CN108069711A - 一种Nb2O5掺杂0.95MgTiO3-0.05CaTiO3陶瓷 - Google Patents

一种Nb2O5掺杂0.95MgTiO3-0.05CaTiO3陶瓷 Download PDF

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CN108069711A
CN108069711A CN201710789844.2A CN201710789844A CN108069711A CN 108069711 A CN108069711 A CN 108069711A CN 201710789844 A CN201710789844 A CN 201710789844A CN 108069711 A CN108069711 A CN 108069711A
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李蔚
韩蕊
傅文平
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East China University of Science and Technology
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Abstract

本发明公开一种Nb2O5掺杂0.95MgTiO3‑0.05CaTiO3（95MCT）陶瓷。其特点是：首先以CaCO3和TiO2为原料合成CaTiO3粉体，以MgCO3和TiO2为原料合成MgTiO3粉体。将两种粉体以0.95molMgTiO3和0.05molCaTiO3的比例混合，再加上二者总量0.4‑1.0wt%的Nb2O粉，一起球磨混和后，干压成型制得素坯，将素坯放入电炉中，1350‑1450℃烧结2‑4h，即可得致密的Nb2O掺杂95MCT陶瓷。这种95MCT陶瓷具有优良的微波介电性能，其介电常数为19.89‑20.01，介电损耗tanδ为（1.04‑1.37）×10‑4，温度系数τ f 为3.32‑5.53 ppm/℃。本发明工艺简单，生产流程短，适合规模化生产。

