CN107500773A - 一种碳化硅基复相高温热敏陶瓷材料 - Google Patents

一种碳化硅基复相高温热敏陶瓷材料 Download PDF

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CN107500773A
CN107500773A CN201710698516.1A CN201710698516A CN107500773A CN 107500773 A CN107500773 A CN 107500773A CN 201710698516 A CN201710698516 A CN 201710698516A CN 107500773 A CN107500773 A CN 107500773A
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silicon carbide
complex phase
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陈健
陈军军
黄政仁
刘学建
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Shanghai Institute of Ceramics of CAS
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Abstract

本发明涉及一种碳化硅基复相高温热敏陶瓷材料，所述碳化硅基复相高温热敏陶瓷材料包括碳化硅基体材料和ZrB2第二相材料，所述ZrB2第二相材料的含量为2～26wt%；当ZrB2含量在2～26wt%变化时，所述碳化硅基复相高温热敏陶瓷材料在＜600℃下具有压敏电阻的非线性伏安特性、在600℃以上的高温下转变为欧姆电阻的线性伏安特性且电阻率在1.2～6.0Ω·cm之间。

Description

一种碳化硅基复相高温热敏陶瓷材料
技术领域
本发明涉及一种碳化硅(SiC)基复相高温热敏陶瓷材料及其制备方法，属于SiC陶瓷领域。
背景技术
碳化硅(SiC)是一种典型的半导体，它不同于金属的正的电阻温度系数，其导电能力会随温度升高而迅速增加，这使其可以用作热敏电阻，用于对电子线路元件的温度补偿或专用检测元件；而又因SiC压敏陶瓷具有良好的非线性伏安特性，其电阻随着电压的增加而急剧减小，在灭电火花、过电压保护、制备避雷针和电压稳定化等方面有着重要的应用。
发明内容
本发明综合SiC陶瓷和ZrB2陶瓷的优点，目的在于提供一种碳化硅基复相高温热敏陶瓷材料，所述碳化硅基复相高温热敏陶瓷材料包括碳化硅基体材料和ZrB2第二相材料，所述ZrB2第二相材料的含量为2～26wt％，优选为＞18wt％且≤26wt％；当ZrB2含量在2～26wt％变化时，所述碳化硅基复相高温热敏陶瓷材料在＜600℃下具有压敏电阻的非线性伏安特性、在600℃以上的高温下转变为欧姆电阻的线性伏安特性且电阻率在1.2～6.0Ω·cm之间。
本发明中，所述碳化硅基复相高温热敏陶瓷材料包括碳化硅基体材料和ZrB2第二相材料。其中碳化硅陶瓷性能稳定，不易老化，使用寿命长，同时具有高温下强度高、高导热、耐腐蚀、耐中子辐照、抗热震性好等优点；而二硼化锆(ZrB2)熔点高、硬度高、导热和导电性能好且抗腐蚀和烧蚀，同时它具有负的电阻温度系数，温度升高时，其电阻率升高。又由于SiC和ZrB2良好的物理匹配性，控制所述ZrB2第二相材料的含量为2～26wt％，使得由二者有机组合而成的复相陶瓷，将兼具二者各自的优势，有望获得物理化学性质稳定，耐高温，耐腐蚀，强度高，具有特殊电学性质的新型材料，使得SiC基陶瓷能在微电子领域得到更广泛的应用。本发明可以通过调控材料所处温度，来使其在低温下表现出SiC半导体的导电特性，而在高温下表现出ZrB2欧姆电阻导电特性。
较佳地，所述碳化硅基复相高温热敏陶瓷材料的密度为3.17～3.59g·cm-3，抗弯强度为310～350MPa。
本发明还提供了一种调节碳化硅基复相高温热敏陶瓷材料的热敏电阻特性的方法，以B或B4C中的至少一种作为烧结助剂，以酚醛树脂、PVA、PVB中的至少一种作为粘结剂无压固相烧结制备碳化硅基复相高温热敏陶瓷材料，通过控制ZrB2第二相材料的含量在2～26wt％之间，以调节碳化硅基复相高温热敏陶瓷材料在600℃以上的高温下转变为欧姆电阻的线性伏安特性且电阻率在1.2～6.0Ω·cm之间可控。本发明所制备的SiC基复相陶瓷可以通过调控环境温度来改变其电学特征，使其在低温下(＜600℃)表现为压敏电阻的非线性伏安特性，高温下(600℃以上)转变为欧姆电阻的线性伏安特性，且电阻率大大小于低温下的电阻率，1.2～6.0Ω·cm之间。
