CN112979314A - 一种中等介电常数高q微波介质陶瓷材料及其制备方法 - Google Patents
一种中等介电常数高q微波介质陶瓷材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了属于电子功能材料与器件技术领域的一种中等介电常数高Q微波介质陶瓷材料及其制备方法。所述陶瓷材料由BaO、SrO、La2O3、TiO2和Al2O3构成,其重量百分比为:0.1%~3.0%BaO、0.1%~8.0%SrO、59%~74%La2O3、21%~30%TiO2、0.1%~7.0%Al2O3;所述陶瓷材料的介电常数为39.2~48.6、Q×f值为51600~89900GHz、谐振频率温度系数为‑0.8~‑30.3ppm/℃。与介电常数相近的微波介质陶瓷材料相比,本发明所述微波介质陶瓷材料具有更高的Q×f值和近零的谐振频率温度系数,有望用于制作介质谐振器、介质滤波器和微波电容器等高性能微波器件。
Description
技术领域
本发明属于电子功能材料与器件技术领域,特别涉及一种中等介电常数高Q微波介质陶瓷材料及其制备方法。
背景技术
微波介质陶瓷是应用于微波频段电路中作为介质材料完成一种或多种功能的陶瓷材料,因为其损耗低、温度稳定性好的特点,在现代通信中被用作谐振器、滤波器、介质天线等微波器件。随着移动通信技术向高频化的发展,对微波器件的性能要求越来越高,要求微波介质陶瓷具有极低的损耗、良好的温度稳定性和较高的介电常数。随着移动通信基站装备对高性能滤波器和电容器的微小型化和高频率选择性的需求,基站用滤波器和电容器要求微波介质陶瓷材料具有更高的介电常数和极低的介质损耗,目前可用于基站的介质滤波器和微波电容器的中等介电常数(40左右)、谐振频率温度系数近零的微波介质陶瓷的Q×f值一般在50000GHz以下,不能满足新一代移动通信基站用介质滤波器和微波电容器的要求,开发一种具有中等介电常数、更高Q微波介质陶瓷材料具有重要的实际意义。
发明内容
为了解决上述问题,本发明提出了一种中等介电常数高Q微波介质陶瓷材料,所述陶瓷材料由BaO、SrO、La2O3和TiO2构成或由BaO、SrO、La2O3、TiO2和Al2O3构成,其重量百分比为:0.1%~3.0%BaO、0.1%~8.0%SrO、59%~74%La2O3、21%~30%TiO2、0.1%~7.0%Al2O3;所述陶瓷材料的介电常数为39.2~48.6、Q×f值为51600~89900GHz、谐振频率温度系数为-0.8~-30.3ppm/℃。
一种中等介电常数高Q微波介质陶瓷材料的制备方法,包括以下步骤:
1)按权利要求1所述百分比称取原料粉体,加入酒精作为球磨介质,混合行星球磨得到浆料;球磨过程的球料比为10:1,球磨时间为8小时以上,转速为300转每分钟;所述二氧化钛为金红石相;
2)将混合均匀的浆料干燥并过80目筛,进行预烧,合成一种具有六方钙钛矿结构的化合物;
3)步骤2)得到的化合物进行二次行星球磨,球磨时间4小时以上,球料比为10:1,转速为300转每分钟;
4)步骤3)得到的粉体经干燥,过80目筛后,加入聚乙烯醇水溶液PVA,研磨造粒,并通过干压成型,得到生坯;
5)对生坯进行排胶和烧结处理。
所述步骤2)中的预烧温度范围为1400~1450℃,预烧时间为2-4小时。
所述步骤4)中生坯的压制压力为100~200兆帕,施加压力方式为轴向压力。
