CN116199508B - 一种5g波导滤波器用微波介质材料及其制备方法、应用 - Google Patents
一种5g波导滤波器用微波介质材料及其制备方法、应用 Download PDFInfo
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- CN116199508B CN116199508B CN202310234136.8A CN202310234136A CN116199508B CN 116199508 B CN116199508 B CN 116199508B CN 202310234136 A CN202310234136 A CN 202310234136A CN 116199508 B CN116199508 B CN 116199508B
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Abstract
本发明涉及一种5G波导滤波器用微波介质材料及其制备方法、应用。所述5G波导滤波器用微波介质材料的化学式为(1+x)(Mg1‑y,Zny)(Ti1‑z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO;其中,MO为添加剂,包括Y2O3、NiO、CuO、La2O3、Sm2O3、Nd2O3、MnO2和碳纳米管。本发明解决了目前国内外同类微波介质材料及5G波导滤波器器件因为陶瓷太脆的原因而导致在热震和1000H温循测试后陶瓷瓷体特别是盲孔位置容易开裂的行业痛点,可以提高其断裂韧性和抗弯强度,满足5G通信***用5G波导滤波器的综合性能要求。
Description
技术领域
本发明涉及电子信息功能材料及器件技术领域,特别是涉及一种5G波导滤波器用微波介质材料及其制备方法、应用。
背景技术
目前,5G滤波器陶瓷材料的脆性是制约其发展的主要因素之一,因此增韧成为5G滤波器陶瓷材料研究领域的核心问题。随着5G网络的快速部署,5G大规模天线(MassiveMIMO)技术使得天线的数量倍数增长,通道数达到64个甚至128个,而每个天线都需要配备相应的介质波导滤波器和双工器,并由相应的滤波器进行信号频率的选择和处理,因此对于滤波器的需求量大量增加;同时,5G通信把远端射频单元(RRU)和天线集成为主动天线单元(AAU),基站的高度集成化和小型化发展对于滤波器的尺寸和发热性能有更高的要求。5G通信对滤波器的小型化、轻量化、低成本、高性能的需求明显,但目前4G通信采用的金属腔体滤波器体积大,重量大,发热多,且价格较贵,难以在高集成化天线中广泛使用。目前,常用的5G滤波器陶瓷材料介电常数εr在18~23之间的高品质因数,中低介电常数材料以复合钙钛矿体系MgTiO3为代表,这类瓷料的缺点是太脆,韧性低,在热震和1000H温循测试后,陶瓷瓷体特别是盲孔位置容易开裂,这是全行业的痛点问题。
发明内容
基于此,有必要针对现有瓷料太脆,韧性低,在热震和1000H温循测试后,陶瓷瓷体特别是盲孔位置容易开裂的技术问题,提供一种5G波导滤波器用微波介质材料及其制备方法、应用。
本发明提出一种5G波导滤波器用微波介质材料,其化学式为:
(1+x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO,
其中:x=0.03-0.08,y=0.01-0.15,z=0.01-0.1,a=0.1-3.5,b=0.1-3.5,c=0.1-3.5;
其中,MO为添加剂,包括Y2O3、NiO、CuO、La2O3、Sm2O3、Nd2O3、MnO2和碳纳米管。
在本发明的一较实施例中,所述(1+x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3的原料为MgO、SrCO3、TiO2、ZnO、ZrO2;
在本发明的一较佳实施例中,x=0.04-0.07,y=0.01-0.11,z=0.02-0.08。
在本发明的一较佳实施例中,x=0.05-0.065,y=0.03-0.08,z=0.03-0.07。
在本发明的一较佳实施例中,a=0.2-1.8,b=0.2-1.8,c=0.2-1.8。
在本发明的一较佳实施例中,a=0.3-1.7,b=0.3-1.7,c=0.3-1.7。
