CN114031404B - 一种介质陶瓷材料的制备方法 - Google Patents
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Abstract
本发明涉及陶瓷材料技术领域,公开了一种介质陶瓷材料的制备方法,包括将原材料三氧化二钐、碳酸锂、三氧化二钕、二氧化钛、碳酸钙与去离子水混合,用球磨机磨成浆料,再过滤脱水、烘干并破碎成粉料,随后预烧结,再次球磨得到二次浆料,继续加入粘合剂并搅拌进行造粒、模压成型、加热排塑,最后将成型材料送至烧结炉中烧结。这种方法制得的介质陶瓷材料拥有较高的品质因数和介电常数、较低的烧结温度,频率温度系数也几近于0,可适用于小型化和集成化的无线通讯系统。
Description
技术领域
本发明涉及陶瓷材料技术领域,尤其涉及一种介质陶瓷材料的制备方法。
背景技术
介质陶瓷材料是指用必要成份的原料进行混合、成型、高温烧结,由粉粒之间的固相反应和烧结过程而获得的微细晶粒无规则集合而成的多晶体,主要用于制作陶瓷电容器和微波介质元件。随着现代通信技术的迅速发展,通信设备使用要求的特殊性使得人们对通信系统装备的重量和尺寸要求越来越高,特别是对移动通信系统中滤波器的小型化、轻便化、高频化、低功耗化方面的要求越来越加强,因此对应用于微波频段电路中作为介质材料的介质陶瓷材料本身的性能要求越来越高,为实现元器件的小型化、集成化甚至模块化,要求介质陶瓷材料拥有高介电常数、稳定的频率温度系数、高品质因数等特点。
发明内容
本发明要解决的技术问题是,提供一种介质陶瓷材料的制备方法,在烧结温度较低的情况下制得了一种具有较高介电常数和品质因数、频率温度系数接近0的介质陶瓷材料,该方法工艺简单,易于工业化生产,且材料性能稳定。
为解决上述问题,本发明提供的方案是:
一种介质陶瓷材料的制备方法,包括以下步骤:
S1:按照质量分数,将原材料8.2~54.0%三氧化二钐、10.4~11.7%碳酸锂、9.0~53.4%三氧化二钕、13.0~22.6%二氧化钛与13.3~18.9%碳酸钙混合;
S2:加入去离子水形成混合料;
S3:用球磨机将:混合料磨成一次浆料;
S4:将一次浆料用压滤机过滤脱水;
S5:将脱水后的一次浆料烘干并破碎成粉料;
S6:将粉料进行预烧结;
S7:向球磨机中加入粉料、去离子水与氧化铜进行二次球磨,得到二次浆料;
S8:向二次浆料中加入粘合剂并搅拌进行造粒得到粉粒;
S9:对粉粒进行模压成型;
S10:对成型后的材料进行加热排塑;
S11:将得到的成型材料送至烧结炉中烧结。
通过二氧化钛的加入,由于变价作用使得晶体内部产生晶格缺陷,活化晶格,促进烧结,为该介质陶瓷材料提供了较低的烧结温度,提高了致密性,碳酸锂作为助烧剂也能降低烧结温度;高介电常数的碳酸钙、稀土金属元素的选取为该介质陶瓷材料提供了较高的介电常数;同时,镧系稀土金属元素的加入有效降低了介电损耗,提高了品质因数,又通过采用不同频率频率温度系数的多种材料复合,实现了正负频率温度系数数值的抵消,拥有近0的频率温度系数,能保证一个稳定的谐振频率,因此在环境温度变化下依旧能稳定工作,可适用于小型化和集成化的无线通讯系统,具有广阔的应用前景。
优选的,粉料的预烧温度设为800~900℃,粉料的预烧时间设为3~5h。
优选的,模压成型时的压力设为1.9~2.4t/cm2。
优选的,加热排塑的温度设为500~600℃并保持60~90min,加热排塑的升温速度小于0.5℃/min。
优选的,成型材料的烧结温度设为1020~1080℃,烧结时间设为2~4h,升温速度小于2.5℃/min。
优选的,一次浆料的粒径分布在0.8~2.2μm范围内。
优选的,二次球磨加入的氧化铜质量百分比设为0~0.75%的粒径分布在0.6~3μm范围内,少量助烧剂氧化铜的加入也有助于适当降低烧结温度,也降低了制备的难度与生产成本。
与现有技术相比,本发明的优点在于:本发明不含重金属成分铅、镍,可在高频领域产品中应用,绿色环保无污染;性能上有较大提升,在烧结温度比较低(1020~1080℃)的情况下,本发明所制得的介质陶瓷材料的介电常数和品质因数值较高,频率温度系数几近于0,可适用于小型化和集成化的无线通讯系统。
附图说明
此处的附图被并入说明书中并构成说明书的一部分,示出了符合本发明的实施例,并与说明书一起用于解释本发明的原理,其中:
