CN108249914B - 一种石榴石结构铝酸盐微波介质陶瓷及其制备方法 - Google Patents

一种石榴石结构铝酸盐微波介质陶瓷及其制备方法 Download PDF

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CN108249914B
CN108249914B CN201810215562.6A CN201810215562A CN108249914B CN 108249914 B CN108249914 B CN 108249914B CN 201810215562 A CN201810215562 A CN 201810215562A CN 108249914 B CN108249914 B CN 108249914B
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余盛全
敬畏
尹文龙
胥涛
方攀
窦云巍
袁泽锐
陈莹
唐明静
康彬
张羽
谢靖
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Abstract

本发明公开了一种石榴石结构铝酸盐微波介质陶瓷，材料化学式组成为CaxY3‑xAl5‑xTixO12，其中x＝1.0～2.0。本发明还提供了所述石榴石结构铝酸盐微波介质陶瓷的制备方法。本发明的石榴石结构的铝酸陶瓷是一种新型的微波介质陶瓷材料，进一步丰富高性能铝酸盐微波介质陶瓷材料的种类。

Description

一种石榴石结构铝酸盐微波介质陶瓷及其制备方法
技术领域
本发明涉及一种介质陶瓷及其制备方法，具体涉及一种石榴石结构铝酸盐微波介质陶瓷及其制备方法，属于电子信息功能材料与器件技术领域。
背景技术
Al2O3陶瓷、尖晶石结构的MAl2O4(M＝Zn、Mg)陶瓷和钙钛矿结构的改性NdAlO3和LaAlO3陶瓷材料均已是重要的铝基微波介质陶瓷材料，而对于具有石榴石结构的铝酸盐陶瓷材料如Y3Al5O12(YAG)陶瓷，是否也能作为微波介质材料应用，还未有确切的研究报道。2009年，Kagomiya通过固相反应法制备了YAG陶瓷，在1650℃烧结24h获得的样品相对密度达99.6％，具有优异的微波介电性能：εr＝10.5，Q×f＝440000GHz，τf＝-50ppm/℃，Q×f值非常高，但τf值较大，制成微波器件后会导致器件温度稳定性差。因此，要将具有石榴石结构的YAG陶瓷开发成一种新的铝酸盐微波介质材料，首先必须将其大的负频率温度系数调控归零，并且同时保持其高Q×f值的优点。
为此提出了YAG陶瓷频率温度系数调零的思路：选择掺杂剂CaTiO3，通过Ca2+/Ti4+离子复合取代进入YAG晶格形成CaxY3-xAl5-xTixO12固溶体结构(0≤x≤3为Ca2+/Ti4+离子掺杂量)，改变晶格结构以调控石榴石结构CaxY3-xAl5-xTixO12固溶体陶瓷微波介电性能。CaTiO3陶瓷本身具有正频率温度系数τf＝+800ppm/℃，而且Ca2+和Ti4+等比列共掺杂能起到协同作用，分别取代Y3+和Al3+，即能保持电荷平衡而且不改变YAG晶格上的离子比列，所以在固溶进入YAG晶格后能够在调控频率温度系数归零的同时，维持改性后CaxY3-xAl5-xTixO12固溶体仍为纯石榴石晶格结构，没有新生杂相，具备获得高Q×f值潜力，是YAG陶瓷频率温度系数调零研究的一种较优新思路。Ca2+/Ti4+离子复合取代势必提高CaxY3-xAl5-xTixO12固溶体陶瓷的介电常数，因此石榴石结构的CaxY3-xAl5-xTixO12固溶体铝酸盐陶瓷将会是一种新中介电常数的微波介质陶瓷。
发明内容
本发明的目的在于提供一种以石榴石结构为主晶相的CaxY3-xAl5-xTixO12固溶体新型铝酸盐微波介质陶瓷材料，进一步丰富高性能铝酸盐微波介质陶瓷材料的种类。
本发明是这样实现的：
石榴石结构铝酸盐微波介质陶瓷，其材料化学式组成为CaxY3-xAl5-xTixO12，其中x＝1.0～2.0；所述的石榴石结构铝酸盐微波介质陶瓷经XRD物相分析为单一石榴石晶格结构，即为CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材料；石榴石结构铝酸盐微波介质陶瓷的介电常数为εr＝25.0～35.0，品质因数Q×f＝20000～45000GHz，频率温度系数为τf＝-20～+30ppm/℃。
本发明还提供了所述石榴石结构铝酸盐微波介质陶瓷的制备方法，具体包括如下步骤：
步骤1：配料。选择Y2O3、Al2O3、CaCO3、TiO2为原料，其纯度为99.9％，按照设计配方CaxY3-xAl5-xTixO12，其中x＝1.0～2.0称量原料。
步骤2：球磨。将步骤1备好的原料放入球磨罐中准备球磨，其中原料粉体、氧化铝磨球和无水乙醇的质量比为：1:5.7:1.6。在行星球磨机上以200r/min的转速球磨24小时。
步骤3：预烧。将经过步骤2球磨的浆料在80℃烘干，再过100目尼龙筛，然后在900℃预烧4小时。
步骤4：成型。将经过步骤3获得的预烧料粉体在20MPa压力下干压成型，获得陶瓷坯体Φ20mm*8mm。
步骤5：烧结。将步骤4所得陶瓷坯体在空气中的1500～1600℃烧结6h，即得到高质量的CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材料。
本发明提供了一种简单有效的石榴石结构铝酸盐微波介质陶瓷的制备方法。通过本发明固相反应法制备的CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材料的微波介电性能为：εr＝25.0～35.0，品质因数Q×f＝20000～45000GHz，频率温度系数为τf＝-20～+30ppm/℃，这是一种新中介电常数的铝酸盐微波介质陶瓷材料。本发明的石榴石结构的铝酸陶瓷是一种新型的微波介质陶瓷材料，进一步丰富高性能铝酸盐微波介质陶瓷材料的种类。
附图说明
图1为本发明提供的CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材料的XRD图。
具体实施方式
一种石榴石晶格结构固溶体铝酸盐微波介质陶瓷材料的化学式组成为CaxY3- xAl5-xTixO12(x＝1.0～2.0)；其制备过程中具体所用到的原料为Y2O3、Al2O3、CaCO3、TiO2，其纯度为99.9％；此新型微波介质陶瓷材料体经XRD物相分析为单一石榴石晶格结构，即为CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材料。此微波介质陶瓷在空气中于1500～1600℃烧结6h，所得介质陶瓷样品的介电常数为εr＝25.0～35.0，品质因数Q×f＝20000～45000GHz，频率温度系数为τf＝-20～+30ppm/℃。
具体实施例1～5
制得这些实施例CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材的具体实施步骤如下：
步骤1：配料。选择Y2O3、Al2O3、CaCO3、TiO2为原料，其纯度为99.9％，按照设计配方CaxY3-xAl5-xTixO12(x＝1.0～2.0)称量原料。
步骤2：球磨。将步骤1备好的原料放入球磨罐中准备球磨，其中原料粉体、氧化铝磨球和无水乙醇的质量比为：1:5.7:1.6。在行星球磨机上以200r/min的转速球磨24小时。
步骤3：预烧。将经过步骤2球磨的浆料在80℃烘干，再过100目尼龙筛，然后在900℃预烧4小时。
步骤4：成型。将经过步骤3获得的预烧料粉体在20MPa压力下干压成型，获得陶瓷坯体Φ20mm*8mm。
步骤5：烧结。将步骤4所得陶瓷坯体在空气中的1500～1600℃烧结6h，即得到高质量的CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材料。
步骤6：微波介电性能测试。将步骤5烧结得到的陶瓷样品在网络分析仪(AgilentTechnologies E5071C)上测试微波介电性能；频率温度系数由公式
Figure BDA0001598485630000041
计算所得，其中t1＝25℃、t2＝80℃，
Figure BDA0001598485630000042
分别为上述两个温度点对应的谐振频率。
实施例1～5所制备的CaxY3-xAl5-xTixO12固溶体铝酸盐陶瓷材料的微波介电性能测试结果如表1所示。
表1实施例1～5的样品化学组成、烧结温度、微波介电性能
Figure BDA0001598485630000051
尽管这里参照本发明的解释性实施例对本发明进行了描述，上述实施例仅为本发明较佳的实施方式，本发明的实施方式并不受上述实施例的限制，应该理解，本领域技术人员可以设计出很多其他的修改和实施方式，这些修改和实施方式将落在本申请公开的原则范围和精神之内。