在本发明的一较佳实施例中,添加剂MO中每种材料的添加量为0.1-1.5wt%,优选0.2-1.0wt%,而碳纳米管至少添加0.05wt%以上。
在本发明的一较佳实施例中,所述微波介质材料介电常数为18.0-23.0,QF值为60000GHz-10000GHz,谐振频率温度系数为0-±5ppm/℃。
本发明还提出一种前述的5G波导滤波器用微波介质材料的制备方法,包括以下步骤:
S1、
将原料按照化学式为(1-x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO进行配料,
其中:x=0.03-0.08,y=0.01-0.15,z=0.01-0.1,a=0.1-3.5,b=0.1-3.5,c=0.1-3.5;MO包括Y2O3、NiO、CuO、La2O3、Sm2O3、Nd2O3、MnO2和碳纳米管;
S2、将原料进行湿法球磨混合,得到浆料A;
S3、将浆料A进行造粒,得到造粒料;
S4、将造粒料进行高温预烧,得到粉料;
S5、将粉料进行湿法球磨,得到浆料B;再将浆料B进行砂磨,得到浆料C;
S6、将浆料C与粘合剂、助剂混合后进行造粒,压片制成生坯,生坯烧结,即得5G波导滤波器用微波介质材料。
在本发明的一较佳实施例中,步骤S2中的湿法球磨包括以下步骤:先将原料、球磨介、去离子水按照1∶2.5∶2.0的质量比置于球磨机中进行湿法球磨5-8h;再置于砂磨机中进行湿法球磨5-8h。
在本发明的一较佳实施例中,步骤S3中的造粒为喷雾干燥造粒,进口温度为210℃-265℃,出口温度为95℃-115℃,雾化盘转速为6500-8500r;优选地,进口温度为225℃-255℃;更优选地,进口温度为235℃-245℃。
在本发明的一较佳实施例中,步骤S4中的高温预烧温度为1150℃-1250℃,预烧时间为3-4h;优选地,高温预烧温度为1165℃-1225℃;优选地,高温预烧温度为1175℃-1205℃。
在本发明的一较佳实施例中,步骤S5中的湿法球磨时间为5-8h,砂磨时间为5-8h。
在本发明的一较佳实施例中,步骤S6中,将浆料C与万分之3-5的消泡剂、千分之3-5的表面活性剂、千分之3-5的脱模剂、千分之3-5的丙三醇以及聚乙烯醇与聚乙二醇粘合剂胶水混合均匀后进行喷雾造粒,得到平均粒径为85-125μm的粉料,其中:胶含量是干料重量的3%-5%,喷雾造粒进口温度为210℃-265℃,出口温度为95-115℃,雾化盘转速为6500-8500r,优选地,进口温度为225℃-255℃,更优选地,进口温度为235℃-245℃;
和/或,压片密度为2.2-2.45g/cm3,生坯直径为15mm、厚度为11-13mm;所述烧结条件为:排胶温区为200℃-500℃,升温时间为3h;其他温段升温时间按照每小时200-300℃;高温烧结温区为1250℃~1350℃,烧结时间为3-4h,然后随炉温降温,成瓷密度3.7-3.9g/cm33。
本发明还提出一种如上述的5G波导滤波器用微波介质材料在5G通信基站用滤波器、谐振器或双工器以及卫星导航天线中的应用。
与现有技术相比,本发明具有以下有益效果:
1.本发明5G陶瓷滤波器材料通过复合添加添加ZnO、ZrO2、Y2O3、Al2O3、SiO2、NiO、CuO、La2O3、Sm2O3、Nd2O3、Nb2O5、MnO2、碳纳米管等增韧剂和改性添加剂,实现了微波介质材料的增韧和良好的微波性能完美统一,解决了目前国内外同类微波介质材料及5G波导滤波器器件因为陶瓷太脆的原因而导致在热震和1000H温循测试后陶瓷瓷体特别是盲孔位置容易开裂的行业痛点,可以提高断裂韧性3-5倍,其抗弯强度达到850MPa,断裂韧性达到10-11.5MPa·m1/2,满足5G通信***用5G波导滤波器的综合性能要求。
2.本发明基于中温固相法,制备方法简单,生产成本较低,能够得到一种高韧性的微波性能良好的中低介电常数的5G微波介质陶瓷材料;本发明方法制得的微波介质陶瓷材料介电常数为18.0-23.0,高品质因数QF为60000GHz~10000GHz,谐振频率温度系数范围为0-±5ppm/℃,具有低介电常数和高品质因数,属于中低介电陶瓷体系。