图1是本发明公开的一种介质陶瓷材料中粉料的生产流程图;
图2是本发明公开的一种介质陶瓷材料中粉料样品的性能测试结果;
具体实施方式
下文的公开提供了许多不同的实施方式或例子用来实现本发明的不同结构。为了简化本发明的公开,下文中对特定例子的部件和设置进行描述。当然,它们仅仅为示例,并且目的不在于限制本发明。此外,本发明可以在不同例子中重复参考数字和/或参考字母,这种重复是为了简化和清楚的目的,其本身不指示所讨论各种实施方式和/或设置之间的关系。此外,本发明提供了的各种特定的工艺和材料的例子,但是本领域普通技术人员可以意识到其他工艺的应用和/或其他材料的使用。
本发明公开了一种介质陶瓷材料的制备方法,包括以下步骤:
将质量分数为8.2~54.0%三氧化二钐、10.4~11.7%碳酸锂、9.0~53.4%三氧化二钕、13.0~22.6%二氧化钛与13.3~18.9%碳酸钙混合,加入重量为原材料重量80~90%的去离子水并使用球磨机研磨成粒径为0.8~2.2μm的浆料。其中,所有原材料的纯度均为99.5%,球磨机内衬材质为聚氨酯。
将上述浆料用压滤机过滤脱水,再将过滤脱水的浆料烘干,并破碎成粒径小于0.2mm的粉料,随后进行预烧结,预烧温度为800~900℃,预烧时间为3~5h。预烧结可以去除原材料中的挥发组份,例如相对而言熔点较低且能有效降低烧结温度的碳酸锂,碳酸锂在高温时会分解为氧化锂和二氧化碳,同时使氧化物相态转变,以防止后续烧结过程中收缩过大而产生裂纹,同时也可形成所需晶相。
再使用球磨机将预烧结后的粉料与重量为原材料重量50~80%的去离子水、质量分数为0~0.75%的氧化铜(作为助烧剂降低了烧结温度)混合,进行二次球磨,得到粒径为0.6~3μm的二次浆料。
向二次浆料中加入粘合剂并配以搅拌,控制进入喷雾塔内的浆料温度,进行喷雾造粒,将粉料制成具球状流动性的粉体颗粒,颗粒球精度好,颗粒均匀,当然,粉料造粒的方式可以为但不限于为喷雾造粒。其中,粘合剂的配方为:聚乙烯醇3~10%、蒸馏水90~97%。加入的粘合剂重量为原材料重量的13%,进口温度控制在250~300℃,出口温度控制在90~120℃。
再将喷雾造粒获得的粉料使用模压工艺成型,将具球状流动性的粉体颗粒制成所需形状的材料,成型时的压力设为1.9~2.4t/cm2,随之将成型后的材料加热至500~600℃,并保持60~90min,升温速度小于0.5℃/min进行排塑。
最终将排塑处理后的成型材料送至烧结炉中烧结,烧结温度设为1020~1080℃,烧结时间设为2~4h,升温速度小于2.5℃/min,即可得到该介质陶瓷材料。
实施例1
本实施例将质量分数为54.0%三氧化二钐、10.4%碳酸锂、9.3%三氧化二钕、13.0%二氧化钛、13.3%碳酸钙与占原材料重量80%的去离子水混合,一次球磨,脱水,烘干,800℃预烧5h,加入占原材料重量50%的去离子水与质量分数为0.5%的氧化铜进行二次球磨,再喷雾造粒(进口温度250℃,出口温度90℃),压力设为1.9t/cm2进行模压成型,升温速度小于0.5℃/min并在500℃保持90min进行加热排塑,最终1050℃烧结4h,升温速度小于2.5℃/min。
实施例2
本实施例将质量分数为8.2%三氧化二钐、10.4%碳酸锂、53.4%三氧化二钕、14.7%二氧化钛、13.3%碳酸钙与占原材料重量90%的去离子水混合,一次球磨,脱水,烘干,900℃预烧3h,再加入占原材料重量80%的去离子水与质量分数为0.6%的氧化铜进行二次球磨,再喷雾造粒(进口温度300℃,出口温度120℃),压力设为2.4t/cm2进行模压成型,升温速度小于0.5℃/min并在600℃保持60min进行加热排塑,最终1060℃烧结2h,升温速度小于2.5℃/min。
实施例3
本实施例将质量分数为51.3%三氧化二钐、11.7%碳酸锂、9.0%三氧化二钕、13.0%二氧化钛、15.0%碳酸钙与占原材料重量85%的去离子水混合,一次球磨,脱水,烘干,850℃预烧4h,再加入占原材料重量70%的去离子水与质量分数为1.0%的氧化铜进行二次球磨,再喷雾造粒(进口温度270℃,出口温度110℃),压力设为2.1t/cm2进行模压成型,升温速度小于0.5℃/min并在550℃保持75min进行加热排塑,最终1040℃烧结3h,升温速度小于2.5℃/min。
