CN114455943A - 一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法 - Google Patents

一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法 Download PDF

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CN114455943A
CN114455943A CN202210328147.8A CN202210328147A CN114455943A CN 114455943 A CN114455943 A CN 114455943A CN 202210328147 A CN202210328147 A CN 202210328147A CN 114455943 A CN114455943 A CN 114455943A
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魏汉军
赵峰
王清远
余亚苹
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Abstract

本发明涉及一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，属于微波吸收材料技术领域。本发明将Si(OC2H5)4溶解于乙醇中得到溶液A，Y(NO3)3·6H2O搅拌溶解于去离子水中得到溶液B；室温下，溶液A和溶液B搅拌混合得到凝胶C，凝胶C干燥得到干凝胶，干凝胶研磨成凝胶粉，凝胶粉进行冷压成型后置于温度为1400～1500℃的空气中烧结热处理2～3h，得到Y2Si2O7粉末；Y2Si2O7粉末采用碳化硅化学气相渗透技术沉积，得到SiC‑Y2Si2O7复合陶瓷，SiC‑Y2Si2O7复合陶瓷经温度为1100～1200℃下氧化2～3h，得到SiO2/SiC‑Y2Si2O7复合陶瓷，SiO2/SiC‑Y2Si2O7复合陶瓷经氮化硅化学气相渗透技术沉积得到Si3N4/SiO2/SiC‑Y2Si2O7复合陶瓷。本发明复相陶瓷的电磁波吸收性能的可控性调节。