3.本发明微波介质材料的原料全部采用电子级原材料,通过对球磨、砂磨粒度的精细控制,以及适当的一次预烧温度工艺,实现了该材料的工业规模化生产。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
下面对本发明做进一步的详细描述。
本发明提供的5G波导滤波器用微波介质材料,微波介质材料制成的介质波导滤波器可以作为5G通信基站用滤波器应用。介质波导滤波器由于具有较高的介电常数,更低的***损耗及近零的频率温度系数,其体积比金属腔滤波器小很多,完全可以满足小型化、轻量化、低损耗及性价比的要求,已经成为5G通信用滤波器的主流解决方案。微波介质材料除用于制备5G通信基站用滤波器之外,还可应用于谐振器或双工器以及卫星导航天线中。
本实施例中提供一种5G波导滤波器用微波介质材料,化学式为(1+x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO,其中:x=0.03-0.08,y=0.01-0.15,z=0.01-0.1,a=0.1-3.5,b=0.1-3.5,c=0.1-3.5。(1+x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3的原料为MgO、SrCO3、TiO2、ZnO、ZrO2。
其中MO为添加剂,包括Y2O3、NiO、CuO、La2O3、Sm2O3、Nd2O3、MnO2和碳纳米管,每种的添加量可为0.1-1.5wt%,优选0.2-1.0wt%,其中碳纳米管至少添加0.05wt%以上。
本实施例中的微波介质材料介电常数为18.0-23.0,QF值为60000GHz-10000GHz,谐振频率温度系数为0-±5ppm/℃。
上述化学式所添加的增韧剂的增韧机理说明如下:
1)相变增韧:添加ZrO2和Y2O3增韧剂,利用ZrO2的相变增韧特性,实现对5G滤波器陶瓷材料的增韧,其增韧机理是:当含有亚稳四方相ZrO2陶瓷受到外加应力作用时,其中的四方相ZrO2颗粒会转变成同素异构体单斜ZrO2相,同时产生3%-5%的体积膨胀,吸收应变能并弥合裂纹,从而提高材料的断裂韧性;同时,由于相变所引起的体积膨胀对裂纹产生压应力,阻碍裂纹的扩展,表现在裂纹尖端应力强度因子降低,从而提高抗裂纹扩展能力;ZrO2颗粒作为增韧剂增韧5G陶瓷滤波器的效果与材料的成分、烧结温度、晶粒尺寸等因素密切相关,尽管相变增韧效果明显,但是受温度的影响很大,通过加入少量的Y2O3稳定剂,能大大提高陶瓷的高温适应能力;
(2)碳纳米管增韧:碳纳米管具有极高的强度、韧性和弹性模量,其模量可达1TMpa,与金刚石模量几乎相同,将微量添加的碳纳米管作为5G滤波器陶瓷材料的增强体,可表现出良好的强度、弹性、抗疲劳性及各向同性;碳纳米管增韧5G滤波器陶瓷材料机理是:利用短纤维增韧的作用,碳纳米管力学性能优异,在拔出和断裂时,都要消耗更多的能量,有利于阻止陶瓷裂纹的扩展;此外,碳纳米管对陶瓷晶粒的桥联、钉扎等作用,能达到传递和均摊载荷的目的,使陶瓷裂纹扩展方式由沿晶断裂转化为穿晶断裂,能显著提高5G滤波器陶瓷的韧性;碳纳米管还能与陶瓷形成独特网络结构,使裂纹沿晶界发生偏转,有助于提高5G滤波器陶瓷的断裂韧性;
(3)晶须增韧:通过Al2O3晶须、ZrO2晶须、SiC晶须在陶瓷中对裂纹的桥接、钉扎或偏转及晶须的拔出等作用,来显著提高5G滤波器陶瓷材料的韧性,晶须增韧机理主要有拔出桥接机制和裂纹偏转机制;
(4)颗粒弥散增韧:颗粒弥散增韧主要是在5G滤波器陶瓷基体中直接或间接加入高弹性模量的非金属材料,如SiC、TiC等,或具有延性的材料如Al、Ni、Cu、Ti等作为第二相粒子,高弹性模量颗粒在基体材料拉伸时阻止横向截面的收缩,要达到和基体相同的横向收缩,必须增加纵向拉应力,使材料强化,增加外界拉应力使材料消耗更多的能量,因此具有增韧效果。本发明通过间接添加碳纳米管,碳纳米管和SiO2、TiO2在球磨的过程中混合均匀,在后续的高温烧结过程中发生固相反应形成了高弹性模量的SiC和TiC,从而达到颗粒弥散增韧的效果;
(5)复合增韧:通过采用多种增韧机制复合增韧的方式提高5G陶瓷滤波器材料韧性,主要方法有:多相颗粒复合增韧、晶须-颗粒复合增韧、晶须-相变复合增韧等。
