CN106083043A - 一种Li基低介低损耗LTCC材料及其制备方法 - Google Patents
一种Li基低介低损耗LTCC材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 13
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 13
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 10
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 5
- 229910015667 MoO4 Inorganic materials 0.000 claims abstract description 3
- 238000005516 engineering process Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
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- 238000005303 weighing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
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- 238000003475 lamination Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 238000009766 low-temperature sintering Methods 0.000 abstract description 6
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 238000010671 solid-state reaction Methods 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 8
- 229910000174 eucryptite Inorganic materials 0.000 description 5
- 238000004891 communication Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910010171 Li2MoO4 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
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- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- PPTSBERGOGHCHC-UHFFFAOYSA-N boron lithium Chemical compound [Li].[B] PPTSBERGOGHCHC-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
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- 239000003989 dielectric material Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
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- 239000006112 glass ceramic composition Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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Abstract
本发明属于微波电子陶瓷材料及其制造领域,具体涉及一种Li基低介电常数的LTCC材料及其制备方法。该材料按照Li2MoSi1+xO6+2x(‑0.2≤x≤0.2)化学计量,通过固相反应合成,最终得到包含两相的复合陶瓷,主晶相为菱方晶系的Li2MoO4,第二相为六方晶系的SiO2。其制备方法为以Li2CO3,MoO3及SiO2为原料,按照配比称取,通过球磨、烘料、煅烧、二次球磨、烘料、造粒、成型、排胶及烧结等一系列工艺过程,最终得到低介低损耗的Li基LTCC材料。该LTCC材料具有在低温烧结(≤900℃)条件下低介(≤5.0)低损耗(7137~14895GHz)的特征,在LTCC基板及集成器件中具有广阔的应用前景。
Description
技术领域
本发明属于微波电子陶瓷材料及其制造领域,具体涉及一种具有低介电常数和低损耗特性的Li基低温共烧陶瓷(Low Temperature Co-fired Ceramic,LTCC)材料及其制备方法。
背景技术
