CN111320473B - 一种低烧微波介质陶瓷材料及其制备方法 - Google Patents
一种低烧微波介质陶瓷材料及其制备方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 36
- 238000005245 sintering Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 238000010304 firing Methods 0.000 claims abstract description 11
- 229910004283 SiO 4 Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000003985 ceramic capacitor Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 2
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 239000003989 dielectric material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000009766 low-temperature sintering Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004891 communication Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 229910021523 barium zirconate Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于微波介质材料技术领域,具体涉及一种BaZrO3体系低温烧结低介电常数C0G微波介质材料及其制备方法。本发明所述低烧微波介质陶瓷材料,以BaZrO3、Mg2SiO4为基础,通过掺杂选定组分和配比的改性添加剂和助烧剂进行制备,所得微波介质陶瓷材料的介电常数可做到12‑16,Q*f值:30000‑50000,尤其是材料的烧结温度可以达到950℃以下,其TCC符合C0G规格,具有较好的低温烧结性,可用于MLCC、微波天线等微波器件的制造。
Description
技术领域
本发明属于微波介质材料技术领域,具体涉及一种BaZrO3体系低温烧结低介电常数C0G微波介质材料及其制备方法。
背景技术
微波介质陶瓷是指应用于微波频段(主要是UHF、SHF频段,
300MHz-300GHz)电路中作为介质材料并完成一种或多种功能的陶瓷,其具有高介电常数、低介电损耗、低谐振频率温度系数等优良性能,是谐振器、滤波器、双工器、天线、稳频振荡器、波导传输线等器件的重要组成元件,可广泛应用于个人便携式移动电话、微波基站、车载电话、卫星通讯、军用雷达等众多领域。尤其是近年来,随着通讯技术的迅速发展,对微波器件的需求量也日益增长,特别是5G通信时代基站数量增加导致滤波器需求增加,陶瓷介质滤波器由于具有高Q值、选频特性好、工作频率稳定性好、插入损耗小及更加小型化和集成化等优势而受到越来越多的关注,这成为近年来国内外对微波介质材料研究领域的一个热点方向。
随着微波通讯技术的发展,对元器件的小型化、集成化以及模块化的要求也越来越迫切,微波陶瓷电容器是目前世界上用量最大、发展最快的电子元件之一。微波陶瓷电容器主要应用于各类军用民用整机的震荡、耦合、滤波、旁路电路中,应用领域已经拓展到自动控制仪表、计算机、手机、数字家电、汽车、电力等行业。目前,微波陶瓷电容器已经成为了电容器市场的重要组成,全球市场的需求量增长速度近15%,不仅市场需求巨大,且产业化市场前景非常广阔。
以微波片式多层陶瓷电容器而言,目前国际上多采用中、高烧体系(烧温>1100℃)的微波介质陶瓷材料匹配银钯内电极浆料进行制造生产。虽然电容器性能可以满足要求,但鉴于选用的微波介质材料需要在中、高温体系下才能完成烧结制造,造成整个工艺能耗较大,进而影响成本较高。
发明内容
为此,本发明所要解决的技术问题在于提供一种以BaZrO3、Mg2SiO4为主料的低温烧结低介电常数的C0G微波介质陶瓷材料,该陶瓷能够在较低温度烧结下,并且具有良好介电性能的同时温度系数满足C0G规格;
本发明所要解决的第二个技术问题在于提高上述微波介质陶瓷材料的制备方法和应用。
为解决上述技术问题,本发明所述的一种低烧微波介质陶瓷材料,以所述微波介质陶瓷材料的制备原料总量计,包括如下质量含量的组分:
具体的,所述改性添加剂包括Mn、Co、Al、Ca和/或Ti的氧化物和/或碳酸盐。优选的,所述改性添加剂包括MnCO3、CoO、Al2O3、CaCO3、TiO2中的一种或几种。
更优选的,所述改性添加剂包括:
具体的,所述助烧剂包括Li、Zn、Bi、B、Si和/或Mg的氧化物和/或碳酸盐。优选的,所述的烧结助剂包括LiOH、ZnO、Bi2O3、H3BO3、SiO2、MgO的一种或几种。
更优选的,所述助烧剂以其总量计,包括如下质量含量的组分:
本发明还公开了一种制备所述低烧微波介质陶瓷材料的方法,包括如下步骤:
(1)取选定成分和含量的所述助烧剂干混混匀,经玻璃熔炉熔制1200-1300℃,保温0.5-2h,将淬火处理后的玻璃研磨成粉体,备用;
(2)取选定含量的所述BaZrO3、Mg2SiO4、改性添加剂和助烧剂混合并进行球磨处理,并加入胶液进行喷雾造粒,即得所需低烧微波介质陶瓷材料。
具体的,所述低烧微波介质陶瓷材料的制备方法,还包括制备所述BaZrO3的步骤,具体包括以BaCO3、ZrO2按摩尔比1:1的比例球磨混合均匀后,于1000-1200℃进行煅烧2-5小时的步骤。
