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
[0001] 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
[0002] 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。
[0003] 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;该工艺在氮化娃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P-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等以氮化娃粉体、娃粉、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〇. 75〜I. Og/cm3,后 部密度1.6〜2.Og/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
[0004] 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。
[0005] 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: 氮化硅(Si3N4)粉体 70〜95% 碳化硅(SiC)粉体 0-10%
[0006] 造孔剂 0~25% 稀土氧化物粉体 3〜15%。
[0007] 其中:
[0008] 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。
[0009] 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。
[0010] 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:
[0011] (1)原材料预处理
[0012] 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;
[0013] (2)冷等静压成型
[00M]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;
[0015] (3)脱脂-气氛压力烧结
[0016] 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°C进行烧结;
[0017] ⑷氧化处理
[0018] 将烧结后坯体在氧化气氛下、600〜1000°C下热处理大于Ih;
[0019] (5)精密加工
[0020] 将热处理后坯体精密加工到预设尺寸。
[0021] 其中:
[0022] 制备时,步骤⑷氧化处理和步骤⑶精密加工两个步骤的顺序可调整。
[0023] 步骤⑷中氧化气氛是空气气氛或富氧气氛。
[0024] 步骤⑶中所述的脱脂过程是温度为200°C〜600°C,真空度小于等于_0.09MPa。
[0025] 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:
[0026] (1)原材料预处理
[0027] 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;
[0028] ⑵冷等静压成型
[0029] 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;
[0030] ⑶脱脂-气氛压力烧结
[0031] 将素坯在真空脱脂炉中脱脂,脱脂过程温度为200°C〜600°C,真空度彡_0.09MPa, 脱脂过程升温速度根据制品大小控制在〇.〇5°C/min〜rC/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°C下烧结2〜4h;
[0032] ⑷氧化处理
[0033] 将烧结后坯体在氧化气氛下600〜1000°C下热处理大于Ih;
[0034] (5)精密加工
[0035] 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。
[0036] 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。
[0037] 本发明具有以下有益效果:
[0038] (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;
[0039] (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;
[0040] (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
[0041] 以下结合实施例对本发明作进一步描述。
[0042] 实施例1
[0043] 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。
[0044] 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。
[0045] 将素坯在真空脱脂炉中脱脂,以TC/min的升温速度从200°C缓慢升温至600°C,真 空度《. 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 °C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°C,保温4h。
[0046] 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。
[0047] 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 X 10_3。
[0048] 实施例2
[0049] 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。
[0050] 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。
[0051] 将素坯在真空脱脂炉中脱脂,以〇.5°C/min的升温速度从200°C缓慢升温至400°C, 真空度彡_〇.〇9MPa;然后将素坯转移至气氛压力烧结炉内,充入1.01〇^的仏,缓慢升温至 1750°C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°C,保温3h。
[0052] 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。
[0053] 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 X 10_3。
[0054] 实施例3
[0055] 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。
[0056] 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SOMPa成型。
[0057] 将素坯在真空脱脂炉中脱脂,以0.3°C/min的升温速度从200°C缓慢升温至600°C, 真空度彡-0. 〇95MPa;然后将素坯转移至气氛压力烧结炉内,充入1.210^的吣,缓慢升温至 1800°C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°C,保温4h。
[0058] 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。
[0059] 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 X 10_3。
[0060] 实施例4
[0061] 将氮化娃粉体75wt%、氧化纪粉体5wt%、氧化铺粉体5wt%、聚乙稀醇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。
[0062] 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IlOMPa成 型。
[0063] 将素坯在真空脱脂炉中脱脂,以0.3°C/min的升温速度从250°C缓慢升温至600°C, 真空度彡-0. 〇95MPa;然后将素坯转移至气氛压力烧结炉内,充入0.710^的吣,缓慢升温至 1850°C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°C,保温4h。
[0064] 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。
[0065] 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 X 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:
Figure CN108147834AC00021
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; ⑵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; ⑶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〇 . 2MPa的压力、氮气气氛 下,1650〜1850°C进行烧结; ⑷氧化处理 将烧结后还体在氧化气氛下、600〜1000 °C下热处理大于Ih; ⑸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⑷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⑷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⑶中所述的脱脂过程是温度为200°C〜600°C,真空度小于等于-0.09MPa。
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