CN107244916A - 一种铌酸盐系低温烧结微波介质陶瓷材料及其制备方法 - Google Patents
一种铌酸盐系低温烧结微波介质陶瓷材料及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 37
- YGBGWFLNLDFCQL-UHFFFAOYSA-N boron zinc Chemical compound [B].[Zn] YGBGWFLNLDFCQL-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011701 zinc Substances 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 9
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- 238000000498 ball milling Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 5
- 210000004127 vitreous body Anatomy 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002242 deionisation method Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 19
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 16
- 239000000919 ceramic Substances 0.000 description 10
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- 230000015572 biosynthetic process Effects 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
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- 239000010955 niobium Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- 238000012512 characterization method Methods 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
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- 238000009766 low-temperature sintering Methods 0.000 description 1
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- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
一种铌酸盐系低温烧结微波介质陶瓷材料及其制备方法,属于微波电子陶瓷材料及其制备领域。包括主晶相和占主晶相重量百分比为1%~4%的锌硼玻璃,所述主晶相为Ni1‑xZnxTiNb2O8,其中,0.2≤x≤0.8;所述锌硼玻璃以其标准物计的含量为:ZnO 50mol%~70mol%,HBO3 30mol%~50mol%。本发明提供的陶瓷材料在900~950℃烧结良好,其介电常数εr=32~35,Q×f=13000~21000GHz,谐振频率温度系数τf=‑15~+6ppm/℃,可广泛应用于LTCC叠层微波器件中。
Description
技术领域
本发明属于微波电子陶瓷材料及其制备领域,具体涉及一种具有中介电常数、低损耗特性和高温度稳定性的铌酸盐系低温共烧陶瓷(Low Temperature Co-firedCeramic,缩写LTCC)材料及其制备方法。
背景技术
微波介质陶瓷是指应用于微波频段(主要是300MHz-30GHz频段)电路中作为介质材料并完成一种或多种功能的陶瓷,在现代通讯中被广泛应用于谐振器、介质滤波器、基片、波导回路等元器件中。随着移动通信技术的不断升级,各类通信设备的更新换代和普及,对器件及材料的要求将会越来越高。
微波介质陶瓷的应用需要满足以下条件:适宜的介电常数有利于器件的小型化(介质元器件的尺寸与介电常数εr的平方根成反比);介电常数的提高要保证一定的Q×f值;接近于零的谐振频率温度系数。而根据介电常数可将微波介质陶瓷分为三类:低介电常数类(εr<20),中介电常数类(20≤εr≤70),高介电常数类(εr>70)。
