CN106866136A - 化学包覆法制备x9r型陶瓷电容器介质材料 - Google Patents
化学包覆法制备x9r型陶瓷电容器介质材料 Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 18
- 239000003989 dielectric material Substances 0.000 title claims abstract description 15
- 238000000576 coating method Methods 0.000 title claims abstract description 8
- 239000000126 substance Substances 0.000 title claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 25
- 239000000725 suspension Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 12
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002485 combustion reaction Methods 0.000 claims abstract description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 4
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 4
- 229910003237 Na0.5Bi0.5TiO3 Inorganic materials 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
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Abstract
本发明公开了一种化学包覆法制备X9R型陶瓷电容器介质材料，先按Na0.5Bi0.5TiO3(NBT)的化学计量比，将硝酸铋和硝酸钠溶于柠檬酸水溶液中，制成溶液A；再将钛酸四丁酯溶于乙二醇中，制成溶液B；将A倒入B中，制成溶胶C；再将BiTiO3分散在聚乙二醇中，得到悬浮液D。将C倒入D中，形成凝胶；按照BaTiO3(BT)与NBT按摩尔比100:10～20，100:21～30，100:31～35制成凝胶E1、E2、E3，自蔓延燃烧，得到BT@NBT的粉体F1、F2、F3，再按其质量比例1:1:1混合，得到悬浊液G；另将Nb(OH)5溶于草酸水溶液中，形成溶液H。将H倒入G中，得到悬浮液I，烘干后得到BT@NBT@Nb的三层粉体，成型后于1200～1270℃下烧结，制得X9R型陶瓷电容器介质材料。本发明工作温度为‑55℃～200℃，晶粒较小且分布均匀，具有良好的应用前景。
Description
技术领域
本发明属于电子信息材料与元器件领域，特别涉及一种以钛酸钡为基，采用化学包覆法制备宽工作温度范围的陶瓷电容器介质及其制备方法。
背景技术
片式多层陶瓷电容器是电子设备最基本的元器件，具有相当广泛的应用。随着电子元器件满足苛刻环境条件的要求越来越高，MLCC用介质材料的上限工作温度要求不断提升。例如，大功率相控阵雷达、装甲车辆、弹载/箭载电路中，均要求器件的工作温度延伸到150℃以上；用来探寻油气储量的电子设备，可能需要遭受近200℃的温度；在中国载人航天工程中，神州7号中的电子设备就用到高温MLCC。然而传统X7R和X8R型陶瓷电容器的工作温度上限分别为125℃和150℃，(根据国际电子工业协会标准，X代表-55℃，R代表ΔC/C＜15％，7代表125℃，8代表150℃)，显然不能满足应用需求，严重制约着我国电子产品的发展。因此亟须提高介质材料的工作温度上限。
为提高器件的集成度，多层陶瓷电容器从0603/0402发展到0201/01005，多层陶瓷电容器的单层介质厚度不断降低，从5um降低到2um，1um甚至更薄，这就对陶瓷介质材料晶粒尺寸提出更高的要求，陶瓷晶粒尺寸也要相应的降低，并且要求陶瓷晶粒的大小均匀。传统固相法所制备介质材料存在晶粒大、晶粒大学分布不均匀等问题，显然无法满足目前电子器件的发展要求。因此，采用新的制备方法研制高工作温度上限的X9R型介质材料(9代表200℃)迫在眉睫。
发明内容
本发明的目的，是克服现有多层陶瓷电容器介质材料工作温度低、晶粒尺寸大且不均匀等缺点，提供一种采用化学包覆法制备的工作温度范围宽(-55℃～200℃)、容量变化率较小(＜±15％)、晶粒分布均匀的多层陶瓷电容器介质。
本发明通过如下技术方案予以实现：
一种化学包覆法制备X9R型陶瓷电容器介质材料，具有如下步骤：
(1)按照Na0.5Bi0.5TiO3简称NBT的化学计量比，将硝酸铋和硝酸钠溶于柠檬酸水溶液中，搅拌至澄清，制成溶液A；将钛酸四丁酯溶于乙二醇中，制成溶液B；再将溶液A缓慢倒入溶液B中，加入氨水调节PH值为4～8，制成溶胶C；
(2)将粒径50～300nm的BiTiO3分散在聚乙二醇中，超声处理30分钟，得到BiTiO3悬浮液D；