本发明以碳化硅(SiC)作为基体材料，可耐受超高温的导电陶瓷ZrB2为第二相材料(含量2～26wt％)，经高温烧结后获得一种具有特殊热敏特性的SiC/ZrB2复相陶瓷(碳化硅基复相高温热敏陶瓷材料)。即在不同的温度下对所述SiC/ZrB2复相陶瓷进行伏安特性测试时，在温度较低(＜600℃)时材料表现出明显的非线性压敏特性，随温度升高非线性逐渐减弱，当测试温度达到600℃及以上时材料均由非线性的压敏电阻导电特性转变为线性的欧姆电阻导电特性，电阻率也在这一过程中急速下降，由半导体转变为导体。
附图说明
图1为ZrB2含量为12wt％的SiC基复相陶瓷不同温度下的伏安特性曲线；
图2为ZrB2含量为16wt％的SiC基复相陶瓷不同温度下的伏安特性曲线；
图3为ZrB2含量为24wt％的SiC基复相陶瓷不同温度下的伏安特性曲线；
图4为ZrB2含量为28wt％的SiC基复相陶瓷不同温度下的伏安特性曲线。
具体实施方式
以下通过下述实施方式进一步说明本发明，应理解，下述实施方式仅用于说明本发明，而非限制本发明。
本发明以碳化硅(SiC)作基体材料，耐超高温的ZrB2为第二相材料，其含量在2～26wt％范围内变化，经高温烧结后获得SiC/ZrB2复相陶瓷。通过伏安特性测试，在600℃以下，材料均表现为很好的压敏电阻特有的非线性伏安特性，其特征为各个材料的电阻率随着电压的增加而降低，随温度的不断升高，其压敏电阻的非线性特征不断减弱，电阻率对电压变化的敏感性逐渐下降，当温度达到600℃时，材料由压敏电阻的非线性特征转变为欧姆电阻的线性特征，材料的电阻率不再随电压的变化而改变，而是随温度升高出现明显下降；另一方面，复相陶瓷随ZrB2含量的不断增多，其电阻率在同一温度下表现出下降的现象，而当ZrB2含量达到28wt％时，材料在不同温度下的伏安特性曲线均表现出线性特征。
以下示例性地说明本发明提供的碳化硅基复相高温热敏陶瓷材料的制备方法。
配置原料粉料：包括质量百分比为74～98wt％的SiC粉体和质量百分比为2～26wt％的ZrB2粉体。本发明的原料中SiC粉体的平均粒径可为0.1～1μm。ZrB2粉体的平均粒径可为1～5μm。其中，SiC粉体可为高纯SiC粉体(氧含量≤1.8wt％，Fe含量≤0.02wt％)。
将原料粉料通过球磨混合，配成固含量为40～45wt％的浆料。球磨过程中可加入水或其它溶剂(例如酒精等)，最后形成固含量为40～45wt％的浆料。所述的球磨混合采用SiC球作为研磨球。配置原料时还在原料粉体中加入0～1wt％(以SiC粉体、ZrB2粉体和烧结助剂的总质量为100％计)的烧结助剂。所述烧结助剂可为B或B4C。配置原料时还在原料粉体中加入5～10wt％(以SiC粉体、ZrB2粉体和烧结助剂的总质量为100％计)粘结剂。所述粘结剂可为酚醛树脂、聚乙烯醇PVA、聚乙烯醇缩丁醛PVB中的至少一种。
将球磨混合后浆料干燥过筛或喷雾造粒，依次进行干压成型和等静压成型或直接进行等静压成型，获得坯体。所述干压成型的压力可为10～100MPa。所述等静压的压力可为150～210MPa。
将坯体真空脱粘后，在常压惰性气氛条件下于1900～2300℃下烧结1～2小时，得所述碳化硅基复相高温热敏陶瓷材料。所述惰性气氛可为氩气等。
作为一个耐高温抗腐蚀SiC/ZrB2复相热敏陶瓷材料的制备方法的详细示例，其主要过程如下：(1)本发明的原料为平均粒径为0.1～1μm的SiC粉体，平均粒径为1～5μm的ZrB2粉体，B或B4C(0～1wt％)为烧结助剂，酚醛树脂、PVA、PVB等有机物作为粘结剂。(2)首先将酚醛树脂或PVA、PVB等有机物根据需要配成溶液，加入量分别为粉体质量的5wt％～10wt％；粉体都配成40～45％的浆料，用SiC球作为研磨球，粉料：SiC球＝1:2(质量)，混合24小时；然后将浆料进行喷雾造粒。得到混合均匀的粉体后，在平板机上以10～100MPa的压力进行干压成型，随后在150～210MPa压力下进行等静压处理。(3)随后在真空脱粘后，于常压Ar气氛下烧结，烧结温度为1900～2300℃，保温时间为60～120min。
将获得的SiC基复相陶瓷加工成Φ12mm厚度2mm的圆片，并将其两端磨平，在其两端均匀涂覆上银浆电极，然后将其在马弗炉中750℃保温10min。