实施例4
本实施例将质量分数为8.2%三氧化二钐、10.4%碳酸锂、39.8%三氧化二钕、22.6%二氧化钛、18.9%碳酸钙与占原材料重量80%的去离子水混合,一次球磨,一次浆料粒径约1.2μm;脱水,烘干,800℃预烧5h,再加入占原材料重量65%的去离子水与质量分数为0.75%的氧化铜进行二次球磨,二次浆料粒径约0.6μm;再加入9%聚乙烯醇粘合剂并配以搅拌,喷雾造粒(进口温度280℃,出口温度105℃),压力设为2.0t/cm2进行模压成型,升温速度小于0.5℃/min并在600℃保持60min进行加热排塑,最终1050℃烧结3h,升温速度小于2.5℃/min。本实施例制备得到的介质陶瓷材料介电常数为95.18,品质常数为6459,频率温度系数为5.1ppm/℃。
实施例5
本实施例将质量分数为8.2%三氧化二钐、10.4%碳酸锂、39.8%三氧化二钕、22.6%二氧化钛、18.9%碳酸钙与占原材料重量80%的去离子水混合,一次球磨,一次浆料粒径约1.2μm;脱水,烘干,800℃预烧5h,再加入占原材料重量60%的去离子水与质量分数为0.75%的氧化铜进行二次球磨,二次浆料粒径约0.6μm;再加入9%聚乙烯醇粘合剂并配以搅拌,喷雾造粒(进口温度280℃,出口温度105℃),压力设为2.0t/cm2进行模压成型,升温速度小于0.5℃/min并在600℃保持60min进行加热排塑,最终1020℃烧结3h,升温速度小于2.5℃/min。本实施例制备得到的介质陶瓷材料介电常数92.34,品质常数4632,频率温度系数18.2ppm/℃。
实施例6
本实施例将质量分数为8.2%三氧化二钐、10.4%碳酸锂、39.8%三氧化二钕、22.6%二氧化钛、18.9%碳酸钙与占原材料重量80%的去离子水混合,一次球磨,一次浆料粒径约1.2μm;脱水,烘干,800℃预烧5h,再加入占原材料重量75%的去离子水与质量分数为0.75%的氧化铜进行二次球磨,二次浆料粒径约0.6μm;再加入9%聚乙烯醇粘合剂并配以搅拌,喷雾造粒(进口温度280℃,出口温度105℃),压力设为2.0t/cm2进行模压成型,升温速度小于0.5℃/min并在600℃保持60min进行加热排塑,最终1080℃烧结3h,升温速度小于2.5℃/min。本实施例制备得到的介质陶瓷材料介电常数95.43,品质常数5156,频率温度系数8.2ppm/℃。
Claims (6)
1.一种介质陶瓷材料的制备方法,其特征在于,包括以下步骤:
S1:按照质量分数,将原材料8.2~54.0%三氧化二钐、10.4~11.7%碳酸锂、9.0~53.4%三氧化二钕、13.0~22.6%二氧化钛与13.3~18.9%碳酸钙混合;
S2:加入去离子水形成混合料;
S3:用球磨机将所述混合料磨成一次浆料;
S4:将所述一次浆料用压滤机过滤脱水;
S5:将脱水后的所述一次浆料烘干并破碎成粉料;
S6:将所述粉料进行预烧结;
S7:向所述球磨机中加入所述粉料、所述去离子水与氧化铜进行二次球磨,得到二次浆料;
S8:向所述二次浆料中加入粘合剂并搅拌进行造粒得到粉粒;
S9:对所述粉粒进行模压成型;
S10:对成型后的材料进行加热排塑;
S11:将得到的成型材料送至烧结炉中烧结,烧结温度设为1020~1080℃,烧结时间设为2~4h,升温速度小于2.5℃/min。
2.根据权利要求1所述的一种介质陶瓷材料的制备方法,其特征在于,所述粉料的预烧温度设为800~900℃,所述粉料的预烧时间设为3~5h。
3.根据权利要求1所述的制备方法,其特征在于,所述粉粒模压成型时的压力设为1.9~2.4t/cm2。
4.根据权利要求1所述的一种介质陶瓷材料的制备方法,其特征在于,所述加热排塑的温度设为500~600℃并保持60~90min,所述加热排塑的升温速度小于0.5℃/min。
5.根据权利要求1所述的一种介质陶瓷材料的制备方法,其特征在于,所述一次浆料的粒径分布在0.8~2.2μm范围内。
6.根据权利要求1所述的一种介质陶瓷材料的制备方法,其特征在于,所述氧化铜的质量分数设为0.5~0.75%,所述二次浆料的粒径分布在0.6~3μm范围内。
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