CN113087507A - 低介硅酸镁微波介质陶瓷材料及其制备方法 - Google Patents
低介硅酸镁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 23
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000391 magnesium silicate Substances 0.000 title claims abstract description 22
- 229910052919 magnesium silicate Inorganic materials 0.000 title claims abstract description 22
- 235000019792 magnesium silicate Nutrition 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title description 10
- 239000000654 additive Substances 0.000 claims abstract description 35
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000000996 additive effect Effects 0.000 claims abstract description 28
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052909 inorganic silicate Inorganic materials 0.000 claims abstract description 25
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910002971 CaTiO3 Inorganic materials 0.000 claims abstract description 18
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 10
- 239000000919 ceramic Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 15
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims 2
- 230000035939 shock Effects 0.000 abstract description 7
- 238000004891 communication Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明适用于介质陶瓷技术领域，公开了一种低介硅酸镁微波介质陶瓷材料，包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为Al2O3、Bi2O3、CaTiO3、TiO2、ZrO2、SnO2、Sm2O3、B2O3、LiF中的至少两个的组合。还提供了一种制备所述低介硅酸镁微波介质陶瓷材料的方法。本发明的低介硅酸镁微波介质陶瓷材料具有高抗热震、介电常数可调、高品质因数和近零的谐振频率温度系数的优点。
Description
技术领域
本发明涉及介质陶瓷技术领域，尤其涉及一种低介硅酸镁微波介质陶瓷材料及其制备方法。
背景技术
随着通信技术的发展，5G通信逐渐实现商业化，5G信号与4G信号相比显著特点是信号传输速度更快(传输速度为4G的10-100倍)，将会极大的方便了人们的生活。5G通信一般采用3Ghz以上的频谱，波长很短，容易受到自金属的干扰；而开发微波陶瓷是进军5G时代的一个重要选择，尤其是在应用于谐振器、天线、滤波器等微波器件的制造。
微波介质陶瓷材料在使用中需要较高的Q×f(品质因数)值、近零的谐振频率温度系数、良好的抗热震性能；若陶瓷抗热震性差，可能会遭受环境温度骤变(热震)而产生裂纹，甚至失效。因此，如何制备出一种满足于现有通信器件需求的微波介质陶瓷材料，是现有技术所面临的技术问题。
发明内容
针对上述的缺陷，本发明的目的在于提供一种具有高抗热震、介电常数可调、高品质因数和近零的谐振频率温度系数的低介硅酸镁微波介质陶瓷材料及其制备方法。
本发明通过以下技术方案实现：