将获得的SiC陶瓷圆片经电化学工作站(IM6，ZAHNER，Germany)测试系统在不同温度下进行测试，不同ZrB2含量的碳化硅基复相高温热敏陶瓷材料的电学特征均在低温下(＜600℃)表现为压敏电阻的非线性伏安特性，高温下(＞600℃)转变为欧姆电阻的线性伏安特性，且高温下的电阻率大大小于低温下的电阻率，在1.21～4.09Ω·cm之间。
经电化学工作站(IM6，ZAHNER，Germany)测试系统测试获得不同ZrB2含量常压固相烧结SiC陶瓷在不同温度下的测得的伏安特性曲线如图1，图2和图3所示。
本发明经阿基米德法测量所得碳碳化硅基复相高温热敏陶瓷材料的密度可为3.17～3.59g·cm-3。经三点弯曲法测量所得碳化硅基复相高温热敏陶瓷材料抗弯强度可为310～350MPa。该SiC/ZrB2复相陶瓷具有特殊的应用价值，有望作为在超高温、强酸强碱等苛刻环境下运行的特种电子元件。
下面进一步例举实施例以详细说明本发明。同样应理解，以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例，即本领域技术人员可以通过本文的说明做合适的范围内选择，而并非要限定于下文示例的具体数值。
实施例1
SiC、ZrB2(12wt％)、烧结助剂B4C(0.6wt％)一共100g，酚醛树脂10g，将粉体配成固含量为45wt％的浆料(溶剂为酒精)，以SiC球200g为球磨介质，混合24h。然后干燥过筛，得到的粉体在平板机上15MPa压力成型，然后在200MPa压力下等静压。脱粘后在常压Ar气氛下烧结，烧结温度为2100℃，保温时间1h，得到的SiC基复相陶瓷密度为3.32g·cm-3，抗弯强度为341MPa。将获得的陶瓷制成Φ12mm厚度2mm的小圆片，两端涂覆银浆电极，然后将其在马弗炉中750℃保温10min，获得的电子元件经电化学工作站测试系统测试，在600℃以下表现为压敏电阻的非线性伏安特性，在600℃以上表现为欧姆电阻的线性伏安特性，温度升高电阻率逐渐下降，测试温度从600℃升到800℃时，电阻率相应的从5.98Ω·cm降到1.87Ω·cm。
实施例2
SiC、ZrB2(16wt％)、烧结助剂B4C(0.6wt％)一共100g，酚醛树脂10g，将粉体配成固含量为45wt％的浆料(溶剂为酒精)，以SiC球200g为球磨介质，混合24h。然后干燥过筛，得到的粉体在平板机上15MPa压力成型，然后在200MPa压力下等静压。脱粘后在常压Ar气氛下烧结，烧结温度为2100℃，保温时间1h，得到的SiC基复相陶瓷密度为3.38g·cm-3，抗弯强度为334MPa。将获得的陶瓷制成Φ12mm厚度2mm的小圆片，两端涂覆银浆电极，然后将其在马弗炉中750℃保温10min，获得的电子元件经电化学工作站测试系统在不同温度下进行测试，如图2所示，在600℃以下表现为压敏电阻的非线性伏安特性，在600℃以上表现为欧姆电阻的线性伏安特性，温度升高电阻率逐渐下降，测试温度从600℃升到800℃时，电阻率相应的从3.03Ω·cm降到1.44Ω·cm。
实施例3
SiC、ZrB2(24wt％)、烧结助剂B4C(0.6wt％)一共100g，PVA 5g，将粉体配成固含量为45wt％的浆料(溶剂为水)，以SiC球200g为球磨介质，混合24h。然后喷雾造粒，得到的粉体在平板机上15MPa压力成型，然后在200MPa压力下等静压，脱粘后在常压Ar气气氛下烧结，烧结温度为2100℃，保温时间1h，得到的SiC基复相陶瓷密度为3.55g·cm-3，抗弯强度为310MPa。将获得的陶瓷制成Φ12mm厚度2mm的小圆片，两端涂覆银浆电极，然后将其在马弗炉中750℃保温10min，获得的电子元件经电化学工作站测试系统在不同温度下进行测试，如图3所示，在600℃以下表现为压敏电阻的非线性伏安特性，在600℃以上表现为欧姆电阻的线性伏安特性，温度升高电阻率逐渐下降，测试温度从600℃升到800℃时，电阻率相应的从1.80Ω·cm降到1.20Ω·cm。
实施例4
SiC、ZrB2(28wt％)、烧结助剂B4C(0.6wt％)一共100g，酚醛树脂10g，将粉体配成固含量为45wt％的浆料(溶剂为酒精)，以SiC球200g为球磨介质，混合24h。然后干燥过筛，得到的粉体在平板机上15MPa压力成型，然后在200MPa压力下等静压。脱粘后在常压Ar气氛下烧结，烧结温度为2100℃，保温时间1h，得到的SiC基复相陶瓷密度为3.64g·cm-3，抗弯强度为316MPa。将获得的陶瓷制成Φ12mm厚度2mm的小圆片，两端涂覆银浆电极，然后将其在马弗炉中750℃保温10min，获得的电子元件经电化学工作站测试系统测试，如图4所示，其伏安特性均表现出欧姆电阻的线性特征。