Description

一种Nb2O5掺杂0.95MgTiO3-0.05CaTiO3陶瓷
技术领域
本发明涉及一种Nb2O5掺杂0.95MgTiO3-0.05CaTiO3陶瓷，属于低介电损耗的微波介质材料领域，可用于微波通讯等领域。
背景技术
MgTiO3陶瓷具有适中的介电常数(εr≈17)，低介电损耗(Q×f ≈160,000GHz)和负的温度系数(τ f ≈-50ppm/ oC)，在与具有较大正温度系数的CaTiO3陶瓷（εr≈170，τ f ≈ +850ppm/ oC)以95：5（摩尔比）的比例复合后，所得0.95MgTiO3-0.05CaTiO3陶瓷（95MCT）的介电常数有所提高(εr≈20)，温度系数较小(τ f 接近于0ppm/ oC)，且介电损耗仍然很低(Q×f≈56000GHz)，是一种性能优异的微波介质材料，同时原料来源丰富，成本低廉，因此可广泛应用在GPS天线、谐振器、介质滤波器等微波通讯领域。近年来，为了进一步改善95MCT陶瓷的性能，人们对其进行了多种掺杂改性工作。例如Cheng-Liang Huang等人在95MCT陶瓷中添加1wt%的ZnO，在1300oC下烧结，可获得优良的介电性能：εr=20，Q×f=6,5000GHz，τ f =-5.8ppm/ oC（测试频率7GHz）。Keshri等人通过以Co和La分别对95MCT陶瓷中Mg和Ca进行取代掺杂，使其微波介电性能进一步提高：εr=25.85，Q×f =80,040 GHz，τ f =0 ppm/ oC（测试频率8.05GHz）。但是，通过单掺Nb2O5来提高95MCT陶瓷介电性能的做法则未见报道。
发明内容
本发明目的在于提供一种Nb2O5掺杂95MCT陶瓷，目的在于降低95MCT的介电损耗，进一步改善其介电性能。
为了实现上述发明目的，本发明采用的技术方案如下：
一、以CaCO3和TiO2为原料（摩尔比为1:1），经湿法球磨 （12-24h）干燥后得到混合料，将混合料置于电炉中于1100-1200℃下煅烧2-5h，自然冷却后即可得到CaTiO3粉体；以MgCO3和TiO2为原料（摩尔比为1.05:1），经湿法球磨 （12-24h）干燥后得到混合料，将混合料置于电炉中于1050-1150℃下煅烧2-5h，自然冷却后即可得到MgTiO3粉体。
优选的，CaTiO3粉体的煅烧温度为1150oC，保温时间为3h，升温速度为2℃/min。MgTiO3粉体的煅烧温度为1100℃，保温时间为3h，升温速度为2 oC/min。
二、将MgTiO3和CaTiO3两种粉体以一定比例置于球磨罐中，再加入一定量的Nb2O粉，加入去离子水和氧化锆球，球磨一段时间后取出，烘干，干压成型。
上述工艺过程的参数为：MgTiO3和CaTiO3两种粉体的比例为0.95：0.05（摩尔比），Nb2O粉的掺杂量为MgTiO3和CaTiO3两种粉体总量的0.4-1.0wt%。球磨时的料：水：球=1：2：3，球磨时间为24h，烘干温度为100-150℃,干压成型压力为80-120MPa。
三、将压制好的样品放置于电炉中，升温至一定温度，保温一段时间后自然冷却，即获得致密的Nb2O掺杂95MCT陶瓷。
上述工艺过程的参数为：电炉的升温速率为2-4℃/min，烧结温度为1350-1450℃，保温2-4h。
按上述方式制备的Nb2O掺杂95MCT陶瓷具有优良的微波介电性能，其介电常数为19.89-20.01，介电损耗tanδ为（1.04-1.37）×10-4，温度系数τ f 为3.32-5.53 ppm/℃（测试频率7.2GHz）。典型地，当Nb2O掺杂量为0.6wt%时，介电损耗tanδ为1.04×10-4，比未掺杂的95MCT的介电损耗（tanδ=1.44×10-4）下降约30%；温度系数τ f 为4.42 ppm/℃，比未掺杂的的95MCT的温度系数τ f （7.00 ppm/℃）更接近于零。
本发明选用Nb2O掺杂来调节改善95MCT陶瓷的介电性能，降低其介电损耗，其操作方法简单，生产流程短，生产成本降低，适合大规模生产。
具体实施方式
实施例1：一种纯95MCT陶瓷，它是通过以下方法制备而成的：
（1）以CaCO3和TiO2为原料（摩尔比为1:1），经湿法球磨24h，干燥后置于电炉中于1150℃下煅烧3h，冷却后，得到CaTiO3粉体；以MgCO3和TiO2为原料（摩尔比为1.05:1），经湿法球磨 24h，干燥后置于电炉中于1100℃下煅烧3h，冷却后，得到MgTiO3粉体;
（2）将两种粉体以0.95molMgTiO3加0.05molCaTiO3的比例加入到球磨罐中，加入去离子水和氧化锆球（料：水：球=1：2：3），球磨24h后取出在120℃下烘24h，得到95MCT粉体;
（3）将所得95MCT粉体在100MPa压力下干压成型，在1400℃下烧结3h，自然冷却后即获得致密的95MCT陶瓷;
（4）利用Hakii-Coleman法来测量样品的介电性能，其介电常数εr=20.09，tanδ=1.44×10-4，τ f =7.00 ppm/℃（测试频率7.2GHz）。
实施例2：一种Nb2O5掺杂95MCT陶瓷，它是通过以下方法制备而成的：
（1）以CaCO3和TiO2为原料（摩尔比为1:1），经湿法球磨24h，干燥后置于电炉中于1150℃下煅烧3h，冷却后，得到CaTiO3粉体；以MgCO3和TiO2为原料（摩尔比为1.05:1），经湿法球磨 24h，干燥后置于电炉中于1100℃下煅烧3h，冷却后，得到MgTiO3粉体;
（2）将MgTiO3和CaTiO3两种粉体（摩尔比0.95：0.05）放入四个球磨罐中，再分别加入为MgTiO3和CaTiO3两种粉体总量的0.4wt%、0.6wt%、0.8wt%、1.0wt%的Nb2O5粉，加入去离子水和氧化锆球（料：水：球=1：2：3），球磨24h后取出在120℃下烘24h，得到不同量Nb2O5掺杂的95MCT粉体;
（3）将所得Nb2O5掺杂95MCT粉体在100MPa压力下干压成型，在1400℃下烧结3h，自然冷却后即获得致密的Nb2O5掺杂95MCT陶瓷;
（4）利用Hakii-Coleman法来测量样品的介电性能，随着Nb2O5掺杂量的增加，样品的其介电常数εr分别为20.01、19.96、19.92、19.89；tanδ分别为1.37×10-4、1.04×10-4、1.29×10-4、1.31×10-4；τ f 分别为5.53 ppm/℃、4.42ppm/℃、6.26 ppm/℃、3.32 ppm/℃（测试频率7.2GHz）。典型地，当Nb2O掺杂量为0.6wt%时，介电损耗比未掺杂的95MCT的介电损耗下降约30%，温度系数比未掺杂的95MCT的温度系数更接近于零。

Claims (7)