一种低介硅酸镁微波介质陶瓷材料，包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为Al2O3、Bi2O3、CaTiO3、TiO2、ZrO2、SnO2、Sm2O3、B2O3、LiF中的至少两个的组合。
可选的，所述改性添加剂分别对应占所述主体成分的质量分比为：Al2O3、Bi2O3、CaTiO3、TiO2、ZrO2、SnO2、Sm2O3、B2O3、LiF为0-20％。
在一种实施方式中，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为Al2O3、TiO2、B2O3的组合物。
其中，所述改性添加剂分别对应占所述主体成分的质量分比为：Al2O3、TiO2、B2O3为0-20％。
在一种实施方式中，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为Bi2O3、TiO2、ZrO2的组合物。
其中，所述改性添加剂分别对应占所述主体成分的质量分比为：Bi2O3、TiO2、ZrO2为0-20％。
在一种实施方式中，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为Bi2O3、CaTiO3、ZrO2、Sm2O3的组合物。
其中，所述改性添加剂分别对应占所述主体成分的质量分比为：Bi2O3、CaTiO3、ZrO2、Sm2O3为0-20％。
在一种实施方式中，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为Al2O3、CaTiO3、SnO2、LiF的组合物。
其中，所述改性添加剂分别对应占所述主体成分的质量分比为：Al2O3、CaTiO3、SnO2、LiF为0-20％。
在一种实施方式中，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂Bi2O3、CaTiO3、SnO2、Sm2O3、LiF的组合物。
其中，所述改性添加剂分别对应占所述主体成分的质量分比为：Bi2O3、CaTiO3、SnO2、Sm2O3、LiF为0-20％。
在一种实施方式中，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为TiO2、SnO2、Sm2O3、LiF的组合物。
其中，所述改性添加剂分别对应占所述主体成分的质量分比为：TiO2、SnO2、Sm2O3、LiF为0-20％。
本发明还提供了一种制备上述任一种低介硅酸镁微波介质陶瓷材料的方法，包括步骤：
1)将MgCO3、SiO2配比成所述Mg2+xSiO4后，与所述改性添加剂混匀得到混合料；
2)将步骤1)获得的所述混合料置于行星球磨机中进行湿法球磨，得到球磨浆料；
3)对步骤2)获得的所述球磨浆料进行烘干处理，得到干燥粉料S1；
4)将所述干燥粉料S1放入高温炉箱式炉中进行预烧，制得预烧块材；
5)将步骤4)获得的所述预烧块材粉碎后，置于行球磨机中进行湿法球磨，制得干燥粉体S2；
6)在所述干燥粉体S2中混匀粘合剂后进行喷雾造粒，制得造粒粉；
7)将步骤6)获得的所述造粒粉干压成型制成生坯；
8)将步骤7)获得的所述生坯置于高温箱式炉中按照设定的温度曲线进行烧结，得到微波介质瓷体。
可选的，步骤4)的预烧温度为1100℃-1400℃，预烧时间为3-5小时。
可选的，步骤5)中的球磨时间为4-8小时。
可选的，步骤6)中的所述粘合剂为7wt％的聚乙烯醇溶液，所述粘合剂的质量占比为1％-2％。
可选的，步骤8)的排胶温区为400-600℃，保温2-4小时，高温烧结温区为1100℃～1400℃，烧结时间为4-6小时。
本发明制备的低介硅酸镁微波介质陶瓷材料，具有高抗热震，微波性能优异，介电常数低，品质因数高及介电常数温度系数较小等优点，可用于谐振器、天线、滤波器等微波器件的制造。
具体实施方式
为使得本发明目的、技术方案和有益效果能够更加清晰、完成的呈现，下面将阐述本发明的部分实施例。实施例仅为解释说明的目的，不以任何方式限制本发明的保护范围。除非另有说明，实施例中使用的材料均为常规的或市售可得的材料，材料和试剂的使用添加方式均为本领域常规操作。所表述的含义均为本领域常规定义，例如10％NaOH溶液指质量分数，55％乙醇溶液指体积分数。
实施例1低介硅酸镁微波介质陶瓷材料
包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，x为0～0.5；所述改性添加剂为Al2O3、TiO2、B2O3的组合物。