Description

一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制 备方法
技术领域
本发明涉及一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，属于微波吸收材料技术领域。
背景技术
无线通信和雷达探测技术已成为爆炸性的应用，严重威胁着人类健康、国防和电子安全。为了缓解这些问题，电磁波吸收材料被广泛应用于许多领域的。大多数电磁波吸收材料被广泛应用于室温。然而，高温潮湿环境的不利环境由于其微观结构恶化和电导率波动，通常导致微波吸收能力差，是其应用的严重障碍。因此，电磁波吸收材料的设计为在环境、高温甚至恶劣环境下保持显著的电磁波吸收性能。
目前，单吸收器阻抗匹配差，单损耗机制不能满足要求。为了扩大电磁波吸收材料的应用环境，二元/三元复合材料的构建在电磁波场中很受欢迎。复合材料的高温吸收性能仍需进一步提高，因此开发适合恶劣环境应用的新型电磁波吸收材料是非常必要的。
发明内容
本发明的目的是提出一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，利用二氧化硅层和氮化硅层结构来改善阻抗匹配特性，通过碳化硅纳米晶体来改善导电损耗，生成的纳米界面进一步促进电磁波的吸收性能；将Y2Si2O7颗粒在1400～1500℃下烧结形成珊瑚结构，形成多孔结构，有利于碳化硅层和氮化硅层在陶瓷孔隙和表面的沉积；碳化硅层包裹Y2Si2O7颗粒形成榴莲结构，经过1100～1200℃氧化形成二氧化硅层，颗粒增大，使榴莲结构变成菜花结构，有利于电导率的降低，导致阻抗匹配的改善。菜花结构明显增加了界面，颗粒的表面变得光滑，孔隙被填充形成一个连续的基体，密度明显增加。
本发明使用溶胶-凝胶法制备Y2Si2O7粉末，Y2Si2O7粉末压制成型后高温焙烧得到多孔Y2Si2O7陶瓷，采用碳化硅化学气相渗透技术沉积，得到SiC-Y2Si2O7复合陶瓷；SiC-Y2Si2O7复合陶瓷在温度为1100～1200℃下氧化处理2～3h，得到SiO2/SiC-Y2Si2O7复合陶瓷；SiO2/SiC-Y2Si2O7复合陶瓷经氮化硅化学气相渗透技术沉积得到Si3N4/SiO2/SiC基微波吸收陶瓷；Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷最外层为非晶态氮化硅层，中间层为二氧化硅层，碳化硅层位于内部，构建了具有逐渐阻抗匹配特征的结构。
一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，具体步骤如下：
(1)将Si(OC2H5)4溶解于乙醇中得到溶液A，Y(NO3)3·6H2O搅拌溶解于去离子水中得到溶液B；室温下，溶液A和溶液B搅拌混合得到凝胶C，凝胶C干燥得到干凝胶，干凝胶研磨成凝胶粉，凝胶粉进行冷压成型后置于温度为1400～1500℃的空气中烧结热处理2～3h，得到Y2Si2O7粉末；
(2)Y2Si2O7粉末经碳化硅化学气相渗透技术沉积，得到SiC-Y2Si2O7复合陶瓷；
(3)SiC-Y2Si2O7复合陶瓷经氧化处理，得到SiO2/SiC-Y2Si2O7复合陶瓷；
(4)SiO2/SiC-Y2Si2O7复合陶瓷经氮化硅化学气相渗透沉积，得到Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷。
所述步骤(1)凝胶C中Si元素与Y的摩尔比为1:1，凝胶C依次置于温度为70～100℃下干燥2～3h和温度为120～150℃下干燥2～3h；
所述步骤(2)碳化硅化学气相渗透的气源为CH3SiCl3，温度为1000～1100℃，压强为5～6kPa，H2为载气，Ar为稀释气，渗透沉积时间为80～85h；
所述步骤(3)氧化处理温度为1100～1200℃，处理时间为2～3h；
所述步骤(4)化学气相渗透沉积的气源为SiCl4和NH3，温度800～900℃，压强为5～6kPa，H2为载气，Ar为稀释气，渗透沉积时间为80～85h。
本发明的有益效果是：
(1)本发明采用化学渗透气相和氧化技术合成了具有菜花状结构的Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷，二氧化硅层和氮化硅层结构来改善阻抗匹配特性，碳化硅纳米晶体提高导电损耗，生成的纳米界面进一步促进了电磁波的吸收性能；
(2)本发明Si3N4/SiO2/SiC-Y2Si2O7陶瓷具有良好的相稳定性和耐水蒸汽腐蚀性能，可用于制备高达1500℃的温度下使用的环境屏障涂层；
(3)本发明方法操作过程简便，易于实施，适合于规模化工业生产应用。
附图说明
图1为实施例3纳米多孔Y2Si2O7陶瓷的SEM图；
图2为实施例3纳米SiC-Y2Si2O7复相陶瓷的SEM图；
图3为实施例3纳米SiO2/SiC-Y2Si2O7复相陶瓷的SEM图；
图4为实施例3纳米Si3N4/SiO2/SiC-Y2Si2O7复相陶瓷的SEM图；
图5为实施例3纳米Si3N4/SiO2/SiC-Y2Si2O7复相陶瓷的TEM图；
图6为实施例3纳米Si3N4/SiO2/SiC-Y2Si2O7复相陶瓷在100～600℃下的反射系数二维曲线。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明，但本发明的保护范围并不限于所述内容。
实施例1：一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，具体步骤如下：
(1)将Si(OC2H5)4搅拌溶解于乙醇中得到溶液A，Y(NO3)3·6H2O搅拌溶解于去离子水中得到溶液B；室温下，溶液A和溶液B搅拌混合得到凝胶C，其中凝胶C中Si元素与Y的摩尔比为1:1，凝胶C置于温度为80℃下干燥2h，再置于温度为130℃下干燥2h得到干凝胶，干凝胶放入玛瑙球磨罐中研磨2h形成凝胶粉，凝胶粉进行冷压成型后置于温度为1400℃的热空气中烧结热处理2h得到Y2Si2O7粉末；其中冷压成型的压强为8Mpa；
