CN107324807A - 一种低压高能SiC半导体电嘴材料的制备方法 - Google Patents

一种低压高能SiC半导体电嘴材料的制备方法 Download PDF

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CN107324807A
CN107324807A CN201710470661.4A CN201710470661A CN107324807A CN 107324807 A CN107324807 A CN 107324807A CN 201710470661 A CN201710470661 A CN 201710470661A CN 107324807 A CN107324807 A CN 107324807A
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王波
赵杉
丁克
张南龙
侯宝强
李春芳
杨建锋
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Xian Jiaotong University
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Abstract

本发明公开了一种低压高能SiC半导体电嘴材料的制备方法，包括以下步骤：1)按照体积配比，选取45～70％的SiC粉末，5～15％的ZrO2粉末，10～30％的Al2O3粉末，10～30％的构成玻璃体系复合氧化物粉末，混合均匀，过200目筛储存备用；2)按照粉料重量：PVA重量＝95:5的比例加入8％固含量的PVA，手动混合均匀后，过80目筛，在80MPa压力下压制形成生坯；3)将生坯放入空气炉中进行烧结，升温速率为5℃/h，升温至450℃，保温12h；4)将排胶后的生坯放入真空烧结炉中，填充Ar，升温至1600～1800℃进行烧结，保温时间为1～3h，升温速率为5℃/min。本发明制备得到的SiC半导体复合材料具有发火电压低，火花能量大、不受气压和环境介质的影响，耐热冲击、耐电火花的腐蚀，熄灭再启动、高空性能好等优良性能。

