CN108147834A - 介电常数可调控的轻质氮化硅天线罩及其制备方法 - Google Patents

介电常数可调控的轻质氮化硅天线罩及其制备方法 Download PDF

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CN108147834A
CN108147834A CN201711435061.0A CN201711435061A CN108147834A CN 108147834 A CN108147834 A CN 108147834A CN 201711435061 A CN201711435061 A CN 201711435061A CN 108147834 A CN108147834 A CN 108147834A
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silicon nitride
dielectric constant
regulatable
oxide
antenna house
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王洪升
张萍萍
朱保鑫
韦其红
栾强
盖莹
温广武
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Abstract

本发明属于结构功能陶瓷材料领域，具体的涉及一种介电常数可调控的轻质氮化硅天线罩及其制备方法。以质量分数计，原料组成如下：氮化硅粉体70～95％，碳化硅粉体0～10％，造孔剂0～25％和稀土氧化物粉体3～15％。本发明利用冷等静压成型，通过控制成型压力和造孔剂含量，可实现素坯密度的控制，更容易实现复杂薄壁结构天线罩的均匀性、一致性控制；SiC与Si3N4的热学、力学等性能接近且不发生物理化学反应，经氧化处理后SiC表面被SiO2包覆，可使材料介电常数大幅提升，介电损耗小幅变化，因此适量SiO2包覆SiC的引入可作为高介电常数组分使用。

