CN108314327B - Ce掺杂低温共烧陶瓷材料及其制备方法 - Google Patents

Ce掺杂低温共烧陶瓷材料及其制备方法 Download PDF

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CN108314327B
CN108314327B CN201810045899.7A CN201810045899A CN108314327B CN 108314327 B CN108314327 B CN 108314327B CN 201810045899 A CN201810045899 A CN 201810045899A CN 108314327 B CN108314327 B CN 108314327B
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韩娇
曾一明
向遥
李世鸿
李文琳
刘继松
白培加
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Sino Platinum Metals Co Ltd
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Abstract

本发明公开了Ce掺杂低温共烧陶瓷材料及其制备方法，属于电子信息功能材料领域，具体涉及一种低温共烧陶瓷材料及其制备方法。本发明陶瓷材料由玻璃粉(质量百分含量为30～50％的CaO，10～20％的B2O3，35～45％的SiO2，0～20％的CeO2经高温熔融水淬法经球磨粉碎过筛烘干制备而成)压制成型烧结而成。本发明陶瓷材料所用玻璃粉粉体密度范围为2.8～3.3g/cm3，软化温度范围为710～750℃，而陶瓷材料热膨胀系数在6.5～8.0×10‑6ppm/℃范围内，介电常数在4～8.5范围内可调，介电损耗在0.9～1.2×10‑3范围内微小波动。

Description

Ce掺杂低温共烧陶瓷材料及其制备方法
技术领域
本发明属于电子信息功能材料领域，涉及一种LTCC基板材料，具体涉及一种低温共烧陶瓷材料及其制备方法。
背景技术
低温共烧陶瓷(low temperature co-fired ceramics,LTCC)技术以其模块化封装和能与金属电极低温匹配共烧的特点，在过去十几年来广泛应用于大规模集成电路封装、雷达、天线和高频无线通信领域，它为无源电子元件的高密度集成和***级电子整机封装提供了理想的技术平台。目前，基于功能陶瓷材料的无源元件的发展相对缓慢，无源元件的模块化和集成化一直不能满足半导体技术快速发展的需求，日益成为半导体技术发展的“瓶颈”。而作为应用于高频通信领域最重要的基板材料之一，钙硼硅(CaO-B2O3-SiO2，CBS)系微晶玻璃具有一系列优异的性能，例如：相对低的烧结温度(<900℃)、极低的介电常数(εr<6.5)和介电损耗(tanδ<1×10-3)，因此成为最重要的LTCC基板材料之一。
随着高频无线通信和微电子封装技术的快速发展，对LTCC技术及微波介质材料提出了更高的要求，包括更高的封装密度、更宽的工艺窗口、更高的力学强度、更低的介电常数和介电损耗等。但CBS系基板材料存在工艺窗口过窄、力学强度不高和共烧过程中物相变化复杂等缺点，随着高频通信技术的快速发展，现有CBS基板材料综合性能越来越难以满足市场需求。因此，开发拥有自主知识产权、适于低温共烧的新材料，成为当下我国低温共烧陶瓷产业发展所必须解决的问题之一。
发明内容
本发明的目的在于提供一种烧结温度、介电性能及热膨胀系数可控的一种低温共烧陶瓷材料及其制备方法。
本发明Ce掺杂低温共烧陶瓷材料按下列步骤实现：
一、掺杂Ce的CBS玻璃粉的制备
1)配制均混料：按比例称量好质量百分含量为30～50％的CaO，10～20％的B2O3，35～45％的SiO2，0～20％的CeO2，并将各原料充分混合均匀，配制成均混料；
2)将上述均混料置于铂金坩埚中，在1300～1500℃的电阻炉中加热熔化，保温2～4h，得到成分均一的玻璃液；
3)将熔制好的玻璃液在倒入去离子水中，经高温熔融水淬法使其快速淬冷形成玻璃颗粒；
4)将得到的玻璃体在行星式球磨机内球磨8～12h，然后将球磨后的物料过500目筛，干燥即得到本发明掺杂Ce的CBS玻璃粉。
所述玻璃粉成分均一，制备温度为1300～1500℃，球磨时间为8～12h，过500目筛，烘干温度为80℃。
所述玻璃粉粉体密度范围为2.8～3.3g/cm3。
所述玻璃粉粒径范围3μm～8μm。
所述玻璃粉软化点范围为710～750℃。
二、掺Ce的低温共烧陶瓷材料制备
将步骤一得到的玻璃粉加入粘结剂PVA进行造粒，在一定压力下压制成型，然后放在烧结垫片上经排胶后常压以750℃～850℃的温度烧结10～30min，自然冷却后即得到掺Ce的低温共烧陶瓷材料。
所述陶瓷材料热膨胀系数在7.6～8.0×10-6ppm/℃范围内。
所述陶瓷材料介电常数在4～8.5范围内可调，介电损耗在0.9～1.2×10-3范围内微小波动。
附图说明
图1是本发明实例1玻璃粉的DSC曲线。
图2是本发明实例1陶瓷材料的热膨胀曲线。
具体实施方式
为了更好地解释本发明，下面结合实施例进一步阐明本发明的具体实施方式及细节，但本发明的内容不仅仅局限于下面所述的实施例，凡根据本发明精神实质所做的等效变化或修饰，都应涵盖在本发明的保护范围之内。
实施例1
(1)将质量百分比为：CaO 38％，B2O3 15％，SiO2 42％，CeO2 5％的原料充分混合均匀，配制成均混料；
(2)将所配制的均混料装入铂金坩埚，在电阻炉内1400℃下保温2～4h，然后将熔熔的玻璃液在倒入去离子水中，使其快速淬冷形成玻璃体；
(3)将得到的玻璃体在行星式球磨机内以450rpm球磨12h，然后将球磨后的物料过500目筛，80℃干燥即得到玻璃粉；
(4)将玻璃粉进行DSC分析测试(如图1所示)，玻璃粉密度为2.97g/cm3，软化点为721℃；
(5)取适量玻璃粉，加入PVA造粒，并在70～100Mpa的压力下压片，将压好的生坯在600℃下保温2h排胶，然后在750-850℃下空气气氛下进行固相烧结15～20min，即得到陶瓷介质材料。
(6)对所得介质材料进行热膨胀系数及介电性能测试，热膨胀系数值为：8.0×10- 6ppm/℃，介电常数为5.8，介电损耗为1.2×10-3。
实施例2
(1)将质量百分比为：CaO 33％，B2O3 12％，SiO2 35％，CeO2 20％的原料充分混合均匀，配制成均混料；
(2)将所配制的均混料装入铂金坩埚，在电阻炉内1400℃下保温2～4h，然后将熔熔的玻璃液在倒入去离子水中，使其快速淬冷形成玻璃体；
(3)将得到的玻璃体在行星式球磨机内以450rpm球磨12h，然后将球磨后的物料过500目筛，80℃干燥即得到玻璃粉；
(4)将玻璃粉进行DSC分析测试，玻璃粉密度为3.26g/cm3，软化点为717℃；
(5)取适量玻璃粉，加入PVA造粒，并在70～100Mpa的压力下压片，将压好的生坯在600℃下保温2h排胶，然后在750-850℃下空气气氛下进行固相烧结15～20min，即得到陶瓷介质材料。
(6)对所得介质材料进行热膨胀系数及介电性能测试，热膨胀系数值为：7.8×10- 6ppm/℃，介电常数为4.1，介电损耗为1.1×10-3。