目前对低介电常数的LTCC微波介质材料的研究已经相对成熟,大量的材料体系已实现商业化生产,而中高介电常数的LTCC微波介质材料研究相对滞后,这主要是由于中高介电常数材料难以同时实现较高的Q×f值和接近于零的温度系数。中介电常数类微波介质陶瓷主要包括ZrTiO4、SnTiO4、铌酸盐、钙基或钡基复合钙钛矿等,这类微波介质陶瓷主要用于卫星通讯和移动通讯基站,其中的铌酸盐由于具有适宜的介电常数(20~80)和较高的Q×f值而被广泛研究。J.X.Bi等(J.X.Bi,C.H.Yang,H.T.Wu.Synthesis,characterization,and microwave dielectric properties of Ni0.5Ti0.5NbO4ceramics through theaqueous sol-gel process,J.Alloys Compd.653(2015)1-6)报道了一种铌酸盐微波介质陶瓷材料Ni0.5Ti0.5NbO4,其具有较高的介电常数εr=59.95和较高的Q×f=15094GHz,但是其谐振频率温度系数τf=111.15ppm/℃,且烧结温度高(1100℃)。中介电常数类微波介质陶瓷可以应用于介质滤波器等的制备,因此,在降低烧结温度的同时保持其良好的介电性能(介电常数和Q×f值),同时调整其谐振频率温度系数接近于零,满足LTCC材料的要求,成为研究者努力的方向。
发明内容
本发明的目的在于:针对上述存在的问题或不足,提供一种可用于LTCC低温烧结(900~950℃),介电常数εr=32~35,Q×f=13000~21000GHz,谐振频率温度系数τf=-15~+6ppm/℃的微波介质陶瓷材料及其制备方法。
本发明的技术方案如下:
一种铌酸盐系低温烧结微波介质陶瓷材料,包括主晶相和占主晶相重量百分比为1%~4%的锌硼玻璃,所述主晶相为Ni1-xZnxTiNb2O8,其中,0.2≤x≤0.8;所述锌硼玻璃以其标准物计的含量为:ZnO 50mol%~70mol%,HBO330mol%~50mol%;所述主晶相中加入占主晶相重量百分比为1%~4%的锌硼玻璃,经球磨、烘干、造粒、干压成型过程后,在900~950℃下烧结6~12h,即得到所述铌酸盐系低温烧结微波介质陶瓷材料。
进一步地,所述锌硼玻璃按照50mol%~70mol%ZnO,30mol%~50mol%HBO3的比例配料后,经4~10h球磨,加热至950~1000℃下保温1~3h,在其熔融状态下快速倒入去离子中淬火得到透明玻璃体,研磨粉碎,得到玻璃相助烧剂锌硼玻璃。
一种铌酸盐系低温烧结微波介质陶瓷材料的制备方法,包括以下步骤:
步骤1、主晶相的制备:以氧化锌(ZnO)、氧化亚镍(NiO)、二氧化钛(TiO2)、五氧化二铌(Nb2O5)为原料,按照分子式Ni1-xZnxTiNb2O8(0.2≤x≤0.8)的比例称料后进行湿法球磨混合,球磨时间为8~24h,烘干后在850~1000℃下预烧6~16h,得到主晶相Ni1- xZnxTiNb2O8;
步骤2、锌硼玻璃的制备:将ZnO和HBO3按照摩尔百分比为50mol%~70mol%ZnO,30mol%~50mol%HBO3的比例配料,行星球磨4~10h后,烘干过筛,然后在950~1000℃下保温1~3h,在其熔融状态下快速倒入去离子中淬火得到透明玻璃体,研磨粉碎,得到锌硼玻璃;
步骤3、在步骤1得到的主晶相中加入占主晶相重量百分比为1%~4%的步骤2得到的锌硼玻璃,经球磨、烘干、造粒、干压成型过程后,得到的坯件在900~950℃下烧结6~12h,即得到所述铌酸盐系低温烧结微波介质陶瓷材料。
本发明的有益效果为:
铌酸钛镍锌体系中含有两种相:四方晶系的Ni0.5Ti0.5NbO4和正交晶系的ZnTiNb2O8,其中,Ni0.5Ti0.5NbO4的谐振频率温度系数为正,ZnTiNb2O8的谐振频率温度系数为负,本发明为了优化介质材料的各项性能,主晶相选择Zn取代一部分Ni的Ni1-xZnxTiNb2O8材料,以获得温度稳定的介电陶瓷,同时加入适当含量的锌硼玻璃作为烧结助剂,不仅有效降低了烧结温度,而且锌硼玻璃中的Zn+会与主晶相材料发生反应,使得ZnTiNb2O8相含量增多,提高了陶瓷材料的Q×f值,且调整了谐振频率温度系数。
本发明提供了一种铌酸盐系低温烧结微波介质陶瓷材料及其制备方法,得到的陶瓷材料在900~950℃烧结良好,其介电常数εr=32~35,Q×f=13000~21000GHz,谐振频率温度系数τf=-15~+6ppm/℃,可广泛应用于LTCC叠层微波器件中。
附图说明
图1为不同Zn取代含量(x=0.2,0.4,0.6,0.7,0.8)的样品的X-射线衍射(XRD)图谱;
图2为主晶相为Ni0.3Zn0.7TiNb2O8、不同玻璃添加量(1wt%,2wt%,3wt%,4wt%)的样品的X-射线衍射(XRD)图谱;
图3为主晶相为Ni0.3Zn0.7TiNb2O8、不同玻璃添加量(1wt%,2wt%,3wt%,4wt%),在950℃下烧结得到的样品的介电常数(εr)、品质因数(Q×f)和谐振频率温度系数性能(τf)曲线。
具体实施方式
下面结合附图和实施例,详述本发明的技术方案。
实施例
