CN106904960B - 一种Mg2SiO4-Li2TiO3复合体系LTCC材料及其制备方法 - Google Patents
一种Mg2SiO4-Li2TiO3复合体系LTCC材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 229910007848 Li2TiO3 Inorganic materials 0.000 claims abstract description 18
- 229910052839 forsterite Inorganic materials 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 34
- 238000000498 ball milling Methods 0.000 claims description 32
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
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- 239000002994 raw material Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
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- 229910052681 coesite Inorganic materials 0.000 claims description 5
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- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 229910010252 TiO3 Inorganic materials 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
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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Mg2SiO4‑Li2TiO3复合体系LTCC材料及其制备方法。本发明提供的LTCC材料，基于Mg2SiO4和Li2TiO3复合体系，通过固相法获得；实现烧结温度800～950℃低于960℃(Ag熔点)，εr＝9.0～18.0，且具有50,000～250,000GHz的高Qf值和近零τf＝‑15～15ppm/℃，在LTCC技术领域具有很高的应用前景和价值。可广泛应用于LTCC基板、叠层微波器件和模块中。
Description
技术领域
本发明属于微波电子陶瓷材料及其制造领域，涉及一种具有谐振频率温度系数近零(τf～ 0ppm/℃)和高Qf值特性的低温共烧陶瓷(Low Temperature Co-fired Ceramic，LTCC)材料及其制备方法，具体为一种Mg2SiO4-Li2TiO3复合体系LTCC材料及其制备方法。
背景技术
随着微电子技术的发展，LTCC技术受到广泛关注。LTCC技术广泛用于国防军工、汽车及信息资讯产品中。其最大的特点是LTCC材料能在低烧结温度(<960℃)下烧结。
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。微波通信频率的高端化及大的信息传输量要求开发高Qf值和趋于零的τf值。高Qf值是为了降低能量散失和增强频率选择性，趋于零的τf值是为了保证频率的稳定性。
Mg2SiO4微波介电陶瓷由于具有高Qf值被广泛研究。Ohsato等(Ohsato H,TsunookaT, Sugiyama T,et al.Forsterite ceramics for millimeterwave dielectrics[J].Journal of Electroceramics, 2006,17(2):445-450)对Mg2SiO4介电性能进行了研究，研究发现Mg2SiO4微波介电陶瓷具有高Qf值(～270,000GHz)。但其烧结温度高(～1450℃)，且谐振频率温度系数τf偏离零较大 (～-67ppm/℃)。使其不能满足LTCC应用需求。