Description

介电常数可调控的轻质氮化硅天线罩及其制备方法
技术领域
本发明属于结构功能陶瓷材料技术领域，具体的涉及一种介电常数可调控的轻质氮化硅天线罩及其制备方法。
背景技术
氮化硅陶瓷是结构陶瓷中综合性能最好的材料之一，具有优良的电学、热学、力学和抗热震性能；多孔氮化硅陶瓷具有较低的介电常数、介电损耗角正切、低密度和合适的强度，优良的综合性能在航空航天透波材料(天线罩、天线窗)的研制方面有很大的应用空间。
早在20世纪80年代美国波音公司开发了“可控密度氮化硅”制备技术，密度可从0.5g/cm3到1.8g/cm3调控；该工艺在氮化硅粉末本体中内嵌孔道，并在粉末压制之后除去孔道，经反应烧结和β-Si3N4生长形成多孔氮化硅陶瓷，通过控制孔隙量，改变材料密度，进而达到控制材料介电常数的目的。1992年美国Verzemnieks等以氮化硅粉体、硅粉、萘及樟脑等造孔剂为原料，通过控制其含量，采用反应烧结技术制备了前部密度0.75～1.0g/cm3，后部密度1.6～2.0g/cm3的氮化硅天线罩。上述研究工作提出了通过降低材料密度，使材料介电常数发生变化的制备方法，但针对弹头电气性能和重量具有特殊需求的战术武器装备，如在较低密度下使陶瓷透波材料的介电常数提高或可调控的方法，国内外还未见报道。
发明内容
本发明的目的是克服现有技术的不足，提供一种介电常数可调控的轻质氮化硅天线罩，实现多孔氮化硅陶瓷材料密度和介电常数的双向调控，且使调控范围满足实际需求；本发明同时提供了其制备方法。
本发明所述的介电常数可调控的轻质氮化硅天线罩，以质量分数计，原料组成如下：
其中：
造孔剂是聚甲基丙烯酸甲酯、苯甲酸、碳酸氢铵、尿素、聚维酮、聚乙二醇或聚乙烯醇中的一种或几种。
稀土氧化物粉体是氧化镱、氧化铥、氧化钇、氧化铒、氧化钆、氧化镧、氧化镝、氧化镨、氧化铽、氧化铈、氧化钕、氧化镥或氧化铕中的一种或几种。
本发明所述的介电常数可调控的轻质氮化硅天线罩的制备方法，具体步骤如下：
(1)原材料预处理
将氮化硅粉体、碳化硅粉体、造孔剂和稀土氧化物粉体在无水乙醇溶剂中球磨混合，然后经喷雾造粒制备成造粒粉体；
(2)冷等静压成型
将造粒粉体装入仿形成型模具中，然后在冷等静压成型机中成型，成型压力30～200MPa；
(3)脱脂-气氛压力烧结
将素坯在真空脱脂炉中脱脂，然后在气氛压力烧结炉内大于0.2MPa的压力、氮气气氛下，1650～1850℃进行烧结；
(4)氧化处理
将烧结后坯体在氧化气氛下、600～1000℃下热处理大于1h；
(5)精密加工
将热处理后坯体精密加工到预设尺寸。
其中：
制备时，步骤(4)氧化处理和步骤(5)精密加工两个步骤的顺序可调整。
步骤(4)中氧化气氛是空气气氛或富氧气氛。
步骤(3)中所述的脱脂过程是温度为200℃～600℃，真空度小于等于-0.09MPa。
作为一个优选的技术方案，本发明所述的介电常数可调控的轻质氮化硅天线罩的制备方法，步骤如下：
(1)原材料预处理
将Si3N4粉体、SiC粉体、造孔剂和稀土氧化物粉体按照配比在无水乙醇等溶剂中球磨，混合均匀，然后经喷雾造粒制备成造粒粉体；
(2)冷等静压成型
将造粒粉体装入仿形成型模具中，然后在冷等静压成型机中成型，成型压力30～200MPa；
(3)脱脂-气氛压力烧结
将素坯在真空脱脂炉中脱脂，脱脂过程温度为200℃～600℃，真空度≤-0.09MPa，脱脂过程升温速度根据制品大小控制在0.05℃/min～1℃/min；然后在气氛压力烧结炉内＞0.2MPa的压力下，氮气气氛下，1650～1850℃下烧结2～4h；
(4)氧化处理
将烧结后坯体在氧化气氛下600～1000℃下热处理大于1h；
(5)精密加工
将热处理后坯体通过内外圆磨床，精密加工到预设尺寸，获得氮化硅陶瓷天线罩。
本发明以多孔氮化硅材料为基础，通过调控其密度和高介电组分SiC粉体含量实现其电气性能、力学性能和重量的控制。陶瓷制备完成后，在氧化气氛下热处理，SiC表面将被氧化产生SiO2，可使材料介电常数大幅提升，介电损耗小幅变化。
本发明具有以下有益效果：
(1)利用冷等静压成型，通过控制成型压力和造孔剂含量，可实现素坯密度的控制，更容易实现复杂薄壁结构天线罩的均匀性和一致性的控制；
(2)采用造孔剂，在真空热处理过程中均可通过分解或升华排除，低温冷却后均可收集，不会对环境造成污染；
(3)SiC与Si3N4的热学、力学等性能接近且不发生物理化学反应，经氧化处理后SiC表面被SiO2包覆，可使材料介电常数大幅提升，介电损耗小幅变化，因此适量SiO2包覆SiC的引入可作为高介电常数组分使用。
具体实施方式
以下结合实施例对本发明作进一步描述。
实施例1
将氮化硅粉体95wt％、氧化镥粉体5wt％与无水乙醇，利用氮化硅研磨球球磨72h，均匀混合，然后经喷雾造粒制备成造粒粉体。
将造粒粉体装入天线罩仿形成型模具中，然后在冷等静压成型机中以50MPa成型。
将素坯在真空脱脂炉中脱脂，以1℃/min的升温速度从200℃缓慢升温至600℃，真空度≤-0.09MPa；然后将素坯转移至气氛压力烧结炉内，充入0.2MPa的N2，缓慢升温至1700℃下保温2h，然后随炉冷却；将烧结后坯体在马弗炉内缓慢升温至750℃，保温4h。
将热处理后坯体利用内圆磨床、外圆磨床，精密加工到预设尺寸，获得氮化硅陶瓷天线罩。
上述方法制备的氮化硅陶瓷天线罩密度为1.65g/cm3，弯曲强度为180MPa，介电常数为3.1，介电损耗角正切为3×10-3。
实施例2
将氮化硅粉体80wt％、碳化硅粉体5wt％、氧化镧粉体6wt％、氧化钐粉体4wt％、聚甲基丙烯酸甲酯5wt％与无水乙醇，利用氮化硅研磨球球磨24h，均匀混合，然后经喷雾造粒制备成造粒粉体。
将造粒粉体装入天线罩仿形成型模具中，然后在冷等静压成型机中以30MPa成型。
将素坯在真空脱脂炉中脱脂，以0.5℃/min的升温速度从200℃缓慢升温至400℃，真空度≤-0.09MPa；然后将素坯转移至气氛压力烧结炉内，充入1.0MPa的N2，缓慢升温至1750℃下保温2h，然后随炉冷却；将烧结后坯体在马弗炉内缓慢升温至850℃，保温3h。
将热处理后坯体利用内圆磨床、外圆磨床，精密加工到预设尺寸，获得氮化硅陶瓷天线罩。
上述方法制备的氮化硅陶瓷天线罩密度为1.40g/cm3，弯曲强度为90MPa，介电常数为3.3，介电损耗角正切为6.5×10-3。
实施例3
将氮化硅粉体75wt％、碳化硅粉体4wt％、氧化钇粉体3wt％、氧化镱粉体3wt％、苯甲酸15wt％与无水乙醇，利用氮化硅研磨球球磨48h，均匀混合，然后经喷雾造粒制备成造粒粉体。
将造粒粉体装入天线罩仿形成型模具中，然后在冷等静压成型机中以80MPa成型。
将素坯在真空脱脂炉中脱脂，以0.3℃/min的升温速度从200℃缓慢升温至600℃，真空度≤-0.095MPa；然后将素坯转移至气氛压力烧结炉内，充入1.2MPa的N2，缓慢升温至1800℃下保温2h，然后随炉冷却；将烧结后坯体在马弗炉内缓慢升温至900℃，保温4h。
将热处理后坯体利用内圆磨床、外圆磨床，精密加工到预设尺寸，获得氮化硅陶瓷天线罩。
上述方法制备的氮化硅陶瓷天线罩密度为1.10g/cm3，弯曲强度为60MPa，介电常数为3.0，介电损耗角正切为6.5×10-3。
实施例4
将氮化硅粉体75wt％、氧化钇粉体5wt％、氧化铈粉体5wt％、聚乙烯醇15wt％与无水乙醇，利用氮化硅研磨球球磨40h，均匀混合，然后经喷雾造粒制备成造粒粉体。
将造粒粉体装入天线罩仿形成型模具中，然后在冷等静压成型机中以110MPa成型。
将素坯在真空脱脂炉中脱脂，以0.3℃/min的升温速度从250℃缓慢升温至600℃，真空度≤-0.095MPa；然后将素坯转移至气氛压力烧结炉内，充入0.7MPa的N2，缓慢升温至1850℃下保温2h，然后随炉冷却；将烧结后坯体在马弗炉内缓慢升温至950℃，保温4h。
将热处理后坯体利用内圆磨床、外圆磨床，精密加工到预设尺寸，获得氮化硅陶瓷天线罩。
上述方法制备的氮化硅陶瓷天线罩密度为1.15g/cm3，弯曲强度为60MPa，介电常数为2.3，介电损耗角正切为3×10-3。

