CN108975913A - 一种ZnO-TiO2-Nb2O5基LTCC材料及其制备方法 - Google Patents
一种ZnO-TiO2-Nb2O5基LTCC材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 14
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 13
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 13
- 239000004615 ingredient Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 15
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
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- 238000000498 ball milling Methods 0.000 claims description 3
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Abstract
本发明属于电子陶瓷及其制造领域，涉及一种ZnO‑TiO2‑Nb2O5基低温共烧陶瓷(LTCC)材料及其制备方法。本发明将原料ZnO、TiO2、Nb2O5、B2O3和SiO2按比例直接配料预烧，制备方法相比现有技术减少了助剂的配制和预烧后的二次配料(简化了制备工艺)，且最终制得的ZnO‑TiO2‑Nb2O5基体系LTCC材料性能优于现有技术。
Description
技术领域
本发明属于电子陶瓷及其制造领域，涉及一种ZnO-TiO2-Nb2O5基低温共烧陶瓷(LTCC)材料及其制备方法。
背景技术
随着近几十年国内通信行业的不断高速发展，无线电移动通讯设备更新换代频繁，具有体积小型化、功能更强大、追求低成本的发展特点。低温共烧陶瓷(LowTemperature Co-fired Ceramic-LTCC)技术在多层陶瓷电路生产中发挥了关键作用，由于其工艺采用了叠层三维布局工艺设计，能够有效的降低各种通信射频器件的体积，从而在医疗，汽车制造和通信设备等领域广泛的应用。
LTCC材料要求与现今生产中所使用的Ag电极进行共烧，防止Ag电极由于温度过高而融化(Ag的熔点为961℃)。所以LTCC材料要求具有低的烧结温度(≤950℃)，此外，要求所使用的微波介电陶瓷在一定的相对介电常数(εr)下要求高品质因数(Q×f)，稳定性的谐振频率温度系数(τf)接近零。其中，相当于介电常数εr通常用来表征介质材料的介电性质或极化性质的物理参数，其值等于以预测材料为介质与以真空为介质制成的同尺寸电容器电容量之比；品质因素Q×f用来表示一个储能器件(如电感线圈、电容等)、谐振电路中所储能量同每周期损耗能量之比的一种质量指标；谐振频率温度系数τf表示为谐振频率对温度变化的灵敏度。在传统的固相反应方法制作电子陶瓷材料时，其烧结温度基本在1000℃以上，故不能满足LTCC工艺的生产要求。
目前对ZnO-TiO2-Nb2O5基陶瓷进行降低烧结温度的研究集中在向预烧后料加入烧结助剂，如CuO、Li2O-ZnO-B2O3、ZnO、BaO-CuO-B2O3等。从现有报道来看，该陶瓷基的温度能降至875～950℃，但最终陶瓷的介电常数εr较低(31)且τf值较大(-59ppm/℃)。
发明内容
针对上述存在问题或不足，为了解决ZnO-TiO2-Nb2O5基LTCC材料εr较低以及τf值较大的问题,本发明提供了一种ZnO-TiO2-Nb2O5基LTCC材料及其制备方法。该电子陶瓷材料能在低温下烧结致密同时保证了优良的微波介电性能。
