CN114409389A - 一种低介低损Ba-Si-B-M基LTCC材料及其制备方法 - Google Patents
一种低介低损Ba-Si-B-M基LTCC材料及其制备方法 Download PDFInfo
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Abstract
本发明属于电子信息陶瓷及其制造领域,具体涉及一种低介低损Ba‑Si‑B‑M基LTCC材料及其制备方法。本发明充分利用了复杂化学键理论由于Si4+离子极化率低和Si‑O键的共价键性高,所以Si‑O键的晶格能高这一特性,通过调整Ba‑Si基陶瓷原料配方,采用固相法,在850℃~950℃的低温下烧结成型致密的Ba‑Si‑B‑M基微波陶瓷材料。在烧结过程中形成低共熔化合物,从而推动晶粒重排,并且随着烧结的进行析出BaSi2O5相的陶瓷;并且没有二次相,确保了陶瓷材料的介电性能和机械性能优异,具有高Q×f值,6~7.5的低介电常数,介电损耗低至6.13×10‑4,可在LTCC中推广应用。
Description
技术领域
本发明属于电子信息陶瓷及其制造领域,涉及一种低介电常数、低介电损耗Ba-Si-B-M基微波介质LTCC材料及其制备方法。
背景技术
随着5G通信技术、物联网和全球卫星通信系统的飞速发展,人类已经进入了高速信息的时代。通信信息的容量正指数增加,无线通信逐渐向更高的微波频段发展。通信技术需要满足超大数据吞吐量、高速传输能力等新兴行业的通信需求。因此,可用于5G开发的低温烧结、低介电常数和低介电损耗的微波介质陶瓷是支持该技术发展的必要基础材料。
与之介质天线、高频衬底、高精度电容器和微型化、集成化的毫米波元件的发展,对微波介质陶瓷的介电常数要求越来越低。低介电常数(εr<10)硅酸盐微波介质陶瓷的性能这方面的研究引起了研究领域的极大关注。此外,为了提高微波介质陶瓷的可用性,需要较小的介电损耗(较高的Q×f值),当温度变化时,频率温度系数τf接近于零,以保证使用的稳定性。低温共烧陶瓷(LTCC)是一种有效、实用的烧结陶瓷技术,已成为复杂微型化电路领域的重要技术,并广泛应用于微波介质陶瓷。以Ag和Cu为电极的低温(≤950℃)共烧陶瓷具有良好的化学相容性、低的介电常数和优良的Q×f值,在实际应用中具有很大的潜力。
硅酸盐微波介质陶瓷,如BaSiO3,Ba2Si3O8,BaSi2O5,Ba5Si8O21等具有低介电常数(εr=6~11)、较低的介电损耗,由于烧结温度高于在LTCC所需的最高烧结温度,不利于其在LTCC中的应用。然而迄今为止,研究人员针对Ba-Si基的低温烧结改性及LTCC应用少有报道。
发明内容
针对上述存在问题或不足,为改善Ba-Si基微波陶瓷的烧结特性不足,使其能够保持良好的介电性能在低至950℃下烧结成瓷,以能够应用于LTCC领域,本发明提供了一种低介低损Ba-Si-B-M基LTCC材料及其制备方法,使烧结的Ba-Si-B-M基微波陶瓷材料不形成二次相(确保介电性能和机械性能优异),具有高Q×f值,低温烧结成瓷,能够应用于LTCC领域。
一种低介低损Ba-Si-B-M基LTCC材料,其化学通式为BaSi2BxMyO5,其中M为金属阳离子的Li、Cu、Ca和/或Zn,x=0.05~0.2,y=0.01~0.09;其主晶相为BaSi2O5,无二次相,介电常数6~7.5,损耗低至6.13×10-4。采用BaCO3、SiO2、H3BO3、CuO、CaCO3、Li2CO3和/或ZnO为原料,通过固相法制得;固相法中在900℃~1000℃预烧,850℃~950℃烧结致密。
上述低介低损Ba-Si-B-M基LTCC材料的制备方法,包括以下步骤:
步骤1、按照化学通式BaSi2BxMyO5将原料BaCO3、SiO2、H3BO3、CuO、CaCO3、Li2CO3和/或ZnO配料备用,x=0.05~0.2,y=0.01~0.09;
M依据金属阳离子Li、Cu、Ca和/或Zn的选定选择相应的原料CuO、CaCO3、Li2CO3和/或ZnO。
步骤2、将步骤1所配全部原料与锆球、去离子水以1:5:2~3行星球磨4~6小时至充分混匀后,取出烘干,然后用40-120目筛网(优选60目)过筛。
步骤3、将步骤2所得粉体在大气气氛中以900℃~1000℃预烧4~6小时得预烧料。
步骤4、将步骤3所得预烧料再次与锆球、去离子水以1:5:2~3的比例球磨4~6小时后,取出烘干;然后向烘干后的粉体中添加粘结剂造粒。所述粘结剂为丙烯酸溶液。