1.一种Nb2O5掺杂0.95MgTiO3-0.05CaTiO3（95MCT）陶瓷，其特征在于：
（1）以CaCO3和TiO2为原料,经湿法球磨、干燥后置于电炉中煅烧一段时间获得的CaTiO3粉体；
（2）以MgCO3和TiO2为原料,经湿法球磨、干燥后置于电炉中煅烧一段时间获得的MgTiO3粉体；
（3）将两种粉体以一定比例混合，再和一定量的Nb2O粉置于球磨罐中，加入去离子水和氧化锆球，球磨一段时间后取出，烘干，干压成型；
（4）将压制好的样品放置于电炉中，升温至一定温度，保温一段时间后自然冷却，即获得致密的Nb2O掺杂95MCT陶瓷。
2.根据权利要求1所述一种Nb2O5掺杂95MCT陶瓷，其特征在于：步骤（1）中，CaCO3和TiO2的配比为1:1（摩尔比），球磨混合时间为12-24h，煅烧温度为1100-1200℃，保温时间为2-5h。
3.根据权利要求1所述一种Nb2O5掺杂95MCT陶瓷，其特征在于：步骤（2）中，MgCO3和TiO2的配比为1.05:1（摩尔比），球磨混合时间为12-24h，煅烧温度为1050-1150℃，保温时间为2-5h。
4.根据权利要求1所述一种Nb2O5掺杂95MCT陶瓷，其特征在于：步骤（3）中， MgTiO3和CaTiO3的比例为0.95：0.05（摩尔比），Nb2O粉的掺杂量为MgTiO3和CaTiO3粉体总量的0.4-1.0wt%；球磨时的料：水：球=1：2：3，球磨时间为24h，烘干温度为100-150℃,干压成型压力为80-120MPa。
5.根据权利要求1所述一种Nb2O5掺杂95MCT陶瓷，其特征在于：步骤（4）中，升温速率为2-4℃/min，烧结温度为1350-1450℃，保温2-4h。
6.根据权利要求1、2、3、4、5所述一种Nb2O5掺杂95MCT陶瓷，其特征在于:按上述方式制备的Nb2O掺杂95MCT陶瓷具有优良的微波介电性能，其介电常数为19.89-20.01，介电损耗tanδ为（1.04-1.37）×10-4，温度系数τ f 为3.32-5.53 ppm/℃。
7.典型地，当Nb2O掺杂量为0.6wt%时，介电损耗tanδ为1.04×10-4，比未掺杂的95MCT的介电损耗（tanδ=1.44×10-4）下降约30%；温度系数τ f 为4.42 ppm/℃，比未掺杂的95MCT的温度系数τ f （7.00 ppm/℃）更接近于零。
CN201710789844.2A 2017-09-05 2017-09-05 一种Nb2O5掺杂0.95MgTiO3-0.05CaTiO3陶瓷 Pending CN108069711A (zh)

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CN111548148A (zh) * 2020-06-05 2020-08-18 陕西华星电子开发有限公司 一种微波介质瓷料、制备方法以及用途
CN111606722A (zh) * 2020-05-21 2020-09-01 苏州瑞玛精密工业股份有限公司 一种制备介质滤波器陶瓷制品用的注射成型粘结剂及其应用
CN111763083A (zh) * 2020-06-15 2020-10-13 苏州瑞玛精密工业股份有限公司 一种低温烧结型超低损耗微波介电陶瓷及其制备方法和应用
CN113755165A (zh) * 2020-11-04 2021-12-07 湖南工商大学 一种锰掺杂95MCT:Yb,Ho上转换发光-介电双功能材料及其制备方法
CN115304367A (zh) * 2022-07-21 2022-11-08 苏州市职业大学 一种微波介电陶瓷的制备方法和产品

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111606722A (zh) * 2020-05-21 2020-09-01 苏州瑞玛精密工业股份有限公司 一种制备介质滤波器陶瓷制品用的注射成型粘结剂及其应用
CN111606722B (zh) * 2020-05-21 2022-07-05 苏州瑞玛精密工业股份有限公司 一种制备介质滤波器陶瓷制品用的注射成型粘结剂及其应用
CN111548148A (zh) * 2020-06-05 2020-08-18 陕西华星电子开发有限公司 一种微波介质瓷料、制备方法以及用途
CN111763083A (zh) * 2020-06-15 2020-10-13 苏州瑞玛精密工业股份有限公司 一种低温烧结型超低损耗微波介电陶瓷及其制备方法和应用
CN111763083B (zh) * 2020-06-15 2022-07-05 苏州瑞玛精密工业股份有限公司 一种低温烧结型超低损耗微波介电陶瓷及其制备方法和应用
CN113755165A (zh) * 2020-11-04 2021-12-07 湖南工商大学 一种锰掺杂95MCT:Yb,Ho上转换发光-介电双功能材料及其制备方法
CN113755165B (zh) * 2020-11-04 2023-06-02 湖南工商大学 一种锰掺杂95MCT:Yb,Ho上转换发光-介电双功能材料及其制备方法
CN115304367A (zh) * 2022-07-21 2022-11-08 苏州市职业大学 一种微波介电陶瓷的制备方法和产品
CN115304367B (zh) * 2022-07-21 2023-03-28 苏州市职业大学 一种微波介电陶瓷的制备方法和产品

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Application publication date: 20180525