Claims (3)

1.一种碳化硅基复相高温热敏陶瓷材料，其特征在于，所述碳化硅基复相高温热敏陶瓷材料包括碳化硅基体材料和ZrB2第二相材料，所述ZrB2第二相材料的含量为2～26wt%；当ZrB2含量在2～26wt%变化时，所述碳化硅基复相高温热敏陶瓷材料在＜600℃下具有压敏电阻的非线性伏安特性、在600℃以上的高温下转变为欧姆电阻的线性伏安特性且电阻率在1.2～6.0 Ω·cm之间。
2.根据权利要求1所述的碳化硅基复相高温热敏陶瓷材料，其特征在于，所述碳化硅基复相高温热敏陶瓷材料的密度为3.17～3.59g·cm-3，抗弯强度为310～350MPa。
3.一种调节碳化硅基复相高温热敏陶瓷材料的高温热敏电阻特性的方法，其特征在于，以B或B4C中的至少一种作为烧结助剂，以酚醛树脂、PVA、PVB中的至少一种作为粘结剂无压固相烧结制备碳化硅基复相高温热敏陶瓷材料，通过控制ZrB2第二相材料的含量在2～26wt%之间，以调节碳化硅基复相高温热敏陶瓷材料在600℃以上的高温下转变为欧姆电阻的线性伏安特性且电阻率在1.2～6.0 Ω·cm之间可控。
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