CN114180939B - 一种低介、低损耗硼化物ltcc材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种低介、低损耗硼化物LTCC材料及其制备方法，该硼化物LTCC材料的化学表达式为ABB5O9，其中A=Li、Na；B=Sr、Ba、Ca。该硼化物LTCC材料制备工艺依次如下：水热法制备ABB5O9粉末、球磨、压制成型、烧结成瓷。本发明制备得到的ABB5O9基LTCC材料的主晶相为ABB5O9（A=Li、Na；B=Sr、Ba、Ca）单相，具有原料成本低、烧结温度低（700~825℃）、介电常数低（4.3~8.5、Qf值较高（10500~58850GHz）、制备工艺简单、重现性好等优点，且可以解决高频通讯中微波信号的时延问题，提高微波信号传输的稳定性，非常适合用作LTCC微波基板。
Description
技术领域
本发明属于微波介质陶瓷领域，尤其涉及一种低介、低损耗硼化物LTCC材料及其制备方法。
背景技术
在微波元器件向小型化、集成化、毫米波化方向发展的情况下和LTCC等电子封装技术的要求下，对微波介质陶瓷材料的性能要求日益提高。目前，市面上商用微波介质陶瓷材料大多都有着较高的烧结温度，需要通过添加烧结助剂来降低烧结温度，但是这又会损害材料的微波介电性能。因此，开发固有本征低烧温度同时兼具优良微波介电性能的低介微波介质材料，对于拓展LTCC微波介质陶瓷材料体系有着非常重要的意义。
目前，具有低烧结温度的低介电常数微波介质陶瓷材料体系的研究主要有玻璃陶瓷、钼酸盐基陶瓷、磷酸盐基陶瓷、钒酸盐基陶瓷、钨酸盐基陶瓷和硼酸盐基陶瓷等。玻璃陶瓷，顾名思义其存在玻璃相。而在毫米波这样高频工作条件下，玻璃相的存在会导致介电损耗增加，不是最佳的LTCC材料选择；而钼酸盐、钨酸盐容易与电极材料发生反应，同时有些材料的谐振频率温度系数τ f 值过大，无法满足LTCC技术的要求；磷酸盐对环境有害，也非理想的LTCC材料选项。相比之下，硼酸盐基陶瓷的开发较少。一般的，由于硼离子B3+的极化率非常低，硼酸盐基陶瓷的相对介电常数也较低 ，介电损耗较小，且与大部分金属电极材料不发生反应。由此可见，硼酸盐体系微波介质陶瓷材料非常具有探索价值。
本发明公开了一种低介、低损耗三元硼化物（ABB5O9）基LTCC材料，该化合物成瓷温度低于950℃，且介电损耗较低，非常适合用作微波介质基板。
发明内容
本发明的目的在于克服低温烧结陶瓷原材料成本较高、对环境有害及易于电极发生反应的问题，提供一种低介、低损耗硼化物LTCC材料及其制备方法，该材料的主晶相为ABB5O9（A=Li、Na；B=Sr、Ba、Ca），具有低成本、低烧结温度、低介电常数、低介电损耗、制备工艺稳定等优点。
为解决现有技术问题，本发明公开了一种低介、低损耗硼化物LTCC材料，该化合物的化学表达式为ABB5O9，其中A=Li、Na；B=Sr、Ba、Ca。
所述的一种低介、低损耗硼化物LTCC材料，其特征在于：晶相具有单斜系结构，其物相在烧结致密化温度范围内稳定存在。
本发明还公开了一种低介、低损耗硼化物LTCC材料的制备方法，其特征在于包括如下步骤：
步骤一、水热法制备ABB5O9粉末：以SrCO3、BaCO3、、CaCO3、NaNO3、LiNO3、和H3BO3高纯粉末为原料，按照化学表达式为ABB5O9进行称量配料形成混合粉末，将混合粉末溶解在去离子水中，制备得到质量浓度为10 %的混合溶液；随后在混合溶液中加入无水乙醇和硅烷偶联剂，其中无水乙醇占总混合溶液体积的30%，硅烷偶联剂占总混合溶液体积的10%；将混合溶液转移至高压反应釜内，逐步升温至120~150℃反应12~24h，冷却至室温，利用去离子水和无水乙醇循环离心洗涤三次，在90℃下烘干4h即可得到ABB5O9粉末。
步骤二、球磨：将水热法制备所得ABB5O9粉末置于行星式球磨机中进行湿磨，球磨介质为无水乙醇，磨球材质为二氧化锆，混合料、磨球与无水乙醇的质量比为1：5：1.2，球磨时间8~12小时，球磨机转速为250~350 rpm；
步骤三、压制成型：将球磨料浆烘干后，加入其重量5～8 wt%的浓度为5 wt%的聚乙烯醇水溶液过筛、造粒；在单向压力机上，以100～150 MPa的压力压成坯体；