其中，Mg2+xSiO4的质量分比为88.335％，Al2O3的质量分比为1.554％、TiO2的质量分比为8.520％、B2O3的质量分比为1.591％；所述x在0～0.5之间取值，以使得Mg与Si之间的配比大于或等于二分之一，从而可提升硅酸镁的性能。
本实施例的低介硅酸镁微波介质陶瓷材料的制备方法，包括步骤如下：
1)将MgCO3、SiO2配比成所述Mg2+xSiO4后，与所述改性添加剂混匀得到混合料；
2)将步骤1)获得的所述混合料置于行星球磨机中进行湿法球磨，得到球磨浆料；
3)对步骤2)获得的所述球磨浆料进行烘干处理，得到干燥粉料S1；
4)将所述干燥粉料S1放入高温炉箱式炉中进行预烧，制得预烧块材；
5)将步骤4)获得的所述预烧块材粉碎后，置于行球磨机中进行湿法球磨，制得干燥粉体S2；
6)在所述干燥粉体S2中混匀粘合剂后进行喷雾造粒，制得造粒粉；
7)将步骤6)获得的所述造粒粉干压成型制成生坯；
8)将步骤7)获得的所述生坯置于高温箱式炉中按照设定的温度曲线进行烧结，得到微波介质瓷体。
可选的，步骤4)的预烧温度为1100℃-1400℃，预烧时间为3-5小时。
步骤5)中的球磨时间为4-8小时。
步骤6)中的所述粘合剂为7wt％的聚乙烯醇溶液，所述粘合剂的质量占比为1％-2％。
步骤8)的排胶温区为400-600℃，保温2-4小时，高温烧结温区为1100℃～1400℃，烧结时间为4-6小时。
实施例2低介硅酸镁微波介质陶瓷材料
包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，x为0～0.5；所述改性添加剂为Bi2O3、TiO2、ZrO2的组合物。
其中，Mg2+xSiO4的质量分比为89.339％，Bi2O3的质量分比为0.262％，TiO2的质量分比为9.010％，ZrO2的质量分比为1.390％。
制备方法：同实施例1。
实施例3低介硅酸镁微波介质陶瓷材料
包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，x为0～0.5；所述改性添加剂为Bi2O3、CaTiO3、ZrO2、Sm2O3的组合物。
其中，Mg2+xSiO4的质量分比为81.649％，Bi2O3的质量分比为2.431％，CaTiO3的质量分比为9.458％，ZrO2的质量分比为3.429％，Sm2O3的质量分比为3.033％。
制备方法：同实施例1。
实施例4低介硅酸镁微波介质陶瓷材料
包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，x为0～0.5；所述改性添加剂为Al2O3、CaTiO3、SnO2、LiF的组合物。
其中，Mg2+xSiO4的质量分比为82.366％，Al2O3的质量分比为0.746％，CaTiO3的质量分比为13.924％，SnO2的质量分比为2.205％，LiF的质量分比为0.759％。
制备方法：同实施例1。
实施例5低介硅酸镁微波介质陶瓷材料
包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，x为0～0.5；所述改性添加剂为Bi2O3、CaTiO3、SnO2、Sm2O3、LiF的组合物。
其中，Mg2+xSiO4的质量分比为80.909％，Bi2O3的质量分比为2.522％，CaTiO3的质量分比为11.77％，SnO2的质量分比为1.088％，Sm2O3的质量分比为3.146％，LiF的质量分比为0.562％。
制备方法：同实施例1。
实施例6低介硅酸镁微波介质陶瓷材料
包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，x为0～0.5；所述改性添加剂为TiO2、SnO2、Sm2O3、LiF的组合物。
其中，Mg2+xSiO4的质量分比为84.139％，TiO2的质量分比为7.239％，SnO2的质量分比为2.277％，Sm2O3的质量分比为5.268％，LiF的质量分比为1.078％。
制备方法：同实施例1。
表1～表2示出了本发明实施例1～实施例6的化学原料配方以及样品测试数据。
表1：
| 实例 | Mg<sub>2+x</sub>SiO<sub>4</sub> | Al<sub>2</sub>O<sub>3</sub> | Bi<sub>2</sub>O<sub>3</sub> | CaTiO<sub>3</sub> | TiO<sub>2</sub> | ZrO<sub>2</sub> | SnO<sub>2</sub> | Sm<sub>2</sub>O<sub>3</sub> | B<sub>2</sub>O<sub>3</sub> | LiF |