(2)Y2Si2O7经碳化硅化学气相渗透沉积，得到SiC-Y2Si2O7复合陶瓷；其中气源为CH3SiCl3，温度为1000℃，压强为5kPa，H2为载气，Ar为稀释气，渗透沉积时间为80h；
(3)SiC-Y2Si2O7复合陶瓷经氧化处理即得SiO2/SiC-Y2Si2O7微波吸收复合陶瓷；其中氧化处理温度为1100℃，氧化处理时间为2h；
(4)SiO2/SiC-Y2Si2O7复合陶瓷经氮化硅化学气相渗透沉积，得到Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷；其中化学气相渗透沉积的气源为SiCl4和NH3，温度800℃，压强为5kPa，H2为载气，Ar为稀释气，渗透沉积时间为80h；
本实施例Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷呈现多孔性质及颗粒状骨骼结构，Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷最外层为非晶态氮化硅层，中间层为二氧化硅层，碳化硅层位于内部，构建了具有逐渐阻抗匹配特征的结构。
实施例2：一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，具体步骤如下：
(1)将Si(OC2H5)4搅拌溶解于乙醇中得到溶液A，Y(NO3)3·6H2O搅拌溶解于去离子水中得到溶液B；室温下，溶液A和溶液B搅拌混合得到凝胶C，其中凝胶C中Si元素与Y的摩尔比为1:1，凝胶C置于温度为90℃下干燥2h，再置于温度为140℃下干燥2h得到干凝胶，干凝胶放入玛瑙球磨罐中研磨2h形成凝胶粉，凝胶粉进行冷压成型后置于温度为1500℃的热空气中烧结热处理2h得到Y2Si2O7粉末；其中冷压成型的压强为9Mpa；
(2)Y2Si2O7经碳化硅化学气相渗透沉积，得到SiC-Y2Si2O7复合陶瓷；其中气源为CH3SiCl3，温度为1100℃，压强为5kPa，H2为载气，Ar为稀释气，渗透沉积时间为82h；
(3)SiC-Y2Si2O7复合陶瓷经氧化处理即得SiO2/SiC-Y2Si2O7微波吸收复合陶瓷；其中氧化处理温度为1100℃，氧化处理时间为3h；
(4)SiO2/SiC-Y2Si2O7复合陶瓷经氮化硅化学气相渗透沉积，得到Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷；其中化学气相渗透沉积的气源为SiCl4和NH3，温度900℃，压强为6kPa，H2为载气，Ar为稀释气，渗透沉积时间为82h；
本实施例Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷呈现多孔性质及颗粒状骨骼结构，Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷最外层为非晶态氮化硅层，中间层为二氧化硅层，碳化硅层位于内部，构建了具有逐渐阻抗匹配特征的结构。
实施例3：一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，具体步骤如下：
(1)将Si(OC2H5)4搅拌溶解于乙醇中得到溶液A，Y(NO3)3·6H2O搅拌溶解于去离子水中得到溶液B；室温下，溶液A和溶液B搅拌混合得到凝胶C，其中凝胶C中Si元素与Y的摩尔比为1:1，凝胶C置于温度为100℃下干燥3h，再置于温度为150℃下干燥2h得到干凝胶，干凝胶放入玛瑙球磨罐中研磨2h形成凝胶粉，凝胶粉进行冷压成型后置于温度为1500℃的热空气中烧结热处理3h得到Y2Si2O7粉末；其中冷压成型的压强为10Mpa；
本实施例多孔Y2Si2O7陶瓷的SEM图见图1，从图中可以观察到陶瓷呈现多孔性质及颗粒状骨骼结构；
(2)Y2Si2O7经碳化硅化学气相渗透沉积，得到SiC-Y2Si2O7复合陶瓷；其中气源为CH3SiCl3，温度为1100℃，压强为6kPa，H2为载气，Ar为稀释气，渗透沉积时间为85h；
(3)SiC-Y2Si2O7复合陶瓷经氧化处理即得SiO2/SiC-Y2Si2O7微波吸收复合陶瓷；其中氧化处理温度为1200℃，氧化处理时间为3h；
(4)SiO2/SiC-Y2Si2O7复合陶瓷经氮化硅化学气相渗透沉积，得到Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷；其中化学气相渗透沉积的气源为SiCl4和NH3，温度900℃，压强为6kPa，H2为载气，Ar为稀释气，渗透沉积时间为85h；
本实施例SiC/Y2Si2O7复合陶瓷的SEM见图2，Y2Si2O7颗粒被碳化硅导电层覆盖，与Y2Si2O7相比，SiC/Y2Si2O7复合陶瓷只有少量的孔隙；纳米SiO2/SiC-Y2Si2O7复相陶瓷的SEM见图3，SiO2/SiC-Y2Si2O7复合陶瓷表面粗糙，多个SiC/Y2Si2O7颗粒通过二氧化硅绝缘层连接在一起，扩大整体陶瓷颗粒，形成花椰菜状结构，许多较小的孔隙转化为微米级的孔隙，在SiO2/SiC-Y2Si2O7复合陶瓷中形成裂纹；纳米Si3N4/SiO2/SiC-Y2Si2O7复相陶瓷的SEM见图4，最外层为非晶态氮化硅层，中间层为二氧化硅层，碳化硅层位于内部，构建了具有逐渐阻抗匹配特征的结构；
Si3N4/SiO2/SiC-Y2Si2O7复相陶瓷的TEM见图5，非晶态氮化硅层均匀地分布和包裹着Y2Si2O7纳米颗粒；纳米Si3N4/SiO2/SiC-Y2Si2O7复相陶瓷在100～600℃下的反射系数二维曲线见图6，复合陶瓷在25～300℃的温度范围内保持了稳定的电磁波吸收性能，RC<-20dB(有效吸收高达99％)。
以上对本发明的具体实施方式作了详细说明，但是本发明并不限于上述实施方式，在本领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下作出各种变化。