步骤四、烧结成瓷：将压坯置于箱式电阻炉中升温经先缓慢升温至500℃，保温2小时，再升温至650℃，保温2小时，再升温至700~825℃，保温6~8小时，最后随炉冷却，即得到低介、低损耗硼化物LTCC材料。
本发明具有的有益效果：
（1）本发明通过水热法合成单相ABB5O9粉末，解决了传统固相法难以合成纯硼化物陶瓷相的难题，该方法制备过程清洁环保，通过调整水热温度和时间即可控制单相粉末的结晶度，在低温下即可合成单相粉末，制备方法稳定，具有较高的商业化价值。
（2）本发明制备得到的ABB5O9（A=Li、Na；B=Sr、Ba、Ca）基LTCC材料的烧结温度为700~825℃，介电常数为4.3~8.5，Qf值为10500~58850GHz，可以解决高频通讯中微波信号的时延问题，提高微波信号传输的稳定性，非常适合用作LTCC微波基板。
附图说明
图1是本发明实施例三制得NaSrB5O9陶瓷的XRD图谱。
图2是本发明实施例三制得NaSrB5O9陶瓷的SEM图。
具体实施方式
下面对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
表1是5种成分配方的混合料末。采用不同的工艺参数将其制备成低介、低损耗硼化物LTCC材料，并分别测定其微波介电性能。
表1 五种成分配方的混合料末（mol%）
实施例一
步骤一、水热法制备ABB5O9粉末：以SrCO3、BaCO3、、CaCO3、NaNO3、LiNO3、和H3BO3高纯粉末为原料，按照化学表达式为ABB5O9进行称量配料形成混合粉末，将混合粉末溶解在去离子水中，制备得到质量浓度为10 %的混合溶液；随后在混合溶液中加入无水乙醇和硅烷偶联剂，其中无水乙醇占总混合溶液体积的30%，硅烷偶联剂占总混合溶液体积的10%；将混合溶液转移至高压反应釜内，逐步升温至120℃反应24h，冷却至室温，利用去离子水和无水乙醇循环离心洗涤三次，在90℃下烘干4h即可得到ABB5O9粉末。
步骤二、球磨：将水热法制备所得ABB5O9粉末置于行星式球磨机中进行湿磨，球磨介质为无水乙醇，磨球材质为二氧化锆，混合料、磨球与无水乙醇的质量比为1：5：1.2，球磨时间8小时，球磨机转速为350 rpm；
步骤三、压制成型：将球磨料浆烘干后，加入其重量5 wt%的浓度为5 wt%的聚乙烯醇水溶液过筛、造粒；在单向压力机上，以100 MPa的压力压成坯体；
步骤四、烧结成瓷：将压坯置于箱式电阻炉中升温经先缓慢升温至500℃，保温2小时，再升温至650℃，保温2小时，再升温至700℃，保温8小时，最后随炉冷却，即得到低介、低损耗硼化物LTCC材料。
对本实施例获得的材料进行性能检测，检测结果如表2所示。
表2 采用实施例一制备出不同材料的介电性能
实施例二
步骤一、水热法制备ABB5O9粉末：以SrCO3、BaCO3、、CaCO3、NaNO3、LiNO3、和H3BO3高纯粉末为原料，按照化学表达式为ABB5O9进行称量配料形成混合粉末，将混合粉末溶解在去离子水中，制备得到质量浓度为10 %的混合溶液；随后在混合溶液中加入无水乙醇和硅烷偶联剂，其中无水乙醇占总混合溶液体积的30%，硅烷偶联剂占总混合溶液体积的10%；将混合溶液转移至高压反应釜内，逐步升温至150℃反应12h，冷却至室温，利用去离子水和无水乙醇循环离心洗涤三次，在90℃下烘干4h即可得到ABB5O9粉末。
步骤二、球磨：将水热法制备所得ABB5O9粉末置于行星式球磨机中进行湿磨，球磨介质为无水乙醇，磨球材质为二氧化锆，混合料、磨球与无水乙醇的质量比为1：5：1.2，球磨时间12小时，球磨机转速为250 rpm；
步骤三、压制成型：将球磨料浆烘干后，加入其重量8 wt%的浓度为5 wt%的聚乙烯醇水溶液过筛、造粒；在单向压力机上，以150 MPa的压力压成坯体；
步骤四、烧结成瓷：将压坯置于箱式电阻炉中升温经先缓慢升温至500℃，保温2小时，再升温至650℃，保温2小时，再升温至825℃，保温6小时，最后随炉冷却，即得到低介、低损耗硼化物LTCC材料。