与现有技术相比,该材料通过复合添加ZnO、ZrO2、Y2O3、Al2O3、SiO2、NiO、CuO、La2O3、Sm2O3、Nd2O3、Nb2O5、MnO2;碳纳米管等增韧剂和改性添加剂;实现了该材料的增韧和良好的微波性能完美统一,解决了目前国内外同类微波介质材料及5G波导滤波器器件因为陶瓷太脆的原因而导致在热震和1000H温循测试后陶瓷瓷体特别是盲孔容易开裂的行业痛点。
本实施例的5G波导滤波器用微波介质材料的制备方法,包括以下步骤:
S1、将原料按照化学式为:
(1-x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO进行配比。
其中:x=0.03-0.08,y=0.01-0.15,m=89.5-99.7,z=0.01-0.1,a=0.1-3.5,b=0.1-3.5,c=0.1-3.5。
S2、将原料、球磨介、去离子水按照1∶2.5∶2.0的质量比置于球磨机湿法球磨5-8h,然后再打到砂磨机中进行湿法球磨5-8h,得到符合粒度要求的浆料料A。
S3、将浆料A进行喷雾干燥造粒,进口温度210-265℃,优选225-255℃,更优选235-245℃;出口温度95-115℃,雾化盘转速6500-8500r,得到符合一定粒度要求的造粒料。
S4、将得到的造粒料置于高温隧道烧结炉中于1150-1250℃(优选1165-1225℃,更优选1175-1205℃)进行预烧,保温时间为3-4小时,得到粉料。
S5、将预烧过的粉料和去离子水置于球磨机中进行湿法球磨5-8h,得到浆料料B。再将浆料B打入砂磨机搅拌罐进行砂磨5-8h,得到符合粒度要求的浆料C。
S6、将浆料C与粘合剂、助剂混合后进行造粒,压片制成生坯,生坯烧结,即得5G波导滤波器用微波介质材料,将烧结好的(1-x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO+陶瓷研磨抛光制成测试样品。
其中:将浆料C与万分之3-5的消泡剂、千分之3-5的表面活性剂、千分之3-5的脱模剂、千分之3-5的丙三醇以及聚乙烯醇与聚乙二醇粘合剂胶水混合均匀后进行喷雾造粒,得到平均粒径为85-125μm的粉料,其中:胶含量是干料重量的3%-5%,喷雾造粒进口温度为210℃-265℃,优选225-255℃,更优选235-245℃;出口温度为95-115℃,雾化盘转速为6500-8500r。
压片制成生坯:压片密度为2.2-2.45g/cm3,生坯直径为15mm、厚度为11-13mm。
生坯烧结:烧结条件为:先以200℃-300℃/h升温至200℃-500℃进行排胶,升温时间为3h。再以200℃-300℃/h升温至1250℃-1350℃进行烧结,烧结时间为3-4h,成瓷密度为3.7-3.9g/cm3。
采用本发明微波介质材料制作的样品,做如下性能测试:用安捷伦E5071B网络分析仪配合平行板法对5G波导滤波器用微波介质材料进行性能测试,测试***包含网络分析仪,厦门大学的电脑分析软件,测试夹具,可程序恒温高低温箱等。
以下给出10个实施例的化学原料配方以及样品测试数据,分别见表1、表2。
表1化学原料配方以及微波性能测试数据
序号 | x=y=z | MgO | SrCO3 | ZnO | ZrO2 | TiO2 | Al2O3 | SiO2 | MO | 介电 | QF | τf |
配方1 | 0.04 | 37.15 | 5.905 | 3.1 | 4.73 | 73.61 | 0.35 | 1.45 | 1.0 | 18.9 | 98500 | ±6ppm |
配方2 | 0.05 | 36.38 | 7.382 | 3.9 | 5.85 | 72.08 | 0.55 | 1.15 | 1.5 | 19.5 | 88100 | ±5ppm |
配方3 | 0.06 | 35.62 | 8.858 | 4.6 | 6.95 | 70.57 | 0.85 | 0.85 | 2.0 | 20.5 | 86300 | ±5ppm |
配方4 | 0.07 | 34.86 | 10.33 | 5.3 | 8.02 | 69.08 | 1.15 | 0.55 | 2.5 | 21.2 | 75400 | ±5ppm |
配方5 | 0.08 | 34.12 | 11.81 | 6.0 | 9.06 | 67.60 | 1.45 | 0.35 | 3.0 | 22.8 | 55500 | ±4ppm |
