
发明内容
本发明提供一种制备大功率用高导电氧化锌基高温陶瓷的方法，采用二次水热法制备了Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)前驱粉体，结合真空热压烧结技术，制备出载流子浓度≥2x1020cm-3、载流子迁移率≥50cm2V-1S-1、电阻率为ρ≤3.0×10-6Ω·m、电阻温度系数为k≤+2.0×10-3/℃、使用温度范围为-100～500℃的Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)导电陶瓷。
一种大功率用高导电氧化锌基高温陶瓷的制备方法，其特征是：以形貌为1～3μm颗粒自组装成的5～15μm花状微米球结构且XRD检测未发现第二相的Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)为前驱粉体，在压力为20～25Mpa，温度为900～1000℃下真空热压烧结，保温1～2h，获得Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)导电陶瓷。
具有花状微米球结构Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)粉体采用二次水热法进行合成，其制备工艺包括以体积比为0.5∶1.5∶8的氨水、三乙醇胺和去离子水混合液作为溶剂，140～180℃进行2～3h一次水热反应；粉体收集后以氨水作为表面活性剂，调制PH值为9.1～9.5，在180～190℃进行1～2h二次水热反应。
本发明的技术特征是：利用二次水热法制备了形貌为1～3μm颗粒自组装成的5～15μm花状微米球结构且XRD检测未发现第二相的Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)的前驱粉体，花状结构有利于块体陶瓷获得高迁移率，粉体中未发现第二相表明高的离子掺杂浓度，该方法克服了掺杂离子固溶量低的问题，前驱粉体经真空热压烧结技术烧结后，获得了高导电的Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)导电陶瓷。
目前，获得电阻率为ρ≤3.0x10-6Ω·m、电阻温度系数为k≤+2.0×10-3/℃、使用温度范围为-100～500℃的Zn1-x-yNixGayO(0≤x≤0.005，0≤y≤0.2)导电陶瓷未见报道。
具体实施方式
1.以Zn(CH3COO)2·2H2O、Ga(NO3)3·xH2O和Ni(NO3)2·6H2O为原料，按照化学通式Zn0.945Ni0.005Ga0.05O配置，以体积比为0.5∶1.5∶8的氨水、三乙醇胺和去离子水混合液作为溶剂，180℃进行2h一次水热反应；粉体收集后以氨水作为表面活性剂，调制PH值为9.1，在180℃进行2h二次水热反应，获得Zn0.945Ni0.005Ga0.05O粉体，该粉体在压力25Mpa，温度为950℃下真空热压烧结，保温1h，制备出电阻率为ρ＝2.7×10-6Ω·m、电阻温度系数为k＝+1.1×10-3/℃、使用温度范围为-100～500℃的Zn0.945Ni0005Ga0.05O导电陶瓷。
2.以Zn(CH3COO)2·2H2O、Ga(NO3)3·xH2O和Ni(NO3)2·6H2O为原料，按照化学通式Zn0.915Ni0.005Ga0.08O配置，以体积比为0.5∶1.5∶8的氨水、三乙醇胺和去离子水混合液作为溶剂，170℃进行2h一次水热反应；粉体收集后以氨水作为表面活性剂，调制PH值为9.5，在190℃进行2h二次水热反应，获得Zn0.915Ni0.005Ga0.08O粉体，该粉体在压力20Mpa，温度为1000℃下真空热压烧结，保温1.5h，制备出电阻率为ρ＝2.2×10-6Ω·m、电阻温度系数为k＝+1.4×10-3/℃、使用温度范围为-100～500℃的Zn0.915Ni0.005Ga0.08O导电陶瓷。
3.以Zn(CH3COO)2·2H2O、Ga(NO3)3·xH2O和Ni(NO3)2·6H2O为原料，按照化学通式Zn0.878Ni0.002Ga0.12O配置，以体积比为0.5∶1.5∶8的氨水、三乙醇胺和去离子水混合液作为溶剂，140℃进行3h一次水热反应；粉体收集后以氨水作为表面活性剂，调制PH值为9.3，在180℃进行1h二次水热反应，获得Zn0.878Ni0.002Ga0.12O粉体，该粉体在压力20Mpa，温度为1000℃下真空热压烧结，保温2h，制备出电阻率为ρ＝1.6×10-6Ω·m、电阻温度系数为k＝+1.9×10-3/℃、使用温度范围为-100～500℃的Zn0.878Ni0.002Ga0.12O导电陶瓷。
4.以Zn(CH3COO)2·2H2O、Ga(NO3)3·xH2O和Ni(NO3)2·6H2O为原料，按照化学通式Zn0.795Ni0.005Ga0.2O配置，以体积比为0.5∶1.5∶8的氨水、三乙醇胺和去离子水混合液作为溶剂，160℃进行3h一次水热反应；粉体收集后以氨水作为表面活性剂，调制PH值为9.5，在180℃进行1h二次水热反应，获得Zn0.795Ni0.005Ga0.2O粉体，该粉体在压力20Mpa，温度为1000℃下真空热压烧结，保温2h，制备出电阻率为ρ＝2.0×10-6Ω·m、电阻温度系数为k＝+1.6×10-3/℃、使用温度范围为-100～500℃的Zn0.795Ni0.005Ga0.2O导电陶瓷。

Claims (1)

1.一种大功率用高导电氧化锌基高温陶瓷的制备方法，其特征是：以Zn(CH3COO)2·2H2O、Ga(NO3)3·xH2O和Ni(NO3)2·6H2O为原料，按照化学通式Zn1-x-yNixGayO配置，0＜x≤0.005，0＜y≤0.2，以体积比为0.5∶1.5∶8的氨水、三乙醇胺和去离子水混合液作为溶剂，140～180℃进行2～3h一次水热反应；粉体收集后以氨水作为表面活性剂，调制pH值为9.1～9.5，在180～190℃进行1～2h二次水热反应，获得形貌为1～3μm颗粒自组装成的5～15μm花状微米球结构且XRD检测未发现第二相的Zn1-x-yNixGayO粉体，0＜x≤0.005，0＜y≤0.2，该粉体在压力20～25MPa，温度为900～1000℃下真空热压烧结，保温1～2h，制备出载流子浓度≥2×1020cm-3、载流子迁移率≥50cm2V-1S-1、电阻率为ρ≤3.0×10-6Ω·m、电阻温度系数为k≤+2.0×10-3/℃、使用温度范围为-100～500℃的Zn1-x-yNixGayO导电陶瓷，0＜x≤0.005，0＜y≤0.2。
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