(3)将步骤(1)的溶胶C缓慢倒入步骤(2)的悬浮液D中，再在80℃下搅拌形成凝胶；按照BaTiO3简称BT与NBT按摩尔比100:10～20，100:21～30，100:31～35分别配料，最终制成凝胶E1、E2、E3；将上述凝胶分别于550℃炉中进行自蔓延燃烧，得到BT@NBT的粉体F1、F2、F3；
(4)将步骤(3)的粉体F1、F2、F3按照质量比例1:1:1混合，在聚乙二醇水溶液中超声分散30分钟，得到悬浊液G；
(5)将Nb(OH)5溶解于草酸水溶液中，磁力搅拌直至彻底澄清，形成溶液H；
(6)将步骤(5)的溶液H倒入步骤(4)的悬浊液G中，搅拌4h，缓慢加入氨水调节PH为4～8，最终得到悬浮液I，其中BT与Nb(OH)5按照摩尔比100:2～6进行配料；
(7)将悬浮液I进行烘干，得到BT@NBT@Nb的三层粉体；再向粉体中外加质量百分比为5.5～8％的石蜡造粒，再过筛，压制成生坯，于1200～1270℃下烧结；
(8)将步骤(7)烧结后的制品上下表面均匀涂覆银浆，经550℃烧渗制备电极，制得X9R型陶瓷电容器介质材料。
所述步骤(7)的过筛为1000孔/cm2分样筛，是在4～10Mpa压强下压制成型。
所述步骤(7)的烧结温度为1250℃。
本发明公开的X9R型陶瓷电容器介质材料的性能优异，工作温度范围宽(-55℃～200℃)，晶粒粒径较小且分布均匀，具有良好的应用前景。
具体实施方式
本发明所用原料均为分析纯原料，下面通过具体实施例对本发明作进一步说明。
按照NBT的化学计量比，将硝酸铋和硝酸钠溶于柠檬酸水溶液中，搅拌至澄清，形成溶液A；将钛酸四丁酯溶于乙二醇中，形成溶液B；将溶液A缓慢倒入溶液B，加入适量氨水调节PH值4～8，形成溶胶C；再将粒径50～300nm的BT分散在聚乙二醇中，超声处理30分钟，得到BT悬浮液D；将溶胶C缓慢倒入悬浮液D中，再在80℃下搅拌形成凝胶；按照BT与NBT摩尔比100:10～20，100:21～30，100:31～35分别配料，最终形成凝胶E1、E2、E3；将凝胶E1、E2、E3分别在550℃的炉中进行自蔓延燃烧得到BT@NBT的粉体F1、F2、F3；再将粉体F1、F2、F3按照质量比例1:1:1混合，在聚乙二醇水溶液中超声分散30分钟，得到悬浊液G；将一定量的Nb(OH)5溶解于草酸水溶液中，磁力搅拌直至彻底澄清，形成溶液H；将溶液H倒入悬浊液G中，搅拌4h，缓慢加入氨水调节PH为6～12得到悬浮液I；按照BT与Nb(OH)5摩尔比100:2～6进行配料；将悬浮液I进行烘干，得到BT@NBT@Nb的三层粉体；三层粉体中外加质量百分比为5.5～8％的石蜡造粒，然后过1000孔/cm2分样筛，在4～10Mpa压强下压制成生坯，再于1200～1270℃下烧结；将所得到的的制品上下表面均匀涂覆银浆，经550℃烧渗制备电极，制得宽工作温度范围的多层陶瓷电容器介质。
本发明具体实施例的主要工艺参数见表1和表2，介电性能详见表3。
表1
表2
表3
本发明并不局限于上述实施例，很多细节的变化时可能的，但这并不因此违背本发明的范围和精神。
Claims (3)
1.一种化学包覆法制备X9R型陶瓷电容器介质材料，具有如下步骤：
(1)按照Na0.5Bi0.5TiO3简称NBT的化学计量比，将硝酸铋和硝酸钠溶于柠檬酸水溶液中，搅拌至澄清，制成溶液A；将钛酸四丁酯溶于乙二醇中，制成溶液B；再将溶液A缓慢倒入溶液B中，加入氨水调节PH值为4～8，制成溶胶C；
(2)将粒径50～300nm的BiTiO3分散在聚乙二醇中，超声处理30分钟，得到BiTiO3悬浮液D；
(3)将步骤(1)的溶胶C缓慢倒入步骤(2)的悬浮液D中，再在80℃下搅拌形成凝胶；按照BaTiO3简称BT与NBT按摩尔比100:10～20，100:21～30，100:31～35分别配料，最终制成凝胶E1、E2、E3；将上述凝胶分别于550℃炉中进行自蔓延燃烧，得到BT@NBT的粉体F1、F2、F3；
(4)将步骤(3)的粉体F1、F2、F3按照质量比例1:1:1混合，在聚乙二醇水溶液中超声分散30分钟，得到悬浊液G；
(5)将Nb(OH)5溶解于草酸水溶液中，磁力搅拌直至彻底澄清，形成溶液H；
(6)将步骤(5)的溶液H倒入步骤(4)的悬浊液G中，搅拌4h，缓慢加入氨水调节PH为4～8，最终得到悬浮液I，其中BT与Nb(OH)5按照摩尔比100:2～6进行配料；
(7)将悬浮液I进行烘干，得到BT@NBT@Nb的三层粉体；再向粉体中外加质量百分比为5.5～8％的石蜡造粒，再过筛，压制成生坯，于1200～1270℃下烧结；
(8)将步骤(7)烧结后的制品上下表面均匀涂覆银浆，经550℃烧渗制备电极，制得X9R型陶瓷电容器介质材料。
2.根据权利要求1所述的化学包覆法制备X9R型陶瓷电容器介质材料，其特征在于，所述步骤(7)的过筛为1000孔/cm2分样筛，是在4～10Mpa压强下压制成型。
3.根据权利要求1所述的化学包覆法制备X9R型陶瓷电容器介质材料，其特征在于，所述步骤(7)的烧结温度为1250℃。
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