从表1可以看出,以上五个实施例都取x=y=z的特殊值,实际应用不限于特殊取值,只要是取本发明化学式优选的任意范围值都可以达到优异的微波性能指标。
表1配方1-5的样品在做温循测试和温度冲击(两箱法)实验后陶瓷体均没有裂纹,测试后微波性能良好,满足5G通信***用5G波导滤波器滤波器的综合性能要求。
表2化学原料配方以及微波性能测试数据
序号 | x=y | MgO | SrCO3 | ZnO | ZrO2 | TiO2 | Al2O3 | SiO2 | MO | 介电 | QF | τf |
配方6 | 0.04 | 37.15 | 5.905 | 3.1 | 0 | 79.87 | 0 | 1.45 | 1.0 | 19.3 | 81500 | ±8ppm |
配方7 | 0.05 | 36.38 | 7.382 | 3.9 | 0 | 79.87 | 0 | 1.15 | 1.5 | 19.8 | 72100 | ±7ppm |
配方8 | 0.06 | 35.62 | 8.858 | 4.6 | 0 | 79.87 | 0 | 0.85 | 2.0 | 20.7 | 71300 | ±6ppm |
配方9 | 0.07 | 34.86 | 10.33 | 5.3 | 0 | 79.87 | 0 | 0.55 | 2.5 | 21.5 | 67200 | ±6ppm |
配方10 | 0.08 | 34.12 | 11.81 | 6.0 | 0 | 79.87 | 0 | 0.35 | 3.0 | 23.0 | 59500 | ±5ppm |
表2作为对比实施例,由于缺少了增韧剂ZrO2和Al2O3,材料的Qf值和温漂等微波性能都有所下降,最大的缺点是,陶瓷的韧性变差。
表2作为对比实施例,配方6-10的样品在做温循测试和温度冲击(两箱法)实验后均发现有个别测试样品陶瓷体有微小的裂纹,测试后微波性能变差。
主要的测试方法如下:
1、温循测试
实验时间:800cycle
实验应力:-40℃-+125℃温度变化速度11-15℃/min(高低温保持30min)
2、温度冲击(两箱法)实验
温度要求:-40℃-+125℃;两箱法,转换在2min内完成;每个温区滞留15min;持续500个循环。
目前,5G滤波器陶瓷材料因为陶瓷材料太脆,在热震、冷热温冲和1000H温循测试后陶瓷瓷体特别是盲孔容易开裂是制约其发展的主要因素之一,因此增韧成为5G滤波器陶瓷材料研究领域的核心问题。本发明提供了一种用作5G波导滤波器的微波介质材料制备方法,、通过配料、混料球磨、喷雾造粒烘干、1150-1250℃/3-4H预烧、球磨、砂磨、喷雾干燥造粒、压制、1250-1350℃/3-4H烧结等步骤方法制备出该材料,制备出的微波介质陶瓷材料具有高的品质因数,
其εr=18-23,Qf=60000-10000GHz,τf=±5ppm/℃,该材料可以用作生产5G通信基站天线用介质波导滤波器。与现有技术相比,本实施例5G滤波器陶瓷材料通过复合添加ZnO、ZrO2、Y2O3、Al2O3、SiO2、NiO、CuO、La2O3、Sm2O3、Nd2O3、Nb2O5、MnO2和碳纳米管等增韧剂和改性添加剂;实现了该材料的增韧和良好的微波性能完美统一,解决了目前国内外同类微波介质材料及5G波导滤波器器件因为陶瓷太脆的原因而导致在热震、冷热温冲和1000H温循测试后陶瓷瓷体特别是盲孔容易开裂的行业痛点。
以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (16)
1.一种5G波导滤波器用微波介质材料,其特征在于,其化学式为:
(1+x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO,
其中:x=0.03-0.08,y=0.01-0.15,z=0.01-0.1,a=0.1-3.5,b=0.1-3.5,c=0.1-3.5;
其中,MO为添加剂,包括Y2O3、NiO、CuO、La2O3、Sm2O3、Nd2O3、MnO2和碳纳米管。