| 实施例1 | 88.335 | 1.554 | 8.520 | 1.591 | ||||||
| 实施例2 | 89.339 | 0.262 | 9.010 | 1.390 | ||||||
| 实施例3 | 81.649 | 2.431 | 9.458 | 3.429 | 3.033 | |||||
| 实施例4 | 82.366 | 0.746 | 13.924 | 2.205 | 0.759 | |||||
| 实施例5 | 80.909 | 2.522 | 11.77 | 1.088 | 3.146 | 0.562 | ||||
| 实施例6 | 84.139 | 7.239 | 2.277 | 5.268 | 1.078 |
表2：
由此可知，本发明制备的低介硅酸镁微波介质陶瓷材料的介电常数为6-9，品质因数Q×f为4000～10000GHz，谐振频率温度系数τf为-10～+10ppm/℃；可应用于5G通信基站用滤波器、GPS天线、谐振器等微波器件，具有高抗热震、介电常数可调、高品质因数和近零的谐振频率温度系数的优点。
以上各实施例仅用以说明本申请的技术方案，而非对其限制；尽管参照前述各实施例对本申请进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本申请各实施例技术方案的范围。
当然，本发明还可有其它多种实施例，在不背离本发明精神及其实质的情况下，熟悉本领域的技术人员当可根据本发明作出各种相应的改变和变形，但这些相应的改变和变形都应属于本发明所附的权利要求的保护范围。
Claims (7)
1.一种低介硅酸镁微波介质陶瓷材料，其特征在于，包括主体成分和改性添加剂，所述主体成分为Mg2+xSiO4，其中x＝0～0.5；所述改性添加剂为Al2O3、Bi2O3、CaTiO3、TiO2、ZrO2、SnO2、Sm2O3、B2O3、LiF中的至少两个的组合。
2.根据权利要求1所述的低介硅酸镁微波介质陶瓷材料，其特征在于，所述改性添加剂分别对应占所述主体成分的质量分比为：Al2O3、Bi2O3、CaTiO3、TiO2、ZrO2、SnO2、Sm2O3、B2O3、LiF为0-20.0％。
3.一种制备权利要求1～2任一项所述低介硅酸镁微波介质陶瓷材料的方法，其特征在于，包括步骤：
1)将MgCO3、SiO2配比成所述Mg2+xSiO4后，与所述改性添加剂混匀得到混合料；
2)将步骤1)获得的所述混合料置于行星球磨机中进行湿法球磨，得到球磨浆料；
3)对步骤2)获得的所述球磨浆料进行烘干处理，得到干燥粉料S1；
4)将所述干燥粉料S1放入高温炉箱式炉中进行预烧，制得预烧块材；
5)将步骤4)获得的所述预烧块材粉碎后，置于行球磨机中进行湿法球磨，制得干燥粉体S2；
6)在所述干燥粉体S2中混匀粘合剂后进行喷雾造粒，制得造粒粉；
7)将步骤6)获得的所述造粒粉干压成型制成生坯；
8)将步骤7)获得的所述生坯置于高温箱式炉中按照设定的温度曲线进行烧结，得到微波介质瓷体。
4.根据权利要求3所述的方法，其特征在于，所述步骤4)的预烧温度为1100℃-1400℃，预烧时间为3-5小时。
5.根据权利要求3所述的方法，其特征在于，所述步骤5)中的球磨时间为4-8小时。
6.根据权利要求3所述的方法，其特征在于，所述步骤6)中的所述粘合剂为7wt％的聚乙烯醇溶液，所述粘合剂的质量占比为1％-2％。
7.根据权利要求3所述的方法，其特征在于，所述步骤8)的排胶温区为400-600℃，保温2-4小时，高温烧结温区为1100℃～1400℃，烧结时间为4-6小时。
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| CN115959895A (zh) * | 2022-12-12 | 2023-04-14 | 大富科技(安徽)股份有限公司 | 微波介质陶瓷材料及其制备方法、微波介质陶瓷器件 |
| CN115959895B (zh) * | 2022-12-12 | 2024-02-20 | 大富科技(安徽)股份有限公司 | 微波介质陶瓷材料及其制备方法、微波介质陶瓷器件 |
| CN117585994A (zh) * | 2023-11-10 | 2024-02-23 | 江苏垦博电子科技有限公司 | 现代通信用超低介电常数微波介质材料及其制备方法 |
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