对本实施例获得的材料进行性能检测，检测结果如表3所示。
表3 采用实施例二制备出不同材料的介电性能
实施例三
步骤一、水热法制备ABB5O9粉末：以SrCO3、BaCO3、、CaCO3、NaNO3、LiNO3、和H3BO3高纯粉末为原料，按照化学表达式为ABB5O9进行称量配料形成混合粉末，将混合粉末溶解在去离子水中，制备得到质量浓度为10 %的混合溶液；随后在混合溶液中加入无水乙醇和硅烷偶联剂，其中无水乙醇占总混合溶液体积的30%，硅烷偶联剂占总混合溶液体积的10%；将混合溶液转移至高压反应釜内，逐步升温至130℃反应18h，冷却至室温，利用去离子水和无水乙醇循环离心洗涤三次，在90℃下烘干4h即可得到ABB5O9粉末。
步骤二、球磨：将水热法制备所得ABB5O9粉末置于行星式球磨机中进行湿磨，球磨介质为无水乙醇，磨球材质为二氧化锆，混合料、磨球与无水乙醇的质量比为1：5：1.2，球磨时间10小时，球磨机转速为300 rpm；
步骤三、压制成型：将球磨料浆烘干后，加入其重量6 wt%的浓度为5 wt%的聚乙烯醇水溶液过筛、造粒；在单向压力机上，以125 MPa的压力压成坯体；
步骤四、烧结成瓷：将压坯置于箱式电阻炉中升温经先缓慢升温至500℃，保温2小时，再升温至650℃，保温2小时，再升温至800℃，保温7小时，最后随炉冷却，即得到低介、低损耗硼化物LTCC材料。
对本实施例获得的材料进行性能检测，检测结果如表4所示。
表4 采用实施例三制备出不同材料的介电性能
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变形，这些改进和变形也应视为本发明的保护范围。
Claims (4)
1.一种低介、低损耗硼化物LTCC材料，其特征在于，该硼化物的化学表达式为ABB5O9，其中A=Li、Na；B=Sr、Ba、Ca；
该低介、低损耗硼化物LTCC材料的制备方法，包括如下步骤：
步骤一、水热法制备ABB5O9粉末：以SrCO3、BaCO3、CaCO3、NaNO3、LiNO3、和H3BO3高纯粉末为原料，通过水热法制备得到ABB5O9单相粉末；
步骤二、球磨：将水热法制备所得ABB5O9粉末置于行星式球磨机中进行湿磨，球磨介质为无水乙醇，磨球材质为二氧化锆，混合料、磨球与无水乙醇的质量比为1：5：1.2，球磨时间8~12小时，球磨机转速为250~350 rpm；
步骤三、压制成型：将球磨料浆烘干后，加入其重量5～8 wt%的浓度为5 wt%的聚乙烯醇水溶液过筛、造粒；在单向压力机上，以100～150 MPa的压力压成坯体；
步骤四、烧结成瓷：将压坯置于箱式电阻炉中升温经先缓慢升温至500℃，保温2小时，再升温至650℃，保温2小时，再升温至700~825℃，保温6~8小时，最后随炉冷却，即得到低介、低损耗硼化物LTCC材料。
2.一种如权利要求1所述的一种低介、低损耗硼化物LTCC材料的制备方法，其特征在于，步骤一中SrCO3、BaCO3、CaCO3、NaNO3、LiNO3和H3BO3粉末的粒度为1~5μm，纯度≥99.5%。
3.根据权利要求2所述的一种低介、低损耗硼化物LTCC材料的制备方法，其特征在于步骤一中水热法制备ABB5O9粉末的具体方法为：将SrCO3、BaCO3、CaCO3、NaNO3、LiNO3、和H3BO3原料粉末按照化学表达式为ABB5O9（A=Li、Na；B=Sr、Ba、Ca）进行称量配料形成混合粉末，将混合粉末溶解在去离子水中，随后在混合溶液中加入无水乙醇和硅烷偶联剂搅拌形成浊液，将浊液转移至高压反应釜内，逐步升温至120~150℃反应12~24h，冷却至室温，利用去离子水和无水乙醇循环离心洗涤三次，在90℃下烘干4h即可得到ABB5O9粉末。
4.根据权利要求2所述的一种低介、低损耗硼化物LTCC材料的制备方法，其特征在于，将混合粉末溶解在去离子水中，制备得到质量浓度为10 %的混合溶液；随后在混合溶液中加入无水乙醇和硅烷偶联剂，其中无水乙醇占总混合溶液体积的30%，硅烷偶联剂占总混合溶液体积的10%。
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