所述步骤5)中的生坯的排胶温度为600℃,排胶时长为4小时,烧结温度为1500~1650℃,烧结时间为4~8小时。
所述步骤1)原料包括碳酸钡、碳酸锶、氧化镧、二氧化钛或氧化铝。
所述步骤1)酒精加入量与原料粉体的质量比为2:1。
所述步骤4)聚乙烯醇水溶液的质量分数为5%,每10g粉体加入2.5mL聚乙烯醇水溶液。
本发明的有益效果:
1.本申请所述陶瓷材料与现有主流的中等介电常数微波介质陶瓷以及六方钙钛矿结构化合物相比,采用了不同比例的TiO2、La2O3和Al2O3掺杂,能够有效调控陶瓷的微波介电性能,使其满足不同的应用场景。
2.在由BaO、SrO、La2O3和TiO2构成的陶瓷材料中掺杂TiO2后,TiO2以第二相的形式存在,其介电常数为105,Q×f值48300GHz,谐振频率温度系数为+410ppm/℃,能够在不大幅降低陶瓷Q×f值的情况下将陶瓷的谐振频率温度系数调至近零。
在由BaO、SrO、La2O3、TiO2和Al2O3构成的陶瓷材料中掺杂La2O3和Al2O3后,La2O3和Al2O3在陶瓷中以固溶体的形式存在,La3+取代晶体结构中的Ba2+和Sr2+,Al3+取代晶体结构中的Ti4+,这种取代使陶瓷的晶格常数减小,六方钙钛矿结构中A位离子和B位离子与O2-的键长减小,离子间结合力增强,晶体结构更加稳定,降低了陶瓷中氧空位等缺陷浓度,降低陶瓷的介电损耗,提高了陶瓷的Q×f值。不同的掺杂都能保证陶瓷材料的介电常数介于39.2~48.6时,使其Q×f值在51600GHz以上,并且具有近零的谐振频率温度系数。
3.本发明设计了一种新型的陶瓷材料成分,具有优秀的微波介电性能;能用于制作介质谐振器、介质滤波器和微波电容器等高性能微波器件。
附图说明
图1为实施例1陶瓷的表面显微形貌图;
图2为实施例1陶瓷的X-射线衍射(XRD)谱图;
图3为实施例2陶瓷的表面显微形貌图。
具体实施方式
以下结合附图和具体实施例对本发明作进一步的详细说明:
下面实施例中如无特殊说明,所述试剂和材料,均可从商业途径获得。
实施例1
1)按照质量分数2.1%BaO、5.7%SrO、63.5%La2O3、27.5%TiO2、1.2%Al2O3的配比,称量碳酸钡、碳酸锶、氧化镧、二氧化钛(金红石相)、氧化铝,加入合适含量的酒精,进行行星球磨8小时;
2)将浆料烘干,过筛后在1450℃条件下预烧4小时;
3)将得到的粉体再球磨4小时,烘干过筛后,加入适量的聚乙烯醇水溶液(PVA),研磨造粒,并通过干压成型。
4)最后将生坯在600℃下排胶4小时,再在1600℃下烧结4小时,即得到所需化学成分比例的陶瓷材料。
陶瓷的SEM表面形貌如图1所示,可知陶瓷的致密度较高,孔隙较少,其体积密度为6.1g/cm3,平均晶粒尺寸为3μm。陶瓷的XRD谱图如图2所示,陶瓷的主要物相结构为六方钙钛矿相,没有明显的第二相存在。用网络分析仪测得介电常数为43.9,Q×f值为84300GHz,谐振频率的温度系数为-18.0ppm/℃。
实施例2
1)按照质量分数2.9%BaO、7.7%SrO、60.8%La2O3、22.3%TiO2、6.3%Al2O3的配比,称量碳酸钡、碳酸锶、氧化镧、二氧化钛(金红石相)、氧化铝,加入合适含量的酒精,进行行星球磨8小时;
2)将浆料烘干,过筛后在1450℃条件下预烧4小时;
3)将得到的粉体再球磨4小时,烘干过筛后,加入适量的聚乙烯醇水溶液(PVA),研磨造粒,并通过干压成型。
4)最后将生坯在600℃下排胶4小时,再在1650℃下烧结4小时,即得到所需化学成分比例的陶瓷材料。