Description

一种低压高能SiC半导体电嘴材料的制备方法
技术领域
本发明涉及一种低压高能半导体电嘴材料，特别涉及一种低压高能SiC半导体电嘴材料的制备方法。
背景技术
航空半导体电嘴的工作原理是在一定电压条件下半导体表面间隙形成火花放电,从而点燃发动机燃油混合气体；由于半导体电嘴直接暴露于高温燃油气中,经受非常苛刻的工作条件，尤其高空熄火时，需要在低温、低气压及气流高速喷射等恶劣条件下进行的，需要点火性能稳定可靠、火花能量大的低压高能点火系统。半导体陶瓷材料是点火电嘴的核心部件，它的物理性能和电性能等指标决定了电嘴的寿命和可靠性。航空半导体电嘴材料一般具有以下性能特点：发火电压低，火花能量大；不受气压和环境介质的影响，在恶劣条件下能正常工作，点火稳定性好；耐热冲击，耐电火花的腐蚀；寿命长，长期使用电性能基本不变；熄灭再启动，高空性能好。从而能够在苛刻的情况下点燃燃油混合气体及其他可燃气体。
国外半导体电嘴从二次世界大战后开始应用，如前苏联生产的CΠ型半导体电嘴和美国钱皮恩公司生产的FHE型半导体电嘴,以及日本NGK公司生产的JS型半导体电嘴等。俄制产品与欧美产品有很大区别,主要区别在电嘴发火端所用半导体材料上。俄制电嘴的发火端大多是以Al2O3陶瓷为基体,在基体上施半导体釉烧制成,而欧美国家的电嘴的发火端多直接采用SiC半导体。目前,国内研制的半导体电嘴同样有2种类型：1)以Cu2O为主的半导体釉型电嘴,其主要材料为半导体釉涂覆在Al2O3陶瓷的基体上,这种结构和俄制产品很相似；2)SiC陶瓷复合材料制备的半导体型电嘴,属于欧美制产品的方式。
SiC陶瓷复合材料由于硬度高、强度好、抗腐蚀性好、耐热冲击、以及高温性能好，作为半导体电嘴材料具有寿命长、可靠性高等优良特性。通过控制SiC含量，可以调控半导体的放电电压。随着SiC含量提高，可以提高半导体陶瓷的放电电压等各项性能，但同时会导致开气孔率增加，容易积碳致产品的失效。另一方面，随着SiC含量提高，半导体陶瓷易出现开裂缺陷。
发明内容
本发明的目的是解决现有SiC半导体电嘴存在的积碳失效问题，耐高温性能差(低于1400℃)，以及耐热冲击性能导致开裂缺陷等问题，提出一种具有发火电压低，火花能量大、不受气压和环境介质的影响，耐热冲击、耐电火花的腐蚀，熄灭再启动、高空性能好的SiC半导体电嘴材料的制备方法。
为达到以上目的，本发明采取如下技术方案予以实现：
一种低压高能SiC半导体电嘴材料的制备方法，包括以下步骤：
1)按照体积配比，选取10～30％的Y2O3，50～70％的SiO2，1～5％的MgO，1～5％的CaO，1～5％的Na2O，1～5％的Sr2O3，1～5％的La2O3，进行称量并混合均匀，其中CaO2，Na2O均以碳酸盐的形式引入，将球磨后的混合料装入坩埚中，在空气炉中快速升温至1000～1100℃，保温1～3h，随炉冷却，形成玻璃体系复合氧化物粉末；
2)按照体积配比，选取45～70％的SiC粉末，5～15％的ZrO2粉末，10～30％的Al2O3粉末，10～30％的构成玻璃体系复合氧化物粉末，混合均匀，过200目筛储存备用；
3)按照粉料重量：PVA重量＝95:5的比例加入8％固含量的PVA，手动混合均匀后，过80目筛，在80MPa压力下压制形成生坯；
4)将生坯放入空气炉中进行排胶，升温速率为5℃/h，升温至450℃，保温12h；
5)将排胶后的生坯放入真空烧结炉中，抽真空至3.6×10-3Pa，填充氩气，从室温升温至1600～1800℃进行烧结，保温时间为1～3h，得到低压高能SiC半导体电嘴材料。
本发明进一步的改进在于，步骤1)所述混合的方法为湿法球磨，磨球为玛瑙球，球磨介质为无水乙醇，球、料、介质的质量比为2：1：1。
本发明进一步的改进在于，步骤2)所述混合混合的方法为湿法球磨，磨球为玛瑙球，球磨介质为无水乙醇，球、料、介质的质量比为2：1：1。
本发明进一步的改进在于，步骤1)中所述快速升温，升温速率为50℃/min。
本发明进一步的改进在于，步骤5)中氮气气氛压力为0.1～0.8MPa。
本发明进一步的改进在于，步骤5)中，升温速率为5℃/min。
本发明的优点在于：
本发明采用稀土氧化物组成玻璃体系复合氧化物粉末为粘结剂，采用高温烧结制备SiC半导体电嘴材料，由于添加高含量的Y2O3，材料可耐受1600℃的高温；添加ZrO2陶瓷颗粒，通过ZrO2的相变增强补韧可提高材料的力学性能和可靠性；添加Sr2O3可改善材料的电性能，由于具有较高体积分数的SiC，半导体电嘴具有低的发火电压(600～800V)，高的火花能量(14～20J)；材料开气孔率很低，可防止油气点燃后产生的表面积碳问题；材料内部具有一定的闭气孔，可提高SiC材料的抗冲击性能，防止材料多次点火后开裂、变形、或失效。
此外，本发明的制备工艺简单，易于操作，通过成分设计和调整烧结温度和保温时间等工艺参数，可以获取微观形貌可控的SiC半导体电嘴材料。
附图说明
图1为实施例6所得的SiC半导体电嘴材料的的SEM显微结构照片。
具体实施方式
现结合实施例和附图，对本发明作进一步描述，但本发明的实施并不仅限于此。
1)按表1配方称量形成玻璃体系的复合氧化物粉末原料，其中K2O，Na2O的引入形式分别为Ca2CO3，Na2CO3，原料等级为实验级分析纯，采用球磨方式混合均匀，球磨介质为无水乙醇，球、料、介质的比例为2：1：1。将混合料装入坩埚中，在空气炉中以表2工艺参数烧结，升温速率为50℃/min，随炉冷却，形成玻璃体系复合氧化物粉末；
2)按表2配方配料，原料等级为实验级分析纯，采用球磨方式混合均匀，球磨介质为无水乙醇，球、料、介质的比例为2：1：1，过200目筛储存备用；
3)按照粉料重量：PVA重量＝95:5的比例加入8％固含量的PVA，手动混合均匀后，过80目筛，在80MPa压力下压制形成生坯；
4)将生坯放入空气炉中进行排胶，升温速率为5℃/h，升温至450℃，保温12h；
5)将排胶后的生坯放入真空烧结炉中，抽真空至3.6×10-3Pa，填充氩气，以表2工艺参数烧结，升温速率为5℃/min。
图1为实施例6所得的SiC半导体电嘴材料的的SEM显微结构照片。从附图中可以看出，材料中包含～4％的闭气孔，可有效改善SiC复合材料的抗热震性能。灰色不规则颗粒为SiC晶粒，白色颗粒为ZrO2，灰白色颗粒为玻璃氧化物，可有效的把SiC晶粒结合在一起。此外，有细小的Al2O3晶粒镶嵌在玻璃体中。
表1.本发明选用的形成玻璃体系的复合氧化物粉末的原料组成(体积比)
表2.本发明选用的原料组成(体积比)与烧结工艺
表3.本发明的SiC半导体电嘴材料的性能