该ZnO-TiO2-Nb2O5基LTCC材料，烧结温度875℃～950℃，烧结后的主晶相为Zn0.5Ti0.5NbO4相，次晶相为Zn0.15Nb0.3Ti0.55O2相，在875～900℃烧结时还存在ZnNb2O6相，在875～925℃烧结时还存在ZnB2O4相；介电常数23～40，损耗低至2.2×10-4，频率温度系数可达+10ppm/℃≤τf≤-10ppm/℃。
其原料为：ZnO、TiO2、Nb2O5、B2O3和SiO2的原始粉料按照下述化学通式配制(0.158+0.37x)ZnO-(0.55-0.05x)TiO2-(0.15+0.35x)Nb2O5-(0.006+0.02x)B2O3-(0.006+0.02x)SiO2(x＝0.4-0.6mol)，通过固相法制得。
其制备方法如下：
步骤1、将ZnO、TiO2、Nb2O5、B2O3和SiO2的原始粉料按照下述化学通式配制(0.158+0.37x)ZnO-(0.55-0.05x)TiO2-(0.15+0.35x)Nb2O5-(0.006+0.02x)B2O3-(0.006+0.02x)SiO2(x＝0.4-0.6mol)；
步骤2、将步骤1所得配料装入球磨罐，以锆球及去离子水作为研磨介质，按照配料：锆球：去离子水质量比1:6～7:3～5行星球磨4～8小时，然后在80～100℃烘干，以40～60目筛网过筛，最后在900～1100℃大气气氛中预烧3～6小时；
步骤3、将步骤2预烧后的粉料、放入球磨罐中进行二次球磨，以粉体：锆球：去离子水质量比1:4～7:2～3，行星球磨3～6小时，再取出烘干后，向得到的粉料加入丙烯酸溶液进行造粒；
步骤4、将步骤3造粒好的粉体压制成型后，排胶，然后升至875～950℃,并保温4～6小时，即可制得低温烧结微波介质陶瓷。
综上所述，本发明将原料ZnO、TiO2、Nb2O5、B2O3和SiO2按比例直接配料预烧，制备方法相比现有技术减少了助剂的配制和预烧后的二次配料(简化了制备工艺)，且最终制得的ZnO-TiO2-Nb2O5基体系LTCC材料性能优于现有技术。
附图说明
图1为x＝0.45mol时的收缩曲线图。
图2为x＝0.45mol，实施例1-6的XRD图。
图3为x＝0.45mol，实施例9的SEM图。
具体实施方式
下面结合附图和实施例对本发明做进一步的详细说明。
步骤1、将ZnO、TiO2、Nb2O5、B2O3和SiO2的原始粉料按照(0.158+0.37x)ZnO-(0.55-0.05x)TiO2-(0.15+0.35x)Nb2O5-(0.006+0.02x)B2O3-(0.006+0.02x)SiO2(x＝0.4-0.6mol)化学通式进行配料；
步骤2、将步骤1所得配料装入球磨罐，以锆球及去离子水作为研磨介质，按照配料：锆球：去离子水质量比1:6:4行星球磨6小时，然后在100℃烘干，以60目筛网过筛，最后在950℃、1050℃大气气氛中预烧4小时；
步骤3、将步骤2预烧后的粉料、放入球磨罐中进行二次球磨，以粉体：锆球：去离子水质量比1:5:2，行星球磨4小时，再取出烘干后，向得到的粉料加入丙烯酸溶液进行造粒；
步骤4、将步骤3造粒好的粉体放入φ15的模具中在20MPa压力下干压成型(尺寸为15mm×10mm的圆柱块体)，然后将圆柱块体在450℃下保温2小时以除去粘结剂，然后升至875～1000℃,下保温4小时，最终制得低温烧结微波介质陶瓷。
图1为x＝0.45mol时的收缩曲线图。从图中可以看出，样品大约在600℃左右开始收缩，随着温度的升高收缩增加，在1100℃左右时收缩可达到20％。
图2为实施例1～6的XRD衍射图样，从图中可以看出，陶瓷的主晶相为Zn0.5Ti0.5NbO4，与JCPDS卡片号48-0323匹配，次晶相为Zn0.15Nb0.3Ti0.55O2(JCPDS#79-1186)。在实施例1，2中存在少量ZnNb2O6相(卡片号JCPDS#37-1371)，实施例1～3中存在少量ZnB2O4相(JCPDS#39-1126)。在实施例4～6中，随着烧结温度的升高，ZnNb2O6相及ZnB2O4相消失。
图3为实施例9的SEM表面形貌图。从图中看出样品表面不致密，晶粒形状大小不一，并且晶粒尺寸较小。
各实施例的成分和微波介电性能如下表格
