CN106278277B - 一种尖锥形碳化硅陶瓷吸收体及其制备方法 - Google Patents
一种尖锥形碳化硅陶瓷吸收体及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种尖锥形碳化硅陶瓷吸收体及其制备方法。具体而言，本发明的尖锥形碳化硅陶瓷吸收体由以重量百分比计的下列组分制成：40～60％的SiC、5～15％的SiO2、15～20％的MgO、0～10％的BaCO3、0～3％的MnO2、0～2％的CoO、0～2％的V2O5、0～2％的Al2O3、5～10％的半精炼石蜡、1～5％的PE塑化剂。上述组分经高温混炼后，注塑成型为尖锥形，经脱脂和烧结，制得最终产品。本发明采用注塑成型法制备具备宽带吸收性能的角锥型陶瓷吸收体，工艺简单，材料性能稳定，具有导热系数好，半球发射率高，真空适用性强等特点。
Description
技术领域
本发明属于功能材料技术领域，具体涉及一种尖锥形碳化硅陶瓷吸收体及其制备方法。
背景技术
作为一种高温电介质型吸收剂，碳化硅材料已有多年研究和应用的历史，主要应用于吸波涂料、规则形状的负载等，但作为宽带吸收部件(如四棱锥吸收器)国内外鲜有研究。随着雷达天线技术及电子测量技术的发展，对于大带宽并且能够承受大功率的吸收部件的需求与日俱增。
吸波箱是基于现代天线测试技术提出的，它是一种小型的微波暗室，同样具备暗室所要求的屏蔽和吸波性能。一般的吸波箱主要针对小型天线(如Bluetooth、Wi-Fi、OTA以及RFID等简单产品)的测试，对吸收率要求较低，带宽窄，不耐功率(≤1kW)，制造成本低。
吸波箱的屏蔽部分主要采用钢板焊接或钢板拼装而成，吸波部分主要是在屏蔽壳体内部贴装聚氨酯泡沫吸波材料，它的致命弱点是易老化、易燃烧、耐功率性差，并且多采用化学黏合剂进行安装，环保性较差，虽然近几年做出了适当改进，如Rantec公司采用包覆橡胶薄膜的方法提高耐候性，但收效甚微。聚氨酯泡沫吸波材料氧指数低(一般为28％)，在遇明火的时候会燃烧，最近的2012年某研究所新装微波暗室发生严重火灾，损失严重，其使用的就是易燃的软质聚氨酯泡沫材料。软质聚氨酯海绵吸波材料使用若干年后，大多会出现垂头现象，使微波吸收性能急剧变差，所以一般吸波箱寿命较短。
一般吸波箱配合高低温综合试验箱使用，其吸波材料经常处于高温高湿以及温度冲击环境条件下，情况会更糟，具有腐蚀性的炭黑粒子会从泡沫体中渗出，直接腐蚀箱体和待测件。2013年中国电科第五研究所对T/R组件进行环境试验，经常发现T/R组件中线路被腐蚀的问题。
现在，对于部分小功率雷达天线的环境试验测试采取的方法一般是在天线的正对面摆上一只吸波屏风或连接一台普通的吸波箱进行雷达天线测试。如果是大功率情况下(≥15kW/m2)，为了安全起见，不开功率或给予很小的功率进行环境试验，而这并不能真实表征产品工作状态下的性能。针对开机状态下(特别是大功率条件下)的环境试验测试所用到的吸波箱未有报道，常规途径未能获得国内外相关资料，可以认为该项技术目前在国内仍处于空白，可以确信主要原因是缺少能够应用于大功率场合的吸波材料。
此外，在卫星天线真空状态测试过程中，应该严格控制整个吸波箱的可凝挥发物，且吸波体要有良好的导热率。一般的吸波体如聚氨酯会掉碳粉很难满足要求，而碳化硅陶瓷吸收体可满足使用要求。
发明内容
为了解决上述技术问题，本发明的目的在于提供一种具有高吸收、耐功率、真空适用能力强、导热良好、生产工艺简单、成本低的尖锥形碳化硅陶瓷吸收体及其制备方法，具体提供了一种以SiC、SiO2、MgO、BaCO3、MnO2、CoO、V2O5、Al2O3、半精炼石蜡和PE塑化剂为原料的尖锥形大功率碳化硅陶瓷吸收体及其制备方法，吸收体在1～18GHz内可获得大于20dB的吸收，耐功率不小于30kW(平均功率)，材料具有导热系数5.5w·m-1℃-1，涂层半球发射率0.85以上，真空总质量损失TML≤1％。
为了达到以上目的，本发明采用如下技术方案：
一种尖锥形碳化硅陶瓷吸收体，其由以重量百分比计的下列组分制成：40～60％的SiC、5～15％的SiO2、15～20％的MgO、0～10％的BaCO3、0～3％的MnO2、0～2％的CoO、0～2％的V2O5、0～2％的Al2O3、5～10％的半精炼石蜡、1～5％的PE塑化剂。