2.根据权利要求1所述的5G波导滤波器用微波介质材料,其特征在于,所述(1+x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3的原料为MgO、SrCO3、TiO2、ZnO、ZrO2;
和/或,x=0.04-0.07,y=0.01-0.11,z=0.02-0.08;
和/或,a=0.2-1.8,b=0.2-1.8,c=0.2-1.8。
3.根据权利要求1所述的5G波导滤波器用微波介质材料,其特征在于,所述微波介质材料介电常数为18.0-23.0,Qf值为60000GHz-10000GHz,谐振频率温度系数为0-±5ppm/℃。
4.一种如权利要求1-3中任一项所述的5G波导滤波器用微波介质材料的制备方法,其特征在于,包括以下步骤:
S1、将原料按照化学式为(1+x)(Mg1-y,Zny)(Ti1-z,Zrz)O3+xSrTiO3+awt%Al2O3+bwt%SiO2+cwt%MO进行配料,
其中:x=0.03-0.08,y=0.01-0.15,z=0.01-0.1,a=0.1-3.5,b=0.1-3.5,c=0.1-3.5;MO包括Y2O3、NiO、CuO、La2O3、Sm2O3、Nd2O3、MnO2和碳纳米管;
S2、将原料进行湿法球磨混合,得到浆料A;
S3、将浆料A进行造粒,得到造粒料;
S4、将造粒料进行高温预烧,得到粉料;
S5、将粉料进行湿法球磨,得到浆料B;再将浆料B进行砂磨,得到浆料C;
S6、将浆料C与粘合剂、助剂混合后进行造粒,压片制成生坯,生坯烧结,即得5G波导滤波器用微波介质材料。
5.根据权利要求4所述的5G波导滤波器用微波介质材料的制备方法,其特征在于,步骤S2中的湿法球磨包括以下步骤:先将原料、球磨介、去离子水按照1∶2.5∶2.0的质量比置于球磨机中进行湿法球磨5-8h;再置于砂磨机中进行湿法球磨5-8h。
6.根据权利要求4所述的5G波导滤波器用微波介质材料的制备方法,其特征在于,步骤S3中的造粒为喷雾干燥造粒,进口温度为210℃-265℃,出口温度为95℃-115℃,雾化盘转速为6500-8500r。
7.根据权利要求6所述的5G波导滤波器用微波介质材料的制备方法,其特征在于:进口温度为225℃-255℃。
8.根据权利要求7所述的5G波导滤波器用微波介质材料的制备方法,其特征在于:进口温度为235℃-245℃。
9.据权利要求4所述的5G波导滤波器用微波介质材料的制备方法,其特征在于,步骤S4中的高温预烧温度为1150℃-1250℃,预烧时间为3-4h。
10.据权利要求9所述的5G波导滤波器用微波介质材料的制备方法,其特征在于:高温预烧温度为1165℃-1225℃。
11.据权利要求10所述的5G波导滤波器用微波介质材料的制备方法,其特征在于:高温预烧温度为1175℃-1205℃。
12.根据权利要求4所述的5G波导滤波器用微波介质材料的制备方法,其特征在于,步骤S5中的湿法球磨时间为5-8h,砂磨时间为5-8h。
13.据权利要求4所述的5G波导滤波器用微波介质材料的制备方法,其特征在于,步骤S6中,将浆料C与万分之3-5的消泡剂、千分之3-5的表面活性剂、千分之3-5的脱模剂、千分之3-5的丙三醇,以及含聚乙烯醇与聚乙二醇的粘合剂胶水混合均匀后进行喷雾造粒,得到平均粒径为85-125μm的粉料,其中:胶含量是干料重量的3%-5%,喷雾造粒进口温度为210℃-265℃,出口温度为95-115℃,雾化盘转速为6500-8500r;
和/或,压片密度为2.2-2.45g/cm3,生坯直径为15mm、厚度为11-13mm;所述烧结条件为:排胶温区为200℃-500℃,升温时间为3h;其他温段升温时间按照每小时200-300℃;高温烧结温区为1250℃~1350℃,烧结时间为3-4h,然后随炉温降温,成瓷密度3.7-3.9g/cm3。
14.据权利要求13所述的5G波导滤波器用微波介质材料的制备方法,其特征在于:喷雾造粒进口温度为225℃-255℃。
15.据权利要求14所述的5G波导滤波器用微波介质材料的制备方法,其特征在于:喷雾造粒进口温度为235℃-245℃。
16.一种如权利要求1-3中任一项所述的5G波导滤波器用微波介质材料在5G通信基站用滤波器、谐振器或双工器以及卫星导航天线中的应用。
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