Claims (7)

1.一种介电常数可调控的轻质氮化硅天线罩，其特征在于：以质量分数计，原料组成如下：
2.根据权利要求1所述的介电常数可调控的轻质氮化硅天线罩，其特征在于：造孔剂是聚甲基丙烯酸甲酯、苯甲酸、碳酸氢铵、尿素、聚维酮、聚乙二醇或聚乙烯醇中的一种或几种。
3.根据权利要求1所述的介电常数可调控的轻质氮化硅天线罩，其特征在于：稀土氧化物粉体是氧化镱、氧化铥、氧化钇、氧化铒、氧化钆、氧化镧、氧化镝、氧化镨、氧化铽、氧化铈、氧化钕、氧化镥或氧化铕中的一种或几种。
4.一种权利要求1所述的介电常数可调控的轻质氮化硅天线罩的制备方法，其特征在于：具体步骤如下：
(1)原材料预处理
将氮化硅粉体、碳化硅粉体、造孔剂和稀土氧化物粉体在无水乙醇溶剂中球磨混合，然后经喷雾造粒制备成造粒粉体；
(2)冷等静压成型
将造粒粉体装入仿形成型模具中，然后在冷等静压成型机中成型，成型压力30～200MPa；
(3)脱脂-气氛压力烧结
将素坯在真空脱脂炉中脱脂，然后在气氛压力烧结炉内大于0.2MPa的压力、氮气气氛下，1650～1850℃进行烧结；
(4)氧化处理
将烧结后坯体在氧化气氛下、600～1000℃下热处理大于1h；
(5)精密加工
将热处理后坯体精密加工到预设尺寸。
5.根据权利要求4所述的介电常数可调控的轻质氮化硅天线罩的制备方法，其特征在于：步骤(4)氧化处理和步骤(5)精密加工两个步骤的顺序可调整。
6.根据权利要求4所述的介电常数可调控的轻质氮化硅天线罩的制备方法，其特征在于：步骤(4)中氧化气氛是空气气氛或富氧气氛。
7.根据权利要求4所述的介电常数可调控的轻质氮化硅天线罩的制备方法，其特征在于：步骤(3)中所述的脱脂过程是温度为200℃～600℃，真空度小于等于-0.09MPa。
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