从上述表格数据可以看出，在预烧950℃，烧结875℃～1000℃之间，样品均取得优异性能，对于实施例1～6，样品的介电常数随烧结温度的提升而先增加后减小，在975℃烧结下(实施例5)取得最佳介电为40.10，此时样品的Q×f值达到24560GHz，但此时样品的τf值较大。综合考虑τf值，样品在实施例2时取得优异性能，此时烧结温度为900℃。在预烧1050℃，烧结900℃～1000℃之间，对于实施例7～11，样品的介电常数随温度从23.54增加至40.68，样品Q×f值从19636增加至20044GHz。在925℃烧结温度下(实施例8)取得综合最佳性能。
综合上述，本发明通过将ZnO、TiO2、Nb2O5、B2O3和SiO2按比例直接配料预烧，且最终制得的ZnO-TiO2-Nb2O5基体系LTCC材料性能优于现有技术。
Claims (2)
1.一种ZnO-TiO2-Nb2O5基LTCC材料，其特征在于：
烧结温度875℃～950℃，烧结后的主晶相为Zn0.5Ti0.5NbO4相，次晶相为Zn0.15Nb0.3Ti0.55O2相，在875～900℃烧结时还存在ZnNb2O6相，在875～925℃烧结时还存在ZnB2O4相；介电常数23～40，损耗低至2.2×10-4，频率温度系数可达+10ppm/℃≤τf≤-10ppm/℃；
其原料为：ZnO、TiO2、Nb2O5、B2O3和SiO2的原始粉料按照下述化学通式配制(0.158+0.37x)ZnO-(0.55-0.05x)TiO2-(0.15+0.35x)Nb2O5-(0.006+0.02x)B2O3-(0.006+0.02x)SiO2，x＝0.4-0.6mo l，通过固相法制得。
2.如权利要求1所述ZnO-TiO2-Nb2O5基LTCC材料的制备方法，具体步骤如下：
步骤1、将ZnO、TiO2、Nb2O5、B2O3和SiO2的原始粉料按照下述化学通式配制(0.158+0.37x)ZnO-(0.55-0.05x)TiO2-(0.15+0.35x)Nb2O5-(0.006+0.02x)B2O3-(0.006+0.02x)SiO2，x＝0.4-0.6mo l；
步骤2、将步骤1所得配料装入球磨罐，以锆球及去离子水作为研磨介质，按照配料：锆球：去离子水质量比1:6～7:3～5行星球磨4～8小时，然后在80～100℃烘干，以40～60目筛网过筛，最后在900～1100℃大气气氛中预烧3～6小时；
步骤3、将步骤2预烧后的粉料、放入球磨罐中进行二次球磨，以粉体：锆球：去离子水质量比1:4～7:2～3，行星球磨3～6小时，再取出烘干后，向得到的粉料加入丙烯酸溶液进行造粒；
步骤4、将步骤3造粒好的粉体压制成型后，排胶，然后升至875～950℃,并保温4～6小时，即可制得低温烧结微波介质陶瓷。
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| CN111233460A (zh) * | 2020-01-19 | 2020-06-05 | 深圳振华富电子有限公司 | 微波介质陶瓷材料及其制备方法 |
| CN111233460B (zh) * | 2020-01-19 | 2022-04-19 | 深圳振华富电子有限公司 | 微波介质陶瓷材料及其制备方法 |
| CN113087526A (zh) * | 2021-04-12 | 2021-07-09 | 中国振华集团云科电子有限公司 | 一种超薄大尺寸ltcc陶瓷基板的制备方法 |
| CN115353383A (zh) * | 2022-10-21 | 2022-11-18 | 云南银峰新材料有限公司 | 一种低温烧结的微波介质陶瓷材料及其制备方法 |
| CN115353383B (zh) * | 2022-10-21 | 2023-01-20 | 云南银峰新材料有限公司 | 一种低温烧结的微波介质陶瓷材料及其制备方法 |
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