LTCC技术最初是由美国休斯公司开发的一种新材料技术,目前已被广泛用于各种国防军工、汽车及信息资讯产品中。LTCC技术可根据预先设计的电路结构,采用厚膜技术工艺实现材料基板、电极和无源器件等的一次烧成,在降低成本的同时,对封装的集成度、功能性和可靠性有大幅度提高。LTCC产品在军事、国防、商业及生活各领域中的应用非常广泛,如全球定位系统(GPS)、汽车电子、手机、蓝牙模块、数码相机、WLAN等。LTCC材料是LTCC技术中的重要核心,其不仅要求材料具有很好的介电或磁性能,而且必须要求能在<950℃的低温下烧结致密,并能与Ag电极材料实现匹配共烧,因此研发的难度较大。
低温烧结微波介质材料是LTCC材料领域中最重要的一个分支,其主要应用于各种LTCC微波基板和微波集成器件/组件中。目前,LTCC微波介质材料的类型主要可分为陶瓷、玻璃和玻璃陶瓷三大类,而介电常数则根据应用需求从低于10到超过100均有研究和应用报道。近年来,随着微波通信技术和雷达系统的发展,可利用的通信频率从微波扩展到毫米波。微波通信频率的高频化与传输速率的提高促进更低介电常数和更低介电损耗的新型LTCC材料研发。其中低介电常数的目的是降低电信号传输的延迟时间,低损耗要求的目的是为了降低能量散失和增强频率的选择性。但是,目前已报道的具有很低介电常数(介电常数通常低于6)的LTCC材料一般都是由玻璃或玻璃陶瓷材料类型构成,如Ferro公司著名的A6低介LTCC材料,其主成分为CaO-B2O3-SiO2的微晶玻璃,其它不少关于低介LTCC材料的报道,主成分也是由类似的微晶玻璃或由大量玻璃与陶瓷的复合体构成。这两种类型LTCC材料的优点是烧结温度低,甚至在800~850℃就能实现致密化。但不足之处一方面由于玻璃相过多,介电损耗相对较高。另一方面,过多的玻璃相容易引起LTCC器件或模块中银电极的扩散,对器件或模块电性能构成一定的影响。因此,研发具有低介电性能的陶瓷型的LTCC材料具有重要的意义。
常见的陶瓷类LTCC材料一般介电常数都比较高,只有硅酸盐系的LTCC微波介质陶瓷有望获得比较低的介电常数,近年来获得了比较多的关注和研究。Sang-HyoKweon等人(Low Temperature Sintering and Microwave Dielectric Properties of B2O3-addedLiAlSiO4Ceramics,J.Am.Ceram.Soc.94(2011)1995–1998.)研究了LiAlSiO4(主料:Li2CO3、Al2O3和SiO2)陶瓷的微波介电性能,研究发现在不添加任何助烧剂条件下,LiAlSiO4陶瓷需要在1350℃的高温下才能烧结,其介电常数为εr=4.8,Q×f=36000GHz,τf~8.0ppm/℃。因此,LiAlSiO4虽然具有良好的性能,但是很难实现低温共烧,在烧结过程需添加助烧剂。当添加大量(12mol%)的B2O3时,样品可在950℃下烧成,且εr=5.3,Q×f=212 000GHz,τf=-7.7ppm/℃。可以看出,在添加助烧剂后,LiAlSiO4烧结温度降低,但同时性能也受到了一定影响,介电常数增大,Q×f降低,并且游离的B2O3在LTCC后期流延工艺过程中易水解,使陶瓷成分不稳定,进一步导致其性能的恶化。Sumesh George等人通过在Li2MgSiO4(主料:Li2CO3、(MgCO3)4·Mg(OH)2·5H2O和SiO2)陶瓷中掺杂硼硅酸锂(lithium borosilicate,LBS)玻璃,在925℃烧结下实现εr为5.5以及tanδ为7×10-5的性能(Low-TemperatureSintering and Microwave Dielectric Properties of Li2MgSiO4Ceramics,J.Am.Ceram.Soc.,92,1244,2009)。总体而言,目前已报道的陶瓷类的低介微波陶瓷材料要么烧结温度还太高,难以降到与LTCC工艺兼容的900℃或以下,要么介电常数偏高,难以实现低于5.0的低介电常数。
发明内容
针对目前低介陶瓷类LTCC材料研发中存在的问题或不足,为实现介电常数低于5.0,用于LTCC工艺的低温烧结陶瓷材料,及其优异的性能参数,本发明提供了一种Li基低介低损耗LTCC材料及其制备方法。尤其适用于具有高传输速率、低信号延迟的LTCC微波基板和器件应用的需要。
该Li基低介低损耗LTCC材料,其配方为Li2CO3、MoO3和SiO2按照Li2MoSi1+xO6+2x(x=-0.2~0.2)化学计量称量,原料组成按照摩尔比Li2CO3:MoO3:SiO2=1:1:0.8~1.2,主晶相为菱方晶系的Li2MoO4,第二相为六方晶系的SiO2。
其烧结温度为800~900℃,对应介电常数5.00~4.33,Q×f值7137~14895GHz。可广泛应用于LTCC基板、叠层微波器件和模块中。
其制备方法如下:
步骤1:按照摩尔比Li2CO3:MoO3:SiO2=1:1:0.8~1.2称料配置原料;将配好的原料进行一次球磨使原料混合均匀,球磨工艺为:以无水乙醇为球磨介质,转速为250~300rpm,球磨时间为4~12h,球磨完将粉料烘干备用;
