CN108774062A - 一种中介电常数微波介质陶瓷材料、制备方法及应用 - Google Patents
一种中介电常数微波介质陶瓷材料、制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种中介电常数微波介质陶瓷材料、制备方法及应用,化学式为Mg2NdTiO5.5。本发明以MgO、Nd2O3、TiO2作为原料,利用固相反应制备出微波介质陶瓷Mg2NdTiO5.5,最终提供了具有中介电常数及较高品质因数的微波介质陶瓷材料,该陶瓷材料的煅烧温区为900~1300℃,烧结温区为1400℃~1550℃,介电常数为24~27,品质因数为7658~15579GHz,性能稳定,能够应用于制造微波元件。本发明的制备工艺操作简单,制备工艺流程可靠、容易实现材料的稳定生产;烧结时的可选参数范围较大且可调控,容错率和良品率较高,大大降低了次品率和总体制造成本,适合工业化生产和大力推广。
Description
技术领域
本发明涉及一种陶瓷材料及其制备方法,具体是一种中介电常数微波介质陶瓷材料、制备方法及应用,属于电子信息材料与元器件领域。
背景技术
微波介质陶瓷是应用于微波技术领域的一类电介质陶瓷。随着移动通信、雷达、卫星定位系统等微波技术的迅速发展,微波器件的小型化、集成化、频率高端化以及低成本化已成为微波技术发展的必然趋势。在微波电路中,传统的金属谐振器的体积和重量较大,难以满足微波器件的发展要求,而微波介质陶瓷具有低微波损耗和稳定的谐振频率温度系数等特点,且可制作成各种微波器件,如介质谐振器、滤波器等。
在微波介质陶瓷中,中介电常数微波介质陶瓷主要用于现代雷达和微波通信技术。目前,中介电常数微波介质陶瓷的研究体系主要有BaO-TiO2系列、ZrO2-SnO-TiO2系列、复合钙钛矿系列以及A2+B5+ 2O6系列。随着信息化程度的提高,新材料体系的开发越来越受到人们重视,尤其是为了满足更高的使用要求,对中介电常数、高品质因数的微波介质陶瓷材料的需求逐渐增加。
此外,目前的微波介质陶瓷材料的制备过程较为繁琐,对工艺要求极为严格,一旦制取过程出现偏差会导致产品报废,直接提升了制造成本。
发明内容
针对上述现有技术存在的问题,本发明的目的是提供一种的中介电常数微波介质陶瓷材料及其制备方法,制得的微波介质陶瓷材料具有中介电常数且品质因数较高,且制备工艺流程可靠,操作简单,容错率较高,可以降低制造成本、适合工业化生产和推广,本发明的另一目的在于提供一种中介电常数微波介质陶瓷材料的应用。
为实现上述目的,本发明采用的技术方案是:一种中介电常数微波介质陶瓷材料,化学式为Mg2NdTiO5.5。
本发明还提供了一种中介电常数微波介质陶瓷材料的制备方法,包括以下步骤:
(1)按化学计量式Mg2NdTiO5.5中各元素的质量比称量化学原料MgO、Nd2O3、TiO2;
(2)将步骤(1)配置好的化学原料放入球磨罐中混合,加入无水乙醇作为球磨介质,球磨6小时;
(3)将步骤(2)球磨后的原料置于干燥箱中于100℃烘干,烘干后的粉料过40目筛;
(4)将步骤(3)过筛后所得的粉料置于坩埚中,在900~1300℃进行煅烧4小时;
(5)对步骤(4)煅烧好的粉料进行处理,放入球磨机中,加入无水乙醇作为球磨介质,球磨12小时;
(6)将步骤(5)球磨后的原料置于干燥箱中于100℃烘干,烘干后的粉料过80目筛;
(7)在步骤(6)烘干后的粉料中外加入石蜡,置于电阻炉上翻炒均匀,过80目筛;
(8)将步骤(7)过筛后的粉料在200MPa的压强下压制成为坯体;
(9)将步骤(8)的坯体于1400~1500℃烧结,升温速率为5℃/分钟,保温4小时,制成中介电常数微波介质陶瓷材料。
优选的,所述步骤(8)得到的坯体为圆柱形,尺寸为:直径d=10mm、高度h=5mm。
作为一个优选的方案,所述步骤(7)中加入的石蜡重量占物质总量的8~10%。
作为另一个优选的方案,所述步骤(2)中,球磨罐中的原料:无水乙醇:锆球的质量比为1:1:1.5;所述步骤(5)中,球磨罐中的粉料:无水乙醇:锆球的质量比为1:1:1.5。
利用本发明的中介电常数微波介质陶瓷材料Mg2NdTiO5.5可以制造小型微波元件。
相对于现有技术,本发明具有如下优势:
(1)本发明以MgO、Nd2O3、TiO2作为原料,利用固相反应制备出微波介质陶瓷Mg2NdTiO5.5,最终提供了具有中介电常数的微波介质陶瓷材料;制得的微波介质陶瓷材料介电常数εr在24~27,且Q×f为7658~15579GHz,品质因数较高,性能稳定,能够应用于制造微波元件;
(2)本发明的制备工艺操作简单,制备工艺流程可靠、容易实现材料的稳定生产;烧结时的煅烧温区为900~1300℃,烧结温区为1400℃~1550℃,可选参数范围较大且可调控,即使因为设备的原因出现温度偏差也能够成功制得产品,容错率和良品率较高,大大降低了次品率和总体制造成本,适合工业化生产和大力推广;