Li2TiO3微波介电陶瓷具有较低烧结温度和谐振频率正温度系数。Bian等(Bian JJ,Dong Y F.New high Q microwave dielectric ceramics with rock saltstructures:(1-x)Li2TiO3+xMgO system(0≤x≤0.5)[J].Journal of the EuropeanCeramic Society,2010,30(2):325-330)研究发现Li2TiO3在1300℃下烧结，其介电性能：εr～22，Qf～65,000GHz，τf～20ppm/℃。同样由于其烧结温度高，且谐振频率温度系数τf偏离零较大使其不能满足于LTCC应用需求。将两种正负τf的微波介电材料进行复合，可得到近零τf的微波介电复合陶瓷。再添加一定的助烧剂可实现低温烧结，同时获得高Qf值和温度稳定型的LTCC材料。
发明内容
针对上述存在问题或不足，本发明提供了一种Mg2SiO4-Li2TiO3复合体系LTCC材料及其制备方法，该材料能在低温(800～950℃)烧结实现致密化，且介电常数在9～18间可调，使其在LTCC集成基板和器件中具有良好的应用前景。
该温度稳定型高Qf值LTCC材料，包含Mg2SiO4、LiTiO2和Li2TiSiO5三相，化学通式为(1-x)Mg2SiO4–xLi2TiO3-yLiF，其中x(0.35～0.85)，y(6～10wt％)；
Mg2SiO4的原料组成为：MgO和SiO2按摩尔比MgO:SiO2＝2:1配料；Li2TiO3的原料组成为：Li2CO3和TiO2按摩尔比Li2CO3:TiO2＝2:1配料；LiF为助烧剂，所占比例y为Mg2SiO4与Li2TiO3之和质量百分比。
其烧结温度为800～950℃，εr＝9.0～18.0，Q×f值50,000～250,000GHz，τf＝-15～15ppm/℃。
上述LTCC材料的具体制备方法如下：
步骤1、将分析纯的MgO和SiO2按摩尔比MgO:SiO2＝2:1配料；然后将其进行一次球磨使配料混合均匀，按照配料与去离子水质量比1:0.8～1.5加入去离子水，在球磨转速250～300 rpm下，球磨4～12h，球磨后将所得粉料在100～120℃下烘干备用。
步骤2、将步骤1所得的烘干粉料过40～100目筛网，过筛后放入坩埚中压实，按2～5℃/min 的升温速率升至1150～1350℃进行预烧，保温3～5h，随炉冷却得到Mg2SiO4预烧料。
步骤3、将分析纯的Li2CO3和TiO2按摩尔比Li2CO3:TiO2＝2:1配料；将配好的原料进行一次球磨使配料混合均匀，按照配料与去离子水质量比1:0.8～1.5加入去离子水，在球磨转速 250～300rpm下，球磨4～12h，球磨后将所得粉料在100～120℃下烘干备用。
步骤4、将步骤3所得的烘干粉料过40～100目筛网，过筛后放入坩埚中压实，按2～5℃/min 的升温速率升至800～900℃进行预烧，保温3～5h，随炉冷却得到Li2TiO3预烧料。
步骤5、将步骤2和步骤4得到预烧料以及LiF，按照(1-x)Mg2SiO4–xLi2TiO3-yLiF配比进行称量配料，其中x＝0.35～0.85，y＝6～10wt％；然后按照配料与去离子水质量比1:0.8～1.5 加入去离子水，在球磨转速250～300rpm下，球磨4～12h，球磨后将粉料在100～120℃下烘干备用。
步骤6、将步骤5所得烘干粉料添加入占其20wt％～30wt％的PVA溶液作为粘结剂，进行造粒并在6～10MPa单轴干压成型。
步骤7、将步骤6所得产物放入烧结炉中，按2～5℃/min的升温速率升至400～600℃排胶3～6h，然后随炉冷却至室温，获得排胶后的生坯样品。
步骤8、将步骤7所得生坯样品再放入烧结炉中，按2～5℃/min的升温速率升至800℃～950 ℃进行烧结，并保温3～6h，后随炉冷却至室温，即可获得温度稳定型高Qf值LTCC材料。
所述步骤6中PVA溶液的浓度为8～10wt％。
本发明提供的LTCC材料，基于Mg2SiO4和Li2TiO3复合体系，通过固相法获得；实现烧结温度800～950℃低于960℃(Ag熔点)，εr＝9.0～18.0，且具有50,000～250,000GHz的高Qf 值和近零τf＝-15～15ppm/℃，在LTCC技术领域具有很高的应用前景和价值。可广泛应用于 LTCC基板、叠层微波器件和模块中。
附图说明
图1为样品在850℃烧结下的X-射线衍射(XRD)图谱；
图2为样品在850℃烧结下的介电性能图。