Claims (2)

1.Ce掺杂低温共烧陶瓷材料的制备方法，其特征在于按下列步骤实现：
(1)将质量百分比为：CaO 33％，B2O3 12％，SiO2 35％，CeO2 20％的原料充分混合均匀，配制成均混料；
(2)将所配制的均混料装入铂金坩埚，在电阻炉内1400℃下保温2～4h，然后将熔融 的玻璃液在倒入去离子水中，使其快速淬冷形成玻璃体；
(3)将得到的玻璃体在行星式球磨机内以450rpm球磨12h，然后将球磨后的物料过500目筛，80℃干燥即得到玻璃粉；
(4)将玻璃粉进行DSC分析测试，玻璃粉密度为3.26g/cm3，软化点为717℃；
(5)取适量玻璃粉，加入PVA造粒，并在70～100Mpa的压力下压片，将压好的生坯在600℃下保温2h排胶，然后在750-850℃下空气气氛下进行固相烧结15～20min，即得到陶瓷介质材料；
(6)对所得介质材料进行热膨胀系数及介电性能测试，热膨胀系数值为：7.8×10-6ppm/℃，介电常数为4.1，介电损耗为1.1×10-3。
2.Ce掺杂低温共烧陶瓷材料的制备方法，其特征在于按下列步骤实现：
(1)将质量百分比为：CaO 38％，B2O3 15％，SiO2 42％，CeO2 5％的原料充分混合均匀，配制成均混料；
(2)将所配制的均混料装入铂金坩埚，在电阻炉内1400℃下保温2～4h，然后将熔融 的玻璃液在倒入去离子水中，使其快速淬冷形成玻璃体；
(3)将得到的玻璃体在行星式球磨机内以450rpm球磨12h，然后将球磨后的物料过500目筛，80℃干燥即得到玻璃粉；
(4)将玻璃粉进行DSC分析测试，玻璃粉密度为2.97g/cm3，软化点为721℃；
(5)取适量玻璃粉，加入PVA造粒，并在70～100Mpa的压力下压片，将压好的生坯在600℃下保温2h排胶，然后在750-850℃下空气气氛下进行固相烧结15～20min，即得到陶瓷介质材料；
(6)对所得介质材料进行热膨胀系数及介电性能测试，热膨胀系数值为：8.0×10-6ppm/℃，介电常数为5.8，介电损耗为1.2×10-3。
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