CN107417273A - 一种低损耗高温度稳定性npo电容器介质材料及其制备方法 - Google Patents
一种低损耗高温度稳定性npo电容器介质材料及其制备方法 Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 31
- 239000003990 capacitor Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 26
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 5
- 229910003122 ZnTiO3 Inorganic materials 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 description 14
- 239000011777 magnesium Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 6
- 229910002370 SrTiO3 Inorganic materials 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 229910002971 CaTiO3 Inorganic materials 0.000 description 3
- 229910017676 MgTiO3 Inorganic materials 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 206010068052 Mosaicism Diseases 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- SXSVTGQIXJXKJR-UHFFFAOYSA-N [Mg].[Ti] Chemical compound [Mg].[Ti] SXSVTGQIXJXKJR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 210000003765 sex chromosome Anatomy 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于微波陶瓷领域，具体涉及一种低损耗高温度稳定性NPO电容器介质材料及其制备方法。所述NPO电容器介质材料的组分表示为：[0.8mol％SrTiO3‑(Mg2/3Zn1/3)TiO3]‑bwt％B2O3，其中0.5≦b≦5。本发明选用B2O3作为助熔剂，在1130℃～1170℃烧结成型，大大降低了烧结温度，节约了能耗；同时，所述NPO电容器介质材料的介电常数在19～25之间，在‑55℃～125℃温度区间范围内的容温系数为‑60～60ppm/℃，具有中介电常数，高的温度稳定性，低损耗等介电性能。
Description
技术领域
本发明属于微波陶瓷领域，具体涉及一种低损耗高温度稳定性NPO电容器介质材料及其制备方法。
背景技术
国际上多层陶瓷电容厂商以美国的ATC，FERRO，NOVACAP，日本的村田，松下和荷兰飞利浦公司均为排名世界前列的公司。多层陶瓷电容器规模化生产以来，近几年已经成为电容器市场的主流，并且每年市场销量增加速度很快。我国的MLCC产业相比电子信息产业强国(如日本美国)一直处于落后状态，国内的MLCC生产厂家以风华高科等公司为代表，在技术落后的主体情况下不断引进国外先进MLCC技术，改进国内现有技术，不断缩短我国与电子信息产业强国MLCC产业间的差距。随着微电子技术的不断进步，对MLCC的可靠性要求逐步提高，特别是温度稳定性方面，开发在一定温度区间内具有高温度稳定性的陶瓷材料组分是目前研究的热点。
镁钛锌系统(MgO-TiO2-ZnO系统)是以氧化物MgO、TiO2、ZnO等为原料而合成。
MgO-TiO2-ZnO系统的主晶相化合物为较多的正钛酸镁2MgO·TiO2和较少量的正钛酸锌2ZnO·TiO2等。这两类主晶相都为尖晶石结构的立方晶系。以该系统为基础研制的陶瓷介质材料具有非常理想的高频性能，并且能够通过改变成分的配比，得到适当配比时，可以有效的减小介质材料的介电损耗。该系统的特点则是整体的介电常数都非常小，一般为几十左右。该系统的缺点就是容温系数为正数，需要容温系数为负数的补偿剂，并且该体系烧结温度过高。
(MgTiO3-ZnTiO3)基的陶瓷组分已经成为常用的低介质常数高稳定瓷料的研发成分，国内外研究的主要针对性问题在于添加的负温度系数补偿材料，工艺的简化和烧结温度的降低。(MgTiO3-ZnTiO3)基的陶瓷主要采用传统固相法制备，高温烧结温度通常在1200～1300℃，国内外研究常见的负温度系数补偿材料有CaTiO3，CaTiO3的介电常数在1300左右，温度系数在-1500～1600ppm/℃，通过添加适量补偿CaTiO3可以将电容温度系数调节到-60～60ppm/℃，但存在烧结温度过高，负温度系数补偿材料添加量难以控制等原因。
发明内容
本发明针对现有技术的不足，目的在于提供一种低损耗高温度稳定性NPO电容器介质材料及其制备方法。
为实现上述发明目的，本发明采用的技术方案为：