具体实施方式
下面以实施例结合附图对本发明做进一步的详细说明。
步骤1：将分析纯的MgO和SiO2按摩尔比MgO:SiO2＝2:1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，按照粉料与去离子水质量比1:1加入去离子水，在球磨转速 300rpm下，球磨4h。球磨完将粉料在120℃下烘干备用。
步骤2：将步骤1所得的烘干粉料过60目筛网，过筛后放入坩埚中压实，按2℃/min的升温速率升至1350℃进行预烧，保温4h，随炉冷却得到Mg2SiO4预烧料。
步骤3：将分析纯的Li2CO3和TiO2按摩尔比Li2CO3:TiO2＝2:1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，按照粉料与去离子水质量比1:1加入去离子水，在球磨转速300rpm下，球磨4h。球磨完将粉料在120℃下烘干备用。
步骤4：将步骤3所得的烘干粉料过60目筛网，过筛后放入坩埚中压实，按2℃/min的升温速率升至900℃进行预烧，保温4h，随炉冷却得到Li2TiO3预烧料。
步骤5：将步骤2和步骤4得到预烧料按照(1-x)Mg2SiO4–xLi2TiO3-yLiF(其中x＝0.35～0.85， y＝6～10wt％)配比进行称量；按照配得粉料与去离子水质量比1:1加入去离子水，在球磨转速300rpm下，球磨4h。球磨完将粉料在120℃下烘干备用。
步骤6：将步骤5所得粉料添加入占其20wt％的PVA溶液作为粘结剂，进行造粒并在10MPa单轴干压成直径×厚度＝12mm×6mm圆柱；
步骤7：将步骤6所得产物放入烧结炉中，按2℃/min的升温速率升至600℃排胶4h，然后随炉冷却至室温，获得排胶后的生坯样品；
步骤8：将步骤7所得生坯样品再放入烧结炉中，按2℃/min的升温速率升至850℃进行烧结，并保温4h，后随炉冷却至室温，获得温度稳定型高Qf值的LTCC材料。
实施例选取了当x＝0.35，0.45，0.55，0.65，0.75和0.85的值。
图1为850℃烧结时，实施例x不同取值对应的XRD图谱。从图中可以看出样品含有Mg2SiO4、LiTiO2和Li2TiSiO5三相的特征峰。
图2为850℃烧结时，实施例x不同取值对应的εr值、Qf值和τf值。
从实施例可见，本发明提供的LTCC材料，基于Mg2SiO4和Li2TiO3复合体系，通过固相法获得；实现烧结温度800～950℃低于960℃(Ag熔点)，且具有高Qf值和近零τf，在LTCC技术领域具有很高的应用前景和价值。
Claims (3)
1.一种Mg2SiO4-Li2TiO3复合体系LTCC材料，其特征在于：包含Mg2SiO4、LiTiO2和Li2TiSiO5三相，其化学通式为(1-x)Mg2SiO4–xLi2TiO3-yLiF，x＝0.35～0.85，y＝6～10wt％；
Mg2SiO4的原料组成为：MgO和SiO2按摩尔比MgO:SiO2＝2:1；
Li2TiO3的原料组成为：Li2CO3和TiO2按摩尔比Li2CO3:TiO2＝2:1；
LiF为助烧剂，所占比例y为Mg2SiO4与Li2TiO3之和质量百分比；
烧结温度为800～950℃，εr＝9.0～18.0，Q×f值50,000～250,000GHz，τf＝-15～15ppm/℃。
2.如权利要求1所述Mg2SiO4-Li2TiO3复合体系LTCC材料的制备方法，包括以下步骤：
步骤1、将分析纯的MgO和SiO2按摩尔比MgO:SiO2＝2:1配料；然后将其进行一次球磨使配料混合均匀，按照配料与去离子水质量比1:0.8～1.5加入去离子水，在球磨转速250～300rpm下，球磨4～12h，球磨后将所得粉料在100～120℃下烘干备用；
步骤2、将步骤1所得的烘干粉料过40～100目筛网，过筛后放入坩埚中压实，按2～5℃/min的升温速率升至1150～1350℃进行预烧，保温3～5h，随炉冷却得到Mg2SiO4预烧料；
步骤3、将分析纯的Li2CO3和TiO2按摩尔比Li2CO3:TiO2＝2:1配料；将配好的原料进行一次球磨使配料混合均匀，按照配料与去离子水质量比1:0.8～1.5加入去离子水，在球磨转速250～300rpm下，球磨4～12h，球磨后将所得粉料在100～120℃下烘干备用；
步骤4、将步骤3所得的烘干粉料过40～100目筛网，过筛后放入坩埚中压实，按2～5℃/min的升温速率升至800～900℃进行预烧，保温3～5h，随炉冷却得到Li2TiO3预烧料；
