CN106565241A - 一种高性能铌酸镧系微波介质陶瓷 - Google Patents

一种高性能铌酸镧系微波介质陶瓷 Download PDF

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CN106565241A
CN106565241A CN201610974029.9A CN201610974029A CN106565241A CN 106565241 A CN106565241 A CN 106565241A CN 201610974029 A CN201610974029 A CN 201610974029A CN 106565241 A CN106565241 A CN 106565241A
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肖谧
顾青青
周子淇
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Abstract

本发明公开了一种高性能铌酸镧系微波介质陶瓷,其组成为(La1‑xSmx)NbO4(0﹤x≤0.1)。先将La2O3,Nb2O5,Sm2O3按(La1‑xSmx)NbO4(0﹤x≤0.1)进行配料,经过磨球、干燥、过筛,于1100℃预烧;再经二次球磨、干燥后外加8%重量百分比粘合剂进行造粒,压制成型为坯体,坯体于1275‑1375℃烧结,制得高性能铌酸镧系介质陶瓷。本发明成功地获得了Q×f达到60000Ghz左右、介电常数约为20左右,谐振频率温度系数近0ppm/℃的高性能微波陶瓷介质。本发明制备工艺简单,过程无污染,是一种很有前途的毫米波电路的微波介质材料。

Description

一种高性能铌酸镧系微波介质陶瓷
技术领域
本发明属于一种以成分为特征的陶瓷组合物,特别涉及一种新型高性能铌酸镧系微波介质陶瓷及其制备方法。
背景技术
现代移动通信的迅速发展,推动着各类微波移动通信终端设备向小型化、轻量化、多功能化及低成本化的方向快速发展。微波介电陶瓷对于制造更小的器件和提高微波集成电路的封装密度非常有效。用于制作介质谐振器等基础和关键材料的介质陶瓷,须满足以下条件:较高的相对介电常数(εr)以提高集成度,较低介电损耗(介电损耗正切角tanδ)以提高工作频率,趋近于零的谐振频率温度系数(τf)以提高温度稳定性。
LaNbO4是一种具有优越微波介电性能的新型的微波介质材料,其介电常数约为20,谐振频率温度系数为10ppm/℃,烧结温度为1325℃,但其Q×f值较低,为50000左右。本发明采用传统固相法,制备出温度稳定性更好,品质因数更高的(La1-xSmx)NbO4微波介质陶瓷,其Q×f值高达60000Ghz,谐振频率温度系数接近于0ppm/℃,烧结温度为1325℃,可在毫米波电路中获得应用。
发明内容
本发明的目的,是以La2O3,Nb2O5,Sm2O3为主要原料,制备出一种具有优越微波介电性能的新型铌酸镧系微波介质陶瓷:(La1-xSmx)NbO4微波介质陶瓷,其中0﹤x≤0.1。
本发明通过如下技术方案予以实现,具有以下步骤:
(1)将La2O3,Nb2O5,Sm2O3原料,按化学式(La1-xSmx)NbO4,其中0﹤x≤0.1进行配料,将粉料放入球磨罐中,加入分散剂,加入氧化锆球,在球磨机上球磨6~10小时;
(2)将步骤⑴球磨后的原料置于110℃温度条件下烘干,待样品原料干燥后,过筛,获得颗粒均匀的粉料;
(3)将步骤⑵混合均匀的粉料于1050℃~1125℃预烧3小时;
(4)在步骤⑶预烧后的陶瓷粉料放入球磨罐中,加入去离子水和氧化锆球,在球磨机上球磨6~10小时;烘干后在陶瓷粉料中外加8%重量百分比的粘合剂进行造粒,过80目筛,再用粉末压片机成型为坯体;
(5)将在步骤⑷的坯体于1325℃烧结,保温4~6小时,制得高性能铌酸镧系微波介质陶瓷。
所述步骤(1)的La2O3,Nb2O5,Sm2O3原料的质量纯度大于99.9%。
所述步骤(3)预烧温度为1100℃。
所述步骤(1)、步骤(4)球磨工艺的原料、去离子水与磨球的质量比为1:16:15。
所述步骤(4)的坯体直径为10mm,厚度为5mm。
所述步骤(5)的烧结温度为1325℃,保温时间4小时。
本发明以LaNbO4微波介质陶瓷为基础,用Sm离子对La离子进行一定含量的取代,成功地获得了微波介电性能较高的微波介质陶瓷:Q×f达到60000Ghz左右、介电常数约为20左右,谐振频率温度系数近0ppm/℃。本发明的制备工艺简单,过程无污染,微波介电性能优异,是一种很有前途的毫米波电路微波介质材料。
具体实施方式
本发明采用纯度大于99.9%的化学原料La2O3,Nb2O5,Sm2O3,制备(La1-xSmx)NbO4(0﹤x≤0.1)微波介质陶瓷。具体实施例如下。
对比实施例
1.依照微波介质陶瓷组分LaNbO4,称La2O3-13.7678g、Nb2O5-11.2322g配料,共25g;混合粉料加入球磨罐中,加入160ml去离子水和150g锆球后,在行星式球磨机上球磨6小时,球磨机转速为1000转/分;
2.将球磨后的原料置于110℃温度条件下烘干,过40目筛,获得颗粒均匀的粉料;
3.将颗粒均匀的粉料于1100℃煅烧3小时;
4.将煅烧后的粉料放入球磨罐中,加入去离子水和氧化锆球,二次球磨6小时,出料后在110℃温度条件下烘干,过40目筛;然后加入8%重量百分比的的粘合剂作进行造粒,并过80目筛;再用粉末压片机以8Mpa的压力压成直径为10mm,厚度为5mm的坯体;