(3)本发明采用的原材料供应充足,价格低廉,使高性能微波陶瓷的低成本化成为可能。
附图说明
图1是按本发明实施例1技术方案制备的陶瓷样品的X射线衍射图谱;
图2是按本发明实施例1技术方案制备的陶瓷样品的扫描电镜图谱。
具体实施方式
下面结合实施例对本发明作进一步详细说明。
实施例1
根据化学式Mg2NdTiO5.5中各元素的化学计量比,分别称量MgO(分析纯)4.9040g、Nd2O3(分析纯)10.2364g、TiO2(分析纯)4.8596g;将称量好的粉料按Nd2O3、TiO2、MgO顺序放入球磨罐中,以去离子水为球磨介质,球磨混合6小时;球磨后的原料经干燥、过筛之后,放入氧化铝坩埚中,利用马弗炉加热至1300℃煅烧4小时;将煅烧后的粉料再次球磨12小时,干燥、过筛,加入石蜡炒均、过80目筛;将适量的粉料倒入模具中,利用粉末压片机在200MPa的压强下制成φ10mm×5mm的圆柱样品;最后将样品放入高温箱式炉中进行烧结,烧结温度为1450℃烧结,升温速率为5℃/分钟,保温4小时,制成Mg2NdTiO5.5微波介质陶瓷。最后,将上述微波介质陶瓷材料用网络分析仪测试其微波介电性能。
参见附图1,它是按本实施例技术方案制备的陶瓷样品的X射线衍射图谱,从图中可以看出,所制备样品的物相组成呈两相共存状态,分别是NdTiO3和MgO结构,其中NdTiO3属于正交晶系,Pbnm空间群。
参见附图2,它是按本实施例技术方案制备的陶瓷样品的扫描电镜图谱,从图中可以看出,样品烧结良好,晶界平直,无明显气孔。
经过上述方法制得的材料介电常数为26.15,品质因数Q×f=15241GHz,谐振频率温度系数为-40.7ppm/℃。
实施例2-15的制备过程与实施例1类似,不同的是预烧温度和烧结温度,如表1所示:
表1各实施例的预烧温度和烧结温度
No | 预烧温度(℃) | 烧结温度(℃) |
实施例1 | 1300 | 1450 |
实施例2 | 1300 | 1400 |
实施例3 | 1300 | 1425 |
实施例4 | 1300 | 1475 |
实施例5 | 1300 | 1500 |
实施例6 | 1100 | 1400 |
实施例7 | 1100 | 1425 |
实施例8 | 1100 | 1450 |
实施例9 | 1100 | 1475 |
实施例10 | 1100 | 1500 |
实施例11 | 900 | 1400 |
实施例12 | 900 | 1425 |
实施例13 | 900 | 1450 |
实施例14 | 900 | 1475 |
实施例15 | 900 | 1500 |
各实施例制备的微波介质陶瓷材料的性能如表2所示:
表2各实施例的微波介电性能
Claims (6)
1.一种中介电常数微波介质陶瓷材料,其特征在于,化学式为Mg2NdTiO5.5。
2.根据权利要求1所述的中介电常数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)按化学计量式Mg2NdTiO5.5中各元素的质量比称量化学原料MgO、Nd2O3、TiO2;
(2)将步骤(1)配置好的化学原料放入球磨罐中混合,加入无水乙醇作为球磨介质,球磨6小时;
(3)将步骤(2)球磨后的原料置于干燥箱中于100℃烘干,烘干后的粉料过40目筛;
(4)将步骤(3)过筛后所得的粉料置于坩埚中,在900~1300℃进行煅烧4小时;
(5)对步骤(4)煅烧好的粉料进行处理,放入球磨机中,加入无水乙醇作为球磨介质,球磨12小时;
(6)将步骤(5)球磨后的原料置于干燥箱中于100℃烘干,烘干后的粉料过80目筛;
(7)在步骤(6)烘干后的粉料中外加入石蜡,置于电阻炉上翻炒均匀,过80目筛;
(8)将步骤(7)过筛后的粉料在200MPa的压强下压制成为坯体;
(9)将步骤(8)的坯体于1400~1500℃烧结,升温速率为5℃/分钟,保温4小时,制成中介电常数微波介质陶瓷材料。
3.根据权利要求2所述的中介电常数微波介质陶瓷材料的制备方法,其特征在于,所述步骤(8)得到的坯体为圆柱形,尺寸为:直径d=10mm、高度h=5mm。
4.根据权利要求2所述的中介电常数微波介质陶瓷材料的制备方法,其特征在于,所述步骤(7)中加入的石蜡重量占物质总量的8~10%。
5.根据权利要求2所述的中介电常数微波介质陶瓷材料的制备方法,其特征在于,所述步骤(2)中,球磨罐中的原料:无水乙醇:锆球的质量比为1:1:1.5;所述步骤(5)中,球磨罐中的粉料:无水乙醇:锆球的质量比为1:1:1.5。
6.一种根据权利要求1所述的中介电常数微波介质陶瓷材料的应用,其特征在于,利用Mg2NdTiO5.5制造小型微波元件。
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