陶瓷的SEM表面形貌如图3所示,可知陶瓷的致密度较高,孔隙较少,其体积密度为6.1g/cm3。用网络分析仪测得介电常数为39.2,Q×f值为89900GHz,谐振频率的温度系数为-25.7ppm/℃。
实施例3
1)按照质量分数2.8%BaO、7.6%SrO、59.6%La2O3、30.0%TiO2的配比,称量碳酸钡、碳酸锶、氧化镧、二氧化钛(金红石相),加入合适含量的酒精,进行行星球磨8小时;
2)将浆料烘干,过筛后在1450℃条件下预烧4小时;
3)将得到的粉体再球磨4小时,烘干过筛后,加入适量的聚乙烯醇水溶液(PVA),研磨造粒,并通过干压成型。
4)最后将生坯在600℃下排胶4小时,再在1600℃下烧结4小时,即得到所需化学成分比例的陶瓷材料。
陶瓷的体积密度为6.0g/cm3。用网络分析仪测得介电常数为48.1,Q×f值为51600GHz,谐振频率的温度系数为-0.8ppm/℃。
Claims (8)
1.一种中等介电常数高Q微波介质陶瓷材料,其特征在于,所述陶瓷材料由BaO、SrO、La2O3和TiO2构成或由BaO、SrO、La2O3、TiO2和Al2O3构成,其重量百分比为:0.1%~3.0%BaO、0.1%~8.0%SrO、59%~74%La2O3、21%~30%TiO2、0.1%~7.0%Al2O3;所述陶瓷材料的介电常数为39.2~48.6、Q×f值为51600~89900GHz、谐振频率温度系数为-0.8~-30.3ppm/℃。
2.一种权利要求1所述中等介电常数高Q微波介质陶瓷材料的制备方法,其特征在于,包括以下步骤:
1)按权利要求1所述百分比称取原料粉体,加入酒精作为球磨介质,混合行星球磨得到浆料;球磨过程的球料比为10:1,球磨时间为8小时以上,转速为300转每分钟;
2)将混合均匀的浆料干燥并过80目筛,进行预烧,合成一种具有六方钙钛矿结构的化合物;
3)步骤2)得到的化合物进行二次行星球磨,球磨时间4小时以上,球料比为10:1,转速为300转每分钟;
4)步骤3)得到的粉体经干燥,过80目筛后,加入聚乙烯醇水溶液,研磨造粒,并通过干压成型,得到生坯;
5)对生坯进行排胶和烧结处理。
3.根据权利要求2所述中等介电常数高Q微波介质陶瓷材料的制备方法,其特征在于,所述步骤2)中的预烧温度范围为1400~1450℃,预烧时间为2-4小时。
4.根据权利要求2所述中等介电常数高Q微波介质陶瓷材料的制备方法,其特征在于,所述步骤4)中生坯的压制压力为100~200兆帕,施加压力方式为轴向压力。
5.根据按照权利要求2所述中等介电常数高Q微波介质陶瓷材料的制备方法,其特征在于,所述步骤5)中的生坯的排胶温度为600℃,排胶时长为4小时,烧结温度为1500~1650℃,烧结时间为4~8小时。
6.根据按照权利要求2所述中等介电常数高Q微波介质陶瓷材料的制备方法,其特征在于,所述步骤1)原料包括碳酸钡、碳酸锶、氧化镧、二氧化钛或氧化铝。
7.根据按照权利要求2所述中等介电常数高Q微波介质陶瓷材料的制备方法,其特征在于,所述步骤1)酒精加入量与原料粉体的质量比为2:1。
8.根据按照权利要求2所述中等介电常数高Q微波介质陶瓷材料的制备方法,其特征在于,所述步骤4)聚乙烯醇水溶液的浓度为质量分数5%,每10g粉体加入2.5mL聚乙烯醇水溶液。
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