一种低损耗高温度稳定性NPO电容器介质材料，所述NPO电容器介质材料为(MgTiO3-ZnTiO3)基中介电常数陶瓷，其组分表示为：[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]-bwt％B2O3，其中0.5≦b≦5。
上述方案中，所述NPO电容器介质材料的介电常数为19～25。
上述方案中，所述NPO电容器介质材料在-55℃～125℃温度区间范围内的容温系数为-60～60ppm/℃。
上述低损耗高温度稳定性NPO电容器介质材料的制备方法，包括如下步骤：
(1)称取原料：以4MgCO3·Mg(OH)2·5H2O、TiO2、ZnO、SrCO3和B2O3为原料，按照组分化学计量比换算[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]-bwt％B2O3，其中0.5≦b≦5，称取各原料组分；
(2)将各原料组分进行第一次球磨混匀、干燥烘干，然后在1080℃～1100℃下预烧2h～3h，随后对预烧后的粉料进行第二次球磨、干燥烘干，再向其中加入PVA溶液作为粘结剂，经造粒、过筛后，压制成陶瓷圆片，置于600℃马弗炉中保温2h～3h排胶，最后在1130℃～1170℃保温2h～3h得到NPO电容器介质材料。
上述方案中，所述第一次球磨和第二次球磨的时间均为24h。
上述方案中，所述干燥烘干的温度均为80℃～100℃。
上述方案中，所述PVA溶液的质量浓度为5wt％。
上述方案中，所述过筛的筛子为100目。
本发明的有益效果：
(1)本发明所述NPO电容器介质材料的组分包含了钛酸镁、钛酸锌、钛酸锶、三氧化二硼，所述NPO电容器介质材料的介电常数在19～25之间，在-55℃～125℃温度区间范围内容温系数在-60～60ppm/℃之间，具有中介电常数，高的温度稳定性，低损耗等介电性能。
(2)本发明所述NPO电容器介质材料为(MgTiO3-ZnTiO3)基中介电常数陶瓷，其中(MgTiO3-ZnTiO3)的容温系数为正数，与作为负容温系数补偿剂的SrTiO3复配可使材料总体的容温系数趋近于0；本发明选用B2O3作为助熔剂，在1130℃～1170℃烧结成型，大大降低了烧结温度；此外，(MgTiO3-ZnTiO3)基的介电常数在20左右，选择SrTiO3和B2O3配合使得所述NPO电容器介质材料的介电常数维持在19～25之间；
(3)本发明所述NPO电容器介质材料的制备方法，具有原料丰富且价格低廉的优点，同时选用碱式碳酸镁为原料，可大大提高反应活性，选用B2O3作为助熔剂大大降低了烧结温度，节约能耗。
附图说明
图1为本发明所述NPO电容器介质材料的容温系数随B2O3含量的变化。
图2为本发明所述NPO电容器介质材料的介电损耗(在1kHz频率下)随B2O3含量的变化，其中横坐标是温度，纵坐标是介电损耗。
图3为本发明所述NPO电容器介质材料的XRD图谱随B2O3含量的变化。
具体实施方式
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明的内容不仅仅局限于下面的实施例。
实施例1
一种中介电常数、低损耗、高温度稳定性(MgTiO3-ZnTiO3)基陶瓷，组分为：[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]-3wt％B2O3，按摩尔比和重量比的可写为：MgTiO3(0.661mol％)，ZnTiO3(0.331mol％)，SrTiO3(0.8mol％)，B2O3(3wt％)，通过如下方法制备得到：
用分析纯氧化物4MgCO3·Mg(OH)2·5H2O(>98％)，TiO2(>99％)，ZnO(>99％)，SrCO3(>99％)，B2O3(>99％)为原料，按照化学计量比计算从而配料合成3wt％B2O3-[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]组分放在球磨罐中混匀。将配好的3wt％B2O3-[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]粉料在球磨机上球磨24小时，在100℃干燥箱内烘干，在1100℃下预烧2h～3h，然后对预烧后的粉料进行二次球磨，经过24小时后在干燥箱中烘干，随后加入5wt％的PVA溶液作为粘结剂，经过造粒、过筛(筛子为100目)后，用压片机在压力约为200MPa下压制成陶瓷圆片(陶瓷坯体厚约为1.5mm，直径约为12mm)，之后在600℃马弗炉中保温2h～3h排胶，最后在1150℃温度条件下保温2h～3h得到陶瓷样品，最后镀银测试介电性能。
本实施例制备所得(MgTiO3-ZnTiO3)基陶瓷的介电常数为18.6，在-55℃～125℃温度区间范围内容温系数在-60-60ppm/℃之间，介电损耗为0.003。
实施例2
一种中介电常数、低损耗、高温度稳定性(MgTiO3-ZnTiO3)基陶瓷，组分为：[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]-1wt％B2O3，按摩尔比和重量比的可写为：MgTiO3(0.661mol％)，ZnTiO3(0.331mol％)，SrTiO3(0.8mol％)，B2O3(1wt％)，通过如下方法制备得到：