本发明提供的一种铌酸盐系低温烧结微波介质陶瓷材料,包括主晶相和占主晶相重量百分比为1%~4%的锌硼玻璃,所述主晶相为Ni1-xZnxTiNb2O8,其中,0.2≤x≤0.8;所述锌硼玻璃以其标准物计的含量为:ZnO 50mol%~70mol%,HBO330mol%~50mol%;所述主晶相中加入占主晶相重量百分比为1%~4%的锌硼玻璃,经球磨、烘干、造粒、干压成型过程后,在900~950℃下烧结6~12h,即得到所述铌酸盐系低温烧结微波介质陶瓷材料。
一种铌酸盐系低温烧结微波介质陶瓷材料的制备方法,包括以下步骤:
步骤1、主晶相的制备:以氧化锌(ZnO)、氧化亚镍(NiO)、二氧化钛(TiO2)、五氧化二铌(Nb2O5)为原料,按照分子式Ni1-xZnxTiNb2O8(x=0.7)的比例称料后以去离子水为球磨介质进行湿法球磨混合,球磨时间为8h,烘干后在850℃下、大气氛围中预烧6h,得到主晶相Ni0.3Zn0.7TiNb2O8;
步骤2、锌硼玻璃的制备:将ZnO和HBO3按照摩尔百分比为60mol%ZnO,40mol%HBO3的比例配料,采用去离子水为球磨介质,行星球磨10h后,烘干过筛,然后在1000℃下保温1~3h,在其熔融状态下快速倒入去离子中淬火得到透明玻璃体,研磨粉碎,得到锌硼玻璃;
步骤3、在步骤1得到的主晶相中加入占主晶相重量百分比为4%的步骤2得到的锌硼玻璃,以去离子水为球磨介质,湿法球磨混合6小时后烘干;
步骤4、在步骤3得到的粉料中加入占主晶相重量百分比为5%~12%的聚乙烯醇溶液作为粘结剂造粒,再干压成型,成型压力为200~300Mpa,然后在500℃下保温1~3h排胶,再在950℃下保温8h进行烧结处理,即可得到中介电常数铌酸盐的微波介质陶瓷材料。
图1为不同Zn取代含量(x=0.2,0.4,0.6,0.7,0.8)的样品的X-射线衍射(XRD)图谱,仅主晶相中的Zn取代含量不同,其他参数及条件与实施例一致;由图1可知,得到的样品中主要有Ni0.5Ti0.5NbO4和ZnTiNb2O8晶相,且随着Zn取代量的增加,ZnTiNb2O8所占比例增多。
图2为主晶相为Ni0.3Zn0.7TiNb2O8、不同玻璃添加量(1wt%,2wt%,3wt%,4wt%)的样品的X-射线衍射(XRD)图谱,仅玻璃的添加量不同,其余参数及条件与实施例一致;由图2可知,随着锌硼玻璃添加量的增加,ZnTiNb2O8晶相的含量增加。
图3为主晶相为Ni0.3Zn0.7TiNb2O8、不同玻璃添加量(1wt%,2wt%,3wt%,4wt%),在950℃下烧结得到的样品的介电常数(εr)、品质因数(Q×f)和谐振频率温度系数性能(τf)曲线;仅玻璃的添加量不同,其余参数及条件与实施例一致。由图3可知,随着锌硼玻璃添加量的增加,样品的介电常数和品质因数呈上升趋势,谐振频率温度系数呈下降趋势。因此,申请人通过大量实验,得出了本发明提供的主晶相及其占主晶相重量百分比为1%~4%的锌硼玻璃形成的陶瓷材料,同时具有较低的烧结温度(900~950℃),介电常数εr=32~35,Q×f=13000~21000GHz,谐振频率温度系数τf=-15~+6ppm/℃,可广泛应用于LTCC叠层微波器件中。
Claims (3)
1.一种铌酸盐系低温烧结微波介质陶瓷材料,包括主晶相和占主晶相重量百分比为1%~4%的锌硼玻璃,所述主晶相为Ni1-xZnxTiNb2O8,其中,0.2≤x≤0.8;所述锌硼玻璃以其标准物计的含量为:ZnO 50mol%~70mol%,HBO3 30mol%~50mol%;所述主晶相中加入占主晶相重量百分比为1%~4%的锌硼玻璃,经球磨、烘干、造粒、干压成型过程后,在900~950℃下烧结6~12h,即得到所述铌酸盐系低温烧结微波介质陶瓷材料。
2.根据权利要求1所述的铌酸盐系低温烧结微波介质陶瓷材料,其特征在于,所述锌硼玻璃的制备过程具体为:按照50mol%~70mol%ZnO,30mol%~50mol%HBO3的比例配料后,经4~10h球磨,加热至950~1000℃下保温1~3h,在其熔融状态下快速倒入去离子中淬火得到透明玻璃体,研磨粉碎,得到玻璃相助烧剂锌硼玻璃。
3.一种铌酸盐系低温烧结微波介质陶瓷材料的制备方法,包括以下步骤:
步骤1、主晶相的制备:以ZnO、NiO、TiO2、Nb2O5为原料,按照分子式Ni1-xZnxTiNb2O8的比例称料后进行湿法球磨混合,其中,0.2≤x≤0.8,球磨时间为8~24h,烘干后在850~1000℃下预烧6~16h,得到主晶相Ni1-xZnxTiNb2O8;
步骤2、锌硼玻璃的制备:将ZnO和HBO3按照摩尔百分比为50mol%~70mol%ZnO,30mol%~50mol%HBO3的比例配料,行星球磨4~10h后,烘干过筛,然后在950~1000℃下保温1~3h,在其熔融状态下快速倒入去离子中淬火得到透明玻璃体,研磨粉碎,得到锌硼玻璃;
步骤3、在步骤1得到的主晶相中加入占主晶相重量百分比为1%~4%的步骤2得到的锌硼玻璃,经球磨、烘干、造粒、干压成型过程后,得到的坯件在900~950℃下烧结6~12h,即得到所述铌酸盐系低温烧结微波介质陶瓷材料。
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