具体的,所述低烧微波介质陶瓷材料的制备方法,还包括制备所述Mg2SiO4的步骤,具体包括以Mg(OH)2、SiO2按摩尔比2:1的比例球磨混合均匀后,于1000-1200℃进行煅烧3-5小时的步骤。
具体的,所述胶液包括PVA胶液和/或丙烯酸胶液。
本发明还公开了一种微波陶瓷电容器,其特征在于,由所述低烧微波介质陶瓷材料制得。
本发明还公开了一种制备所述微波陶瓷电容器的方法,包括将所述低烧微波介质陶瓷材料经干压成型后于900-930℃进行烧结2-8h的步骤。
本发明所述低烧微波介质陶瓷材料,以BaZrO3、Mg2SiO4为基础,通过掺杂选定组分和配比的改性添加剂和助烧剂进行制备,所得微波介质陶瓷材料的介电常数可做到12-16,Q*f值:30000-50000,尤其是材料的烧结温度可以达到950℃以下,其TCC符合C0G规格,具有较好的低温烧结性,可用于MLCC、微波天线等微波器件的制造。
具体实施方式
按照摩尔比1:1取BaCO3和ZrO2球磨混合均匀后,在1100℃煅烧4小时,制得所需BaZrO3。
按照摩尔比2:1取Mg(OH)2和SiO2球磨混合均匀后,在1150℃煅烧4小时,制得所需Mg2SiO4。
分别按照下表1中列明的含量取所述BaZrO3和Mg2SiO4,并加入如下表1所述组分及含量的改性添加剂和助烧剂混合,并进行球磨处理;将球磨后的物料加入丙烯酸胶液(胶含量5wt%),采用喷雾干燥机进行喷雾造粒,控制进口温度210±10℃,出口温度130±10℃,即得所需低烧微波介质陶瓷材料。
所述助烧剂为按照如下表1中选定成分和含量组分混匀,经玻璃熔炉熔制1200℃,保温2h后淬火处理制得,并研磨成粉体。
表1低烧微波介质陶瓷材料的成分及用量表(kg)
实验例
将上述造粒后的物料分别进行干压成型,并分别将压制的生坯进行保温煅烧3h,并记录可使各材料生坯成型的烧结温度。
分别对上述实施例1-5及对比例1-4中制得的微波介质陶瓷材料进行性能测试,具体包括材料的介电常数、25℃的f*Q值、以及频率温度系数τf;
所述介电常数、25℃的f*Q值采用现有技术已知方法即可;
所述频率温度系数τf代表具有良好的温度特性,通过分别测试-40℃、25℃、110℃时的共振频率f,并按照如下公式计算:
τf=[(f110℃-f-40℃)/f25℃]/150*106(ppm/℃)。
测定及计算结果见下表2。
表2微波介质陶瓷材料的性能测试结果
编号 | f*Q(GHz) | τf(ppm/℃)(-40℃-110℃) | 介电常数 | 烧结温度(℃) |
实施例1 | 50363 | -8.53 | 12.25 | 915 |
实施例2 | 32761 | -0.39 | 15.86 | 915 |
实施例3 | 48623 | -6.55 | 13.47 | 915 |
实施例4 | 39462 | -7.01 | 13.21 | 915 |
实施例5 | 37596 | -4.63 | 14.62 | 915 |
对比例1 | 200 | 150 | 40 | 1550 |
对比例2 | 185 | 87 | 36 | 1150 |
对比例3 | 163093 | -57.82 | 7 | 1450 |
对比例4 | 124231 | -44.62 | 6.51 | 1150 |
可见,本发明所述复合微波介质陶瓷材料品质因数较高,介电常数在12-16左右,25℃的f*Q值为30000-50000,尤其是材料的烧结温度仅为950℃以下,其TCC符合C0G规格,低温烧结性能大幅提升,可以大批稳定生产,可用于MLCC、微波天线等微波器件的制造。
显然,上述实施例仅仅是为清楚地说明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (6)
1.一种低烧微波介质陶瓷材料,其特征在于,以所述微波介质陶瓷材料的制备原料总量计,由如下质量含量的组分组成:
BaZrO3 40-70wt%;
Mg2SiO4 10-40wt%;
改性添加剂 0.5-10wt%;
助烧剂 5-20wt%;其中,
所述改性添加剂由如下组分组成:
MnCO3 0.3-1.0wt%;
Al2O3 0.05-0.3wt%;
CoO 0.05-0.5wt%;
CaCO3 1-5wt%;
TiO2 1-5wt%;
所述助烧剂以其总量计,由如下质量含量的组分组成:
LiOH 10-40wt%;
ZnO 15-45wt%;
Bi2O3 0-5wt%;
H3BO3 5-15wt%;
SiO2 10-20wt%;
MgO 1-5wt%。
2.一种制备权利要求1所述低烧微波介质陶瓷材料的方法,其特征在于,包括如下步骤:
(1)取选定成分和含量的所述改性添加剂混匀,经熔制及淬火处理后,研磨成粉体,备用;
(2)取选定成分和含量的所述助烧剂混匀,经熔制及淬火处理后,研磨成粉体,备用;
(3)取选定含量的所述BaZrO3、Mg2SiO4、改性添加剂和助烧剂混合并进行球磨处理,并加入胶液进行喷雾造粒,即得所需低烧微波介质陶瓷材料。
3.根据权利要求2所述低烧微波介质陶瓷材料的制备方法,其特征在于,还包括制备所述BaZrO3的步骤,具体包括以BaCO3、ZrO2 按摩尔比1:1的比例球磨混合均匀后,于1000-1100℃进行煅烧2-5小时的步骤。
4.根据权利要求2或3所述低烧微波介质陶瓷材料的制备方法,其特征在于,还包括制备所述Mg2SiO4的步骤,具体包括以Mg(OH)2、SiO2 按摩尔比2:1的比例球磨混合均匀后,于1000-1200℃进行煅烧3-5小时的步骤。
5.一种微波陶瓷电容器,其特征在于,由权利要求1所述低烧微波介质陶瓷材料制得。
6.一种制备权利要求5所述微波陶瓷电容器的方法,其特征在于,包括将权利要求1所述低烧微波介质陶瓷材料经干压成型后于900℃-930℃进行烧结2-8h的步骤。
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