步骤5、将步骤2和步骤4得到预烧料以及LiF，按照(1-x)Mg2SiO4–xLi2TiO3-yLiF配比进行称量配料，其中x＝0.35～0.85，y＝6～10wt％；然后按照配料与去离子水质量比1:0.8～1.5加入去离子水，在球磨转速250～300rpm下，球磨4～12h，球磨后将粉料在100～120℃下烘干备用；
步骤6、将步骤5所得烘干粉料添加入占其20wt％～30wt％的PVA溶液作为粘结剂，进行造粒并在6～10MPa单轴干压成型；
步骤7、将步骤6所得产物放入烧结炉中，按2～5℃/min的升温速率升至400～600℃排胶3～6h，然后随炉冷却至室温，获得排胶后的生坯样品；
步骤8、将步骤7所得生坯样品再放入烧结炉中，按2～5℃/min的升温速率升至800℃～950℃进行烧结，并保温3～6h，后随炉冷却至室温，即可获得Mg2SiO4-Li2TiO3复合体系LTCC材料。
3.如权利要求2所述Mg2SiO4-Li2TiO3复合体系LTCC材料的制备方法，其特征在于：所述步骤6中PVA溶液的浓度为8～10wt％。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4632534B2 (ja) * | 2000-12-27 | 2011-02-16 | 京セラ株式会社 | 誘電体磁器及びその製造方法 |
| CN102674828A (zh) * | 2012-05-16 | 2012-09-19 | 桂林电子科技大学 | 一种低介电损耗温度稳定型微波介电陶瓷材料及其制备方法 |
| CN103274688A (zh) * | 2013-05-31 | 2013-09-04 | 上海大学 | 无玻璃相的两相复合微波介质陶瓷材料Li2TiO3-Li2WO4的制备方法 |
| CN105801119A (zh) * | 2016-05-11 | 2016-07-27 | 电子科技大学 | 一种微波介电ltcc材料及其制备方法 |
| CN105801109A (zh) * | 2016-04-01 | 2016-07-27 | 桂林理工大学 | 低损耗温度稳定型低介电常数微波介电陶瓷Li2Mg2TiO5 |
| CN106116550A (zh) * | 2016-06-26 | 2016-11-16 | 桂林理工大学 | 一种硅酸盐Li2SiO3作为温度稳定型高品质因数微波介电陶瓷的应用 |
-
2017
- 2017-03-14 CN CN201710149952.3A patent/CN106904960B/zh not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4632534B2 (ja) * | 2000-12-27 | 2011-02-16 | 京セラ株式会社 | 誘電体磁器及びその製造方法 |
| CN102674828A (zh) * | 2012-05-16 | 2012-09-19 | 桂林电子科技大学 | 一种低介电损耗温度稳定型微波介电陶瓷材料及其制备方法 |
| CN103274688A (zh) * | 2013-05-31 | 2013-09-04 | 上海大学 | 无玻璃相的两相复合微波介质陶瓷材料Li2TiO3-Li2WO4的制备方法 |
| CN105801109A (zh) * | 2016-04-01 | 2016-07-27 | 桂林理工大学 | 低损耗温度稳定型低介电常数微波介电陶瓷Li2Mg2TiO5 |
| CN105801119A (zh) * | 2016-05-11 | 2016-07-27 | 电子科技大学 | 一种微波介电ltcc材料及其制备方法 |
| CN106116550A (zh) * | 2016-06-26 | 2016-11-16 | 桂林理工大学 | 一种硅酸盐Li2SiO3作为温度稳定型高品质因数微波介电陶瓷的应用 |
Non-Patent Citations (1)
| Title |
|---|
| 低温烧结硅酸镁陶瓷及其微波介电性能研究;杨桃;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20160215;第B015-296页 * |
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