步骤5、将步骤4所得产物压制成型,在400~600℃保温2小时排胶后在850~950℃大气气氛中烧结4~6小时,即可制得低介低损Ba-Si-B-M基LTCC材料BaSi2BxMyO5。
本发明充分利用了复杂化学键理论由于Si4+离子极化率低和Si-O键的共价键性高,所以Si-O键的晶格能高这一特性,通过调整Ba-Si基陶瓷原料配方,采用固相法,在850℃~950℃的低温下烧结成型致密的Ba-Si-B-M基微波陶瓷材料。在烧结过程中形成低共熔化合物,从而推动晶粒重排,并且随着烧结的进行析出BaSi2O5相的陶瓷;并且没有二次相,确保了陶瓷材料的介电性能和机械性能优异,具有高Q×f值,6~7.5的低介电常数,介电损耗低至6.13×10-4,能够应用于LTCC领域。
综上所述,本发明通过调整Ba-Si基陶瓷原料配方组成,在850℃~950℃烧结致密,有效解决了Ba-Si基微波介质陶瓷材料烧结温度过高,难以应用于LTCC领域的问题。制备工艺简单,陶瓷材料主晶相为BaSi2O5,具有6~7.5的低介电常数,介电损耗低至6.13×10-4,可在LTCC中推广应用。
附图说明
图1为实施例2、3样品的XRD衍射图谱。
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。
实施例中按照化学通式BaSi2BxMyO5(其中M为金属阳离子的Li、Ca和/或Zn,x=0.05~0.2mol,y=0.05~0.09mol)进行配料,原料为BaCO3、SiO2、Li2CO3、CaCO3、CuO、ZnO和H3BO3。由固相反应制备成本发明材料,具体制备步骤同上述发明内容步骤一致。
样品1~7在最佳烧结温度时的微波介电性能:
图1为实施例2、3样品陶瓷材料的XRD衍射图谱,从图1可以看出,主晶相为BaSi2O5(PDF#26-0176),没有二次相,确保了陶瓷材料的介电性能和机械性能优异,性能均一、可控。
表格数据示出了在化学通式BaSi2BxMyO5配比,850℃~950℃的烧结温度范围内的配料结果及烧熟样品性能。
通过以上实施例的数据可见:本发明配方BaSi2BxMyO5基微波陶瓷材料在850℃~950℃的烧结温度范围内,微波介电性能优异,最佳烧结温度为950℃,能够在低于银电极熔点(961℃)的温度下烧结成瓷,说明该材料能够满足于LTCC工艺要求,有效解决了Ba-Si基微波介质陶瓷材料烧结温度过高的问题。陶瓷材料主晶相为BaSi2O5,具有6~7.5的低介电常数,介电损耗低至6.13×10-4,可在LTCC中推广应用。
Claims (4)
1.一种低介低损Ba-Si-B-M基LTCC材料,其特征在于:
其化学通式为BaSi2BxMyO5,其中M为金属阳离子的Li、Cu、Ca和/或Zn,x=0.05~0.2,y=0.01~0.09;其主晶相为BaSi2O5,无二次相,介电常数6~7.5,损耗低至6.13×10-4;
采用BaCO3、SiO2、H3BO3、CuO、CaCO3、Li2CO3和/或ZnO为原料,通过固相法制得;固相法中在900℃~1000℃预烧,850℃~950℃烧结致密。
2.如权利要求1所述低介低损Ba-Si-B-M基LTCC材料的制备方法,其特征在于,包括以下步骤:
步骤1、按照化学通式BaSi2BxMyO5将原料BaCO3、SiO2、H3BO3、CuO、CaCO3、Li2CO3和/或ZnO配料备用,其中x=0.05~0.2,y=0.01~0.09;
M依据金属阳离子Li、Cu、Ca和/或Zn的选定选择相应的原料CuO、CaCO3、Li2CO3和/或ZnO;
步骤2、将步骤1所配全部原料与锆球、去离子水以1:5:2~3行星球磨4~6小时至充分混匀后,取出烘干,然后用40-120目筛网过筛;
步骤3、将步骤2所得粉体在大气气氛中以900℃~1000℃预烧4~6小时得预烧料;
步骤4、将步骤3所得预烧料再次与锆球、去离子水以1:5:2~3的比例球磨4~6小时后,取出烘干;然后向烘干后的粉体中添加粘结剂造粒;
步骤5、将步骤4所得产物压制成型,在400~600℃保温2小时排胶后在850~950℃大气气氛中烧结4~6小时,即可制得低介低损Ba-Si-B-M基LTCC材料BaSi2BxMyO5。
3.如权利要求2所述低介低损Ba-Si-B-M基LTCC材料的制备方法,其特征在于:所述步骤2中筛网采用60目筛网。
4.如权利要求1所述低介低损Ba-Si-B-M基LTCC材料的制备方法,其特征在于:所述步骤3中粘结剂为丙烯酸溶液。
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