Claims (5)

1.一种以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，其特征在于，具体步骤如下：
(1)将Si(OC2H5)4溶解于乙醇中得到溶液A，Y(NO3)3·6H2O搅拌溶解于去离子水中得到溶液B；室温下，溶液A和溶液B搅拌混合得到凝胶C，凝胶C干燥得到干凝胶，干凝胶研磨成凝胶粉，凝胶粉进行冷压成型后置于温度为1400～1500℃的空气中烧结热处理2～3h，得到Y2Si2O7粉末；
(2)Y2Si2O7粉末经碳化硅化学气相渗透沉积，得到SiC-Y2Si2O7复合陶瓷；
(3)SiC-Y2Si2O7复合陶瓷经氧化处理得到SiO2/SiC-Y2Si2O7复合陶瓷；
(4)SiO2/SiC-Y2Si2O7复合陶瓷经氮化硅化学气相渗透沉积，得到Si3N4/SiO2/SiC-Y2Si2O7复合陶瓷。
2.根据权利要求1所述以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，其特征在于：步骤(1)凝胶C中Si元素与Y的摩尔比为1:1，凝胶C依次置于温度为70～100℃下干燥2～3h和温度为120～150℃下干燥2～3h。
3.根据权利要求1所述以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，其特征在于：步骤(2)化学气相渗透沉积的气源为CH3SiCl3，温度1000～1100℃，压强为5～6kPa，H2为载气，Ar为稀释气，渗透沉积时间为80～85h。
4.根据权利要求1所述以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，其特征在于：步骤(3)氧化处理的温度为1100～1200℃，处理时间为2～3h。
5.根据权利要求1所述以Y2Si2O7为基体的Si3N4/SiO2/SiC基微波吸收陶瓷的制备方法，其特征在于：步骤(4)化学气相渗透沉积的气源为SiCl4和NH3，温度800～900℃，压强为5～6kPa，H2为载气，Ar为稀释气，渗透沉积时间为80～85h。
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