5.将坯体于1325℃烧结,保温4小时,制得高性能铌酸镧系微波介质陶瓷;
最后,通过网络分析仪及相关测试夹具测试所得样品微波特性。
实施例1
1.依照微波介质陶瓷组分(La1-xSmx)NbO4(x=0.02),称La2O3-13.4819g、Nb2O5-11.2236g、Sm2O3-0.2945g配料,共25g;混合粉料加入球磨罐中,加入160ml去离子水和150g锆球后,在行星式球磨机上球磨6小时,球磨机转速为1000转/分;
2.将球磨后的原料置于110℃温度条件下烘干,过40目筛,获得颗粒均匀的粉料;
3.将颗粒均匀的粉料于1100℃煅烧3小时;
4.将煅烧后的粉料放入球磨罐中,加入去离子水和氧化锆球,二次球磨6小时,出料后在110℃温度条件下烘干,过40目筛;然后加入8%重量百分比的粘合剂作进行造粒,并过80目筛;再用粉末压片机以8Mpa的压力压成直径为10mm,厚度为5mm的坯体;
5.将坯体于1325℃烧结,保温4小时,制得高性能铌酸镧系微波介质陶瓷;
最后,通过网络分析仪及相关测试夹具测试所得样品微波特性。
实施例2
1.依照微波介质陶瓷组分(La1-xSmx)NbO4(x=0.04),称La2O3-13.1965g、Nb2O5-11.2149g、Sm2O3-0.5885g配料,共25g;混合粉料加入球磨罐中,加入160ml去离子水和150g锆球后,在行星式球磨机上球磨6小时,球磨机转速为1000转/分;
2.将球磨后的原料置于110℃温度条件下烘干,过40目筛,获得颗粒均匀的粉料;
3.将颗粒均匀的粉料于1100℃煅烧3小时;
4.将煅烧后的粉料放入球磨罐中,加入去离子水和氧化锆球,二次球磨6小时,出料后在110℃温度条件下烘干,过40目筛;然后加入8%重量百分比的粘合剂作进行造粒,并过80目筛;再用粉末压片机以8Mpa的压力压成直径为10mm,厚度为5mm的坯体;
5.将坯体于1325℃烧结,保温4小时,制得高性能铌酸镧系微波介质陶瓷;
最后,通过网络分析仪及相关测试夹具测试所得样品微波特性。
实施例3
1.依照微波介质陶瓷组分(La1-xSmx)NbO4(x=0.06),称La2O3-12.9116g、Nb2O5-11.2063g、Sm2O3-0.8821g配料,共25g;混合粉料加入球磨罐中,加入160ml去离子水和150g锆球后,在行星式球磨机上球磨6小时,球磨机转速为1000转/分;
2.将球磨后的原料置于110℃温度条件下烘干,过40目筛,获得颗粒均匀的粉料;
3.将颗粒均匀的粉料于1100℃煅烧3小时;
4.将煅烧后的粉料放入球磨罐中,加入去离子水和氧化锆球,二次球磨6小时,出料后在110℃温度条件下烘干,过40目筛;然后加入8%重量百分比的粘合剂作进行造粒,并过80目筛;再用粉末压片机以8Mpa的压力压成直径为10mm,厚度为5mm的坯体;
5.将坯体于1325℃烧结,保温4小时,制得高性能铌酸镧系微波介质陶瓷;
最后,通过网络分析仪及相关测试夹具测试所得样品微波特性。
实施例4
1.依照微波介质陶瓷组分(La1-xSmx)NbO4(x=0.08),称La2O3-12.6272g、Nb2O5-11.1976g、Sm2O3-1.1752g配料,共25g;混合粉料加入球磨罐中,加入160ml去离子水和150g锆球后,在行星式球磨机上球磨6小时,球磨机转速为1000转/分;
2.将球磨后的原料置于110℃温度条件下烘干,过40目筛,获得颗粒均匀的粉料;
3.将颗粒均匀的粉料于1100℃煅烧3小时;
4.将煅烧后的粉料放入球磨罐中,加入去离子水和氧化锆球,二次球磨6小时,出料后在110℃温度条件下烘干,过40目筛;然后加入8%重量百分比的粘合剂作进行造粒,并过80目筛;再用粉末压片机以8Mpa的压力压成直径为10mm,厚度为5mm的坯体;
5.将坯体于1325℃烧结,保温4小时,制得高性能铌酸镧系微波介质陶瓷;
最后,通过网络分析仪及相关测试夹具测试所得样品微波特性。
实施例5
1.依照微波介质陶瓷组分(La1-xSmx)NbO4(x=0.1),称La2O3-12.3431g、Nb2O5-11.1890g、Sm2O3-1.4679g配料,共25g;混合粉料加入球磨罐中,加入160ml去离子水和150g锆球后,在行星式球磨机上球磨6小时,球磨机转速为1000转/分;
2.将球磨后的原料置于110℃温度条件下烘干,过40目筛,获得颗粒均匀的粉料;
3.将颗粒均匀的粉料于1100℃煅烧3小时;
4.将煅烧后的粉料放入球磨罐中,加入去离子水和氧化锆球,二次球磨6小时,出料后在110℃温度条件下烘干,过40目筛;然后加入8%重量百分比的粘合剂作进行造粒,并过80目筛;再用粉末压片机以8Mpa的压力压成直径为10mm,厚度为5mm的坯体;
5.将坯体于1325℃烧结,保温4小时,制得高性能铌酸镧系微波介质陶瓷;
最后,通过网络分析仪及相关测试夹具测试所得样品微波特性。
本发明具体实施例的检测方法如下:
1.借助Agilent 8720ES网络分析仪,采用开始抢平行板法测量所制备圆柱形陶瓷材料的节电常数,将测试夹具放入ESPEC MC-710F型高低温循环温箱进行谐振频率温度系数的测量,温度范围为25-85℃测试频率在6-15GHz范围内。
2.采用闭式腔法测量所制备圆柱形陶瓷样品的品质因数。
本发明具体实施例的各项关键参数及介电性能检测结果详见表1。
表1