优选的，上述尖锥形碳化硅陶瓷吸收体由以重量百分比计的下列组分制成：55～60％的SiC、5～15％的SiO2、15～18的MgO、0～3％的BaCO3、0～0.5％的MnO2、0～0.8％的CoO、0～1％的V2O5、0～1.2％的Al2O3、5～10％的半精炼石蜡、1～3.5％的PE塑化剂。
优选的，上述尖锥形碳化硅陶瓷吸收体的外形为四棱锥形，锥体高度为50～90毫米，底面边长为10～20毫米。
在上述尖锥形碳化硅陶瓷吸收体中，所述半精炼石蜡是一种板块状白色固体，其相对密度随熔点的上升而增加，化学稳定性好，含油量适中，具有良好的防潮和绝缘性能，可塑性好，广泛用于各个行业领域，与广大人民群众生活息息相关。
在上述尖锥形碳化硅陶瓷吸收体中，所述PE塑化剂是一种高分子材料助剂，其种类繁多，最常见的品种是低密度聚乙烯，工业上应用广泛。
一种上述尖锥形碳化硅陶瓷吸收体的制备方法，其包括以下步骤：
a)按照预定的重量百分比称取各种组分，并置于混炼机中混炼，得到块料；
b)将步骤a)中所得块料置于粉碎机中粉碎，得到颗粒料；
c)将步骤b)中所得颗粒料置于注塑成型机的料筒中注塑成型，坯体脱模冷却至室温，得到陶瓷生坯；
d)将步骤c)中所得陶瓷生坯置于汽油介质中预脱脂，取出后自然晾干，得到预脱脂生坯；
e)将步骤d)中所得预脱脂生坯置于烧结炉中完全脱脂，得到完全脱脂生坯；
f)将步骤e)中所得完全脱脂生坯置于莫来石承烧盒中烧结，得到最终的尖锥形碳化硅陶瓷吸收体。
优选的，在上述制备方法中，步骤a)中所述混炼的程序为先将半精炼石蜡和PE塑化剂熔化，再逐一加入其他组分，温度为100～120℃，转速为30～40转/分钟，时间为0.5～3小时。
优选的，在上述制备方法中，步骤b)中所述颗粒料的粒径为1～5毫米。
优选的，在上述制备方法中，步骤c)中所述注塑成型机的注塑温度为100～200℃，成型压力为5～10MPa。
优选的，在上述制备方法中，步骤d)中所述预脱脂的浸泡时间为24～36小时。
优选的，在上述制备方法中，步骤e)中所述完全脱脂的温度为800～1000℃，时间为3～5小时。
优选的，在上述制备方法中，步骤f)中所述烧结的升温速度在3℃/分钟以内，温度为1280～1380℃，时间为3～5小时。
与现有技术相比，采用上述技术方案的本发明具有以下有益效果：
1、本发明通过调整碳化硅的百分含量，获得吸收比高的陶瓷体，经检测具有较宽的吸收频带，吸收率高，耐功率及导热性好，真空适用性强等特点；
2、通过选择塑化成型工艺，成功制备了尖锥形陶瓷吸收体，该工艺避免了磨加工的工序，节省了大量劳动成本；
3、该体系可以在空气中烧结，助剂的使用可以细化晶粒，使晶粒生长均匀，瓷体气孔率降低，电性能得到提高，同时降低了烧结温度，从而节约烧结成本；
4、本发明的产品适合批量化生产，成本较低，具有较大的经济价值。
附图说明
图1为本发明的尖锥形碳化硅陶瓷吸收体的外形图。
图2为本发明实施例2所得尖锥形碳化硅陶瓷吸收体的扫描电镜图(SEM)。
具体实施方式
以下将结合附图和具体实施例来进一步说明本发明中的技术方案。除非另有说明，下列实施例中所使用的仪器、材料、试剂等均可通过商业手段获得。
实施例1：尖锥形碳化硅陶瓷吸收体的制备及性能测试。
a)按照下列重量百分比称取各种组分：55％的SiC、7％的SiO2、18％的MgO、3％的BaCO3、0.5％的MnO2、0.8％的CoO、1％的V2O5、1.2％的Al2O3、10％的半精炼石蜡、3.5％的低密度聚乙烯颗粒，并将上述各种组分置于混炼机中混炼，温度为100℃，转速为30转/分钟，时间为3小时，出料时为色泽均匀的块料；
b)将步骤a)中所得混合料置于粉碎机中粉碎，得到颗粒料，粒径为2～4毫米；
c)将步骤b)中所得颗粒料置于注塑成型机的料筒中注塑成型，注塑温度为150℃，成型压力为10MPa，坯体脱模冷却至室温，得到陶瓷生坯；
d)将步骤c)中所得陶瓷生坯置于汽油介质中进行预脱脂，浸泡时间为24小时，取出后自然晾干，得到预脱脂生坯；