用分析纯氧化物4MgCO3·Mg(OH)2·5H2O(>98％)，TiO2(>99％)，ZnO(>99％)，SrCO3(>99％)，B2O3(>99％)为原料，按照化学计量比计算从而配料合成1wt％B2O3-[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]组分放在球磨罐中混匀。将配好的1wt％B2O3-[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]粉料在球磨机上球磨24小时，在100℃干燥箱内烘干，在1100℃下预烧2h～3h，然后对预烧后的粉料进行二次球磨，经过24小时后在干燥箱中烘干，随后加入5wt％的PVA溶液作为粘结剂，经过造粒、过筛(筛子为100目)后，用压片机在压力约为200MPa下压制成陶瓷圆片(陶瓷坯体厚约为1.5mm，直径约为12mm)，之后在600℃马弗炉中保温2h～3h排胶，最后在1150℃温度条件下保温2h～3h得到陶瓷样品，最后镀银测试介电性能。
本实施例制备所得(MgTiO3-ZnTiO3)基陶瓷的介电常数为19.7，在-55℃～125℃温度区间范围内容温系数在-60-60ppm/℃之间，介电损耗为0.0027。
实施例3
一种中介电常数、低损耗、高温度稳定性(MgTiO3-ZnTiO3)基陶瓷，组分为：[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]-0.5wt％B2O3，按摩尔比和重量比的可写为：MgTiO3(0.661mol％)，ZnTiO3(0.331mol％)，SrTiO3(0.8mol％)，B2O3(0.5wt％)，通过如下方法制备得到：
用分析纯氧化物4MgCO3·Mg(OH)2·5H2O(>98％)，TiO2(>99％)，ZnO(>99％)，SrCO3(>99％)，B2O3(>99％)为原料，按照化学计量比计算从而配料合成5wt％B2O3-[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]组分放在球磨罐中混匀。将配好的5wt％B2O3-[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]粉料在球磨机上球磨24小时，在100℃干燥箱内烘干，在1100℃下预烧2h～3h，然后对预烧后的粉料进行二次球磨，经过24小时后在干燥箱中烘干，随后加入5wt％的PVA溶液作为粘结剂，经过造粒、过筛(筛子为100目)后，用压片机在压力约为200MPa下压制成陶瓷圆片(陶瓷坯体厚约为1.5mm，直径约为12mm)，之后在600℃马弗炉中保温2h～3h排胶，最后在1130℃温度条件下保温2h～3h得到陶瓷样品，最后镀银测试介电性能。
本实施例制备所得(MgTiO3-ZnTiO3)基陶瓷的介电常数为20.6，在-55℃～125℃温度区间范围内容温系数在-30-30ppm/℃之间，介电损耗为0.002。
显然，上述实施例仅仅是为清楚地说明所作的实例，而并非对实施方式的限制。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。而因此所引申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内。
Claims (8)
1.一种低损耗高温度稳定性NPO电容器介质材料，其特征在于，所述NPO电容器介质材料为(MgTiO3-ZnTiO3)基中介电常数陶瓷，其组分表示为：[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]-bwt％B2O3，其中0.5≦b≦5。
2.根据权利要求1所述的低损耗高温度稳定性NPO电容器介质材料，其特征在于，所述NPO电容器介质材料的介电常数为19～25。
3.根据权利要求1所述的低损耗高温度稳定性NPO电容器介质材料，其特征在于，所述NPO电容器介质材料在-55℃～125℃温度区间范围内的容温系数为-60～60ppm/℃。
4.权利要求1～3任一所述低损耗高温度稳定性NPO电容器介质材料的制备方法，其特征在于，包括如下步骤：
(1)称取原料：以4MgCO3·Mg(OH)2·5H2O、TiO2、ZnO、SrCO3和B2O3为原料，按照组分化学计量比换算[0.8mol％SrTiO3-(Mg2/3Zn1/3)TiO3]-bwt％B2O3，其中0.5≦b≦5，称取各原料组分；
(2)将各原料组分进行第一次球磨混匀、干燥烘干，然后在1080℃～1100℃下预烧2h～3h，随后对预烧后的粉料进行第二次球磨、干燥烘干，再向其中加入PVA溶液作为粘结剂，经造粒、过筛后，压制成陶瓷圆片，置于600℃马弗炉中保温2h～3h排胶，最后在1130℃～1170℃保温2h～3h得到NPO电容器介质材料。
5.根据权利要求4所述的制备方法，其特征在于，所述第一次球磨和第二次球磨的时间均为24h。
6.根据权利要求4所述的制备方法，其特征在于，所述干燥烘干的温度均为80℃～100℃。
7.根据权利要求4所述的制备方法，其特征在于，所述PVA溶液的质量浓度为5wt％。
8.根据权利要求4所述的制备方法，其特征在于，所述过筛的筛子为100目。
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