Claims (7)

1.一种高性能铌酸镧系微波介质陶瓷,其组成为(La1-xSmx)NbO4,其中0﹤x≤0.1。
上述高性能铌酸镧系微波陶瓷的制备方法,具有以下步骤:
(1)将La2O3,Nb2O5,Sm2O3原料,按化学式(La1-xSmx)NbO4,其中0﹤x≤0.1进行配料,将粉料放入球磨罐中,加入去离子水,加入氧化锆球,在球磨机上球磨6~10小时;
(2)将步骤⑴球磨后的原料置于110℃温度条件下烘干,待原料干燥后,过筛,获得颗粒均匀的粉料;
(3)将步骤⑵混合均匀的粉料于1050℃~1125℃预烧3小时;
(4)在步骤⑶预烧后的陶瓷粉料放入球磨罐中,加入去离子水和氧化锆球,在球磨机上二次球磨6~10小时,并于110℃温度条件下烘干;烘干后在陶瓷粉料中外加8%重量百分比的粘合剂进行造粒,过80目筛,再用粉末压片机成型为坯体;
(5)将在步骤⑷的坯体于1275-1375℃烧结,保温4~6小时,制得高性能铌酸镧系微波介质陶瓷。
2.根据权利要求1的一种高性能铌酸镧系微波介质陶瓷,其特征在于,所述步骤(1)的La2O3,Nb2O5,Sm2O3原料的质量纯度大于99.9%。
3.根据权利要求1的一种高性能铌酸镧系微波介质陶瓷,其特征在于,所述步骤(3)预烧温度为1100℃。
4.根据权利要求1的一种新型的高性能铌酸镧系微波介质陶瓷,其特征在于,所述步骤(1)、步骤(4)球磨工艺的原料、去离子水与磨球的质量比为1:16:15。
5.根据权利要求1的一种新型的高性能铌酸镧系微波介质陶瓷,其特征在于,所述步骤(4)的粉末压片机的压力为8Mpa。
6.根据权利要求1的一种新型的高性能铌酸镧系微波介质陶瓷,其特征在于,所述步骤(4)的坯体直径为10mm,厚度为5mm。
7.根据权利要求1的一种新型的高性能铌酸镧系微波介质陶瓷,其特征在于,所述步骤(5)的烧结温度1325℃,保温时间4小时。
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