步骤2:将步骤1所得的烘干粉料放入坩埚中压实,按2~5℃/min的升温速率升至700℃进行预烧,保温3~5h,随炉冷却得到预烧料,并放入球磨罐中进行二次球磨,球磨工艺同一次球磨,球磨完成后烘干备用;
步骤3:将步骤2所得粉料添加入20wt%~30wt%的PVA溶液,浓度8~12wt%,作为粘结剂,进行造粒并在8-12MPa干压成型;
步骤4:将步骤3所得产物放入烧结炉中,按2~5℃/min的升温速率升至100℃并保温2~3h,再继续升温至400~600℃并保温3~6h,然后随炉冷却至室温,获得排胶后的生坯;
步骤5:将步骤4所得生坯再放入烧结炉中,按2~5℃/min的升温速率升至800℃~900℃进行烧结,并保温3~6h,后随炉冷却至室温,获得Li基低介电常数的LTCC微波介电陶瓷。
本发明中Li基低介低损耗LTCC材料,介电常数5.00~4.33,Q×f值7137~14895GHz。在800℃~900℃低温烧结就可实现致密化,晶相为Li2MoO4和SiO2的混合陶瓷相,同时该材料无需再添加任何玻璃相的助烧剂来进行助烧即可实现低温烧结,因而能够很好的抑制Ag电极在LTCC材料中的扩散,可广泛应用于LTCC基板、叠层微波器件和模块中,在LTCC技术领域具有很高的应用价值。
附图说明
图1为本发明的制备工艺流程图;
图2为实施例烧结样品的X-射线衍射(XRD)图谱;
图3为实施例烧结样品的扫描电子显微镜(SEM)图;
图4为实施例烧结样品的性能图。
具体实施方式
下面所述为本发明的LTCC微波介电陶瓷材料的具体实施例。其具体制备方法如下:
步骤1:按照摩尔比Li2CO3:MoO3:SiO2=1:1:1称料配置原料;将配好的原料进行一次球磨使原料混合均匀,球磨工艺为:无水乙醇为球磨介质,转速为300rpm,球磨时间为4h,球磨完将所得粉料烘干备用;
步骤2:将步骤1所得的烘干后结块的粉料在研钵中捣碎,放入坩埚中压实,按2℃/min的升温速率升至700℃进行预烧,保温4h后随炉冷却至室温得到预烧料,并放入球磨罐中进行二次球磨,球磨工艺同步骤1球磨,球磨完将所得粉料烘干备用;
步骤3:将步骤2所得粉料加入20wt%的PVA溶液,浓度10wt%,作为粘结剂,进行造粒并在10MPa下干压成型为6mm厚的圆柱生坯;
步骤4:将步骤3所得生坯放入高温烧结炉中,按2℃/min的升温速率升至100℃并保温2h,再继续升温至600℃并保温5h,然后随炉冷却至室温,获得排胶后的生坯;
步骤5:将步骤4所得排胶后的生坯放入高温烧结炉中,按2℃/min的升温速率分别升温至800℃,850℃,900℃进行烧结,并保温4h,后随炉冷却至室温,获得前述3种烧结温度的Li基低介低损耗的LTCC微波介电陶瓷。
图2为不同烧结温度的样品XRD图谱。从图中可以看出样品含有Li2MoO4和SiO2两相的特征峰。
图3为不同烧结温度的样品SEM图谱。从图中可以看出样品在800和850℃下烧结时明显存在两种不同大小的晶粒分布,随着温度升高,晶粒逐渐长大,结晶度增加。当烧结温度达到900℃时,结晶度最佳。
图4为不同烧结温度的样品介电常数(εr)和品质因数(Q×f),从图中可以看出,随着烧结温度的增加,介电常数逐渐减小,但品质因数逐渐减小。
Claims (4)
1.一种Li基低介低损耗LTCC材料,其特征在于:原料配方为Li2CO3、MoO3和SiO2按照Li2MoSi1+xO6+2x,-0.2≤x≤0.2,化学计量称量,组成按照摩尔比Li2CO3:MoO3:SiO2=1:1:0.8~1.2,主晶相为菱方晶系的Li2MoO4,第二相为六方晶系的SiO2。
2.如权利要求1所述Li基低介低损耗LTCC材料,其特征在于:烧结温度为800~900℃,对应介电常数5.00~4.33,Q×f值7137~14895GHz。
3.如权利要求1所述Li基低介低损耗LTCC材料,其特征在于:应用于LTCC基板、叠层微波器件和模块中。
4.如权利要求1所述Li基低介低损耗LTCC材料,其制备方法如下:
步骤1、按照摩尔比Li2CO3:MoO3:SiO2=1:1:0.8~1.2称料配置原料;将配好的原料进行一次球磨使原料混合均匀;球磨工艺为:以无水乙醇为球磨介质,转速为250~300rpm,球磨时间为4~12h,球磨完将所得粉料烘干备用;
步骤2、将步骤1所得的烘干粉料放入坩埚中压实,按2~5℃/min的升温速率升至700℃进行预烧,保温3~5h,随炉冷却得到预烧料,并放入球磨罐中进行二次球磨,球磨工艺同步骤1球磨,球磨完将所得粉料烘干备用;
步骤3、将步骤2所得粉料添加入20wt%~30wt%的PVA溶液,浓度8~12wt%,作为粘结剂,进行造粒并在8-12MPa干压成型;
步骤4、将步骤3所得产物放入烧结炉中,按2~5℃/min的升温速率升至100℃并保温2~3h,再继续升温至400~600℃并保温3~6h,然后随炉冷却至室温,获得排胶后的生坯;
步骤5、将步骤4所得生坯放入烧结炉中,按2~5℃/min的升温速率升至800℃~900℃进行烧结,并保温3~6h,后随炉冷却至室温,即获得Li基低介低损耗LTCC材料。
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