e)将步骤d)中所得预脱脂生坯置于烧结炉中进行完全脱脂，脱脂温度为800℃，保温3小时，得到完全脱脂生坯；
f)将步骤e)中所得完全脱脂生坯置于莫来石承烧盒中，升温速度为3℃/分钟，于1280℃下烧结5小时，得到最终的尖锥形碳化硅陶瓷吸收体，四棱锥体的高度为90毫米，底面尺寸为20毫米×20毫米，其外形图如图1所示。
利用GJB 5239-2004规定的弓形法测定样品的微波吸收性能，结果显示在4～8GHz带宽内优于-30dB。
实施例2：尖锥形碳化硅陶瓷吸收体的制备及性能测试。
a)按照下列重量百分比称取各种组分：60％的SiC、5％的SiO2、15％的MgO、3％的BaCO3、0.5％的MnO2、0.8％的CoO、1％的V2O5、1.2％的Al2O3、10％的半精炼石蜡、3.5％的低密度聚乙烯颗粒，并将上述各种组分置于混炼机中混炼，温度为100℃，转速为30转/分钟，时间为2小时，出料时为色泽均匀的块料；
b)将步骤a)中所得料块置于粉碎机中粉碎，得到颗粒料，粒径为2～4mm；
c)将步骤b)中所得颗粒料置于注塑成型机的料筒中注塑成型，注塑成型机的注塑温度为150℃，成型压力为10MPa，坯体脱模冷却至室温，得到陶瓷生坯；
d)将步骤c)中所得陶瓷生坯置于汽油介质中预脱脂，浸泡时间为36小时，取出后自然晾干，得到预脱脂生坯；
e)将步骤d)中所得预脱脂生坯置于烧结炉中完全脱脂，脱脂温度为800℃，保温3小时，得到完全脱脂生坯；
f)将步骤e)中所得完全脱脂生坯置于莫来石承烧盒中，升温速度为3℃/分钟，于1380℃下烧结5小时，得到最终的尖锥形碳化硅陶瓷吸收体，四棱锥体的高度为50毫米，底面尺寸为10毫米×10毫米。
利用GJB 5239-2004规定的弓形法测定样品的微波吸收性能，结果显示在8～12GHz带宽内优于-25dB。
对样品的横断面进行SEM扫描，其结果如图2所示。从图2中可知，陶瓷吸收体的微观结构均匀，体系中含有较多的玻璃相。
Claims (6)
1.一种尖锥形碳化硅陶瓷吸收体，其由以重量百分比计的下列组分制成：55～60％的SiC、5～15％的SiO2、15～18％的MgO、0～3％的BaCO3、0～0.5％的MnO2、0～0.8％的CoO、0～1％的V2O5、0～1.2％的Al2O3、5～10％的半精炼石蜡、1～3.5％的PE塑化剂，且所述BaCO3、MnO2、CoO、V2O5以及Al2O3的含量均不为0；所述尖锥形碳化硅陶瓷吸收体的外形为四棱锥形，锥体高度为50～90毫米，底面边长为10～20毫米；所述尖锥形碳化硅陶瓷吸收体由以下制备方法制备：
a)按照预定的重量百分比称取各种组分，并置于混炼机中混炼，得到块料；
b)将步骤a)中所得块料置于粉碎机中粉碎，得到颗粒料；
c)将步骤b)中所得颗粒料置于注塑成型机的料筒中注塑成型，坯体脱模冷却至室温，得到陶瓷生坯；
d)将步骤c)中所得陶瓷生坯置于汽油介质中预脱脂，取出后自然晾干，得到预脱脂生坯；
e)将步骤d)中所得预脱脂生坯置于烧结炉中完全脱脂，得到完全脱脂生坯；
f)将步骤e)中所得完全脱脂生坯置于莫来石承烧盒中烧结，得到最终的尖锥形碳化硅陶瓷吸收体；所述烧结的升温速度在3℃/分钟以内，温度为1280～1380℃，时间为3～5小时。
2.根据权利要求1所述的尖锥形碳化硅陶瓷吸收体，其特征在于，步骤a)中所述混炼的程序为先将半精炼石蜡和PE塑化剂熔化，再逐一加入其他组分，温度为100～120℃，转速为30～40转/分钟，时间为0.5～3小时。
3.根据权利要求1所述的尖锥形碳化硅陶瓷吸收体，其特征在于，步骤b)中所述颗粒料的粒径为1～5毫米。
4.根据权利要求1所述的尖锥形碳化硅陶瓷吸收体，其特征在于，步骤c)中所述注塑成型机的注塑温度为100～200℃，成型压力为5～10MPa。
5.根据权利要求1所述的尖锥形碳化硅陶瓷吸收体，其特征在于，步骤d)中所述预脱脂的浸泡时间为24～36小时。
6.根据权利要求1所述的尖锥形碳化硅陶瓷吸收体，其特征在于，步骤e)中所述完全脱脂的温度为800～1000℃，时间为3～5小时。
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