Claims (4)

1.石榴石结构铝酸盐微波介质陶瓷，其特征在于：材料化学式组成为CaxY3-xAl5-xTixO12，其中x＝1.0～2.0；其制备方法包括如下步骤：
步骤1：配料；选择Y2O3、Al2O3、CaCO3、TiO2为原料，其纯度为99.9％，按照设计配方CaxY3- xAl5-xTixO12，其中x＝1.0～2.0称量原料；
步骤2：球磨；将步骤1备好的原料放入球磨罐中准备球磨，其中原料粉体、氧化铝磨球和无水乙醇的质量比为：1:5.7:1.6；在行星球磨机上以200r/min的转速球磨24小时；
步骤3：预烧；将经过步骤2球磨的浆料在80℃烘干，再过100目尼龙筛，然后在900℃预烧4小时；
步骤4：成型；将经过步骤3获得的预烧料粉体在20MPa压力下干压成型，
步骤5：烧结；将步骤4所得陶瓷坯体在空气中的1500～1600℃烧结6h，即得到高质量的CaxY3-xAl5-xTixO12固溶体铝酸盐微波介质陶瓷材料。
2.根据权利要求1所述石榴石结构铝酸盐微波介质陶瓷，其特征在于：
所述的石榴石结构铝酸盐微波介质陶瓷经XRD物相分析为单一石榴石晶格结构。
3.根据权利要求1或2所述石榴石结构铝酸盐微波介质陶瓷，其特征在于：
所述石榴石结构铝酸盐微波介质陶瓷的介电常数为εr＝25.0～35.0，品质因数Q×f＝20000～45000GHz，频率温度系数为τf＝-20～+30ppm/℃。
4.根据权利要求1所述石榴石结构铝酸盐微波介质陶瓷，其特征在于：
步骤4中，干压成型后获得陶瓷坯体Φ20mm*8mm。
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