Claims (6)

1.一种低压高能SiC半导体电嘴材料的制备方法，其特征在于，包括以下步骤：
1)按照体积配比，选取10～30％的Y2O3，50～70％的SiO2，1～5％的MgO，1～5％的CaO，1～5％的Na2O，1～5％的Sr2O3，1～5％的La2O3，进行称量并混合均匀，其中CaO2，Na2O均以碳酸盐的形式引入，将球磨后的混合料装入坩埚中，在空气炉中快速升温至1000～1100℃，保温1～3h，随炉冷却，形成玻璃体系复合氧化物粉末；
2)按照体积配比，选取45～70％的SiC粉末，5～15％的ZrO2粉末，10～30％的Al2O3粉末，10～30％的构成玻璃体系复合氧化物粉末，混合均匀，过200目筛储存备用；
3)按照粉料重量：PVA重量＝95:5的比例加入8％固含量的PVA，手动混合均匀后，过80目筛，在80MPa压力下压制形成生坯；
4)将生坯放入空气炉中进行排胶，升温速率为5℃/h，升温至450℃，保温12h；
5)将排胶后的生坯放入真空烧结炉中，抽真空至3.6×10-3Pa，填充氩气，从室温升温至1600～1800℃进行烧结，保温时间为1～3h，得到低压高能SiC半导体电嘴材料。
2.根据权利要求1所述的一种低压高能SiC半导体电嘴材料的制备方法，其特征在于，步骤1)所述混合的方法为湿法球磨，磨球为玛瑙球，球磨介质为无水乙醇，球、料、介质的质量比为2：1：1。
3.据权利要求1所述的一种低压高能SiC半导体电嘴材料的制备方法，其特征在于，步骤2)所述混合混合的方法为湿法球磨，磨球为玛瑙球，球磨介质为无水乙醇，球、料、介质的质量比为2：1：1。
4.据权利要求1所述的一种低压高能SiC半导体电嘴材料的制备方法，其特征在于，步骤1)中所述快速升温，升温速率为50℃/min。
5.据权利要求1所述的一种低压高能SiC半导体电嘴材料的制备方法，其特征在于，步骤5)中氮气气氛压力为0.1～0.8MPa。
6.据权利要求1所述的一种低压高能SiC半导体电嘴材料的制备方法，其特征在于，步骤5)中，升温速率为5℃/min。
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RU2779289C1 (ru) * 2022-01-18 2022-09-05 Акционерное Общество "Уфимское агрегатное производственное объединение" (АО "УАПО") Способ изготовления полупроводникового элемента запальной свечи
CN116477953A (zh) * 2023-05-15 2023-07-25 西安交通大学 一种SiC半导体点火材料、制备方法及应用
CN116675537A (zh) * 2023-05-15 2023-09-01 西安交通大学 一种等离子点火用SiC半导体材料、制备方法及电嘴

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RU2779289C1 (ru) * 2022-01-18 2022-09-05 Акционерное Общество "Уфимское агрегатное производственное объединение" (АО "УАПО") Способ изготовления полупроводникового элемента запальной свечи
CN116477953A (zh) * 2023-05-15 2023-07-25 西安交通大学 一种SiC半导体点火材料、制备方法及应用
CN116675537A (zh) * 2023-05-15 2023-09-01 西安交通大学 一种等离子点火用SiC半导体材料、制备方法及电嘴

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