CN114105636A - 利用硒化铟改性铌锌锆钛酸铅体系并制得4m聚能换能片的方法 - Google Patents
利用硒化铟改性铌锌锆钛酸铅体系并制得4m聚能换能片的方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910052451 lead zirconate titanate Inorganic materials 0.000 title description 4
- -1 indium selenide modified niobium-zinc lead Chemical class 0.000 title description 3
- 239000000919 ceramic Substances 0.000 claims abstract description 39
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 20
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- AKUCEXGLFUSJCD-UHFFFAOYSA-N indium(3+);selenium(2-) Chemical compound [Se-2].[Se-2].[Se-2].[In+3].[In+3] AKUCEXGLFUSJCD-UHFFFAOYSA-N 0.000 claims abstract description 9
- VOLIIUVAEXIKFU-UHFFFAOYSA-N niobium zinc Chemical compound [Zn].[Zn].[Zn].[Nb] VOLIIUVAEXIKFU-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 18
- 229910052709 silver Inorganic materials 0.000 claims description 18
- 239000004332 silver Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 230000010287 polarization Effects 0.000 claims description 7
- 238000007639 printing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 6
- 238000000889 atomisation Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003292 glue Substances 0.000 description 9
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 239000011787 zinc oxide Substances 0.000 description 7
- 238000000465 moulding Methods 0.000 description 6
- 230000026683 transduction Effects 0.000 description 5
- 238000010361 transduction Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- SITXNCAAFPTBGM-UHFFFAOYSA-N [Pb].[Nb].[Zn] Chemical compound [Pb].[Nb].[Zn] SITXNCAAFPTBGM-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种利用硒化铟改性铌锌锆钛酸铅体系并制得4M聚能换能片的方法，所述方法以Pb3O4，Nb2O5，ZnO，ZrO2，TiO2，BaCO3，In2Se3为初始原料，采用传统固相法，即混料、混合、成型、排胶、烧成、印银、烧银、极化等工序，合成的一种新型压电陶瓷，该压电陶瓷的制备方法工艺简单、易控，换能片频率由3MHz提升到4MHz，制作雾化效果得到显著提升。
Description
技术领域
本发明属于无机材料领域，具体涉及一种利用硒化铟改性铌锌锆钛酸铅体系并制得4M聚能换能片的方法。
背景技术
换能器，顾名思义就是指可以进行能量转换的器件，压电换能器是指利用压电材料的正逆压电效应制成的换能器, 压电效应将电信号转换为机械振动。这种换能器电声转换效率高，原材料价格便宜，制作方便，也不容易老化，常用的材料有石英晶体、钛酸钡和锆钛酸铅。压电换能器的应用十分广泛，按应用的行业分为工业、 农业、 交通运输、生活、医疗及军事等。
现有技术仅能制备出频率为3M的压电元件，为提高压电片的功率，降低能耗，需要研究开发出频率为4M的适宜的压电元件，以满足市场的需求。
发明内容
为了实现4M换能片的制造，本发明通过将硒化铟加入铌锌锆钛酸铅体系，首次制备出性能卓越的4M换能片，由该方法所述材料可适用于制备超声波声呐、超声波雾化、超声波换能等压电陶瓷元件。
本发明提供如下技术方案：
本发明提供了一种利用硒化铟改性铌锌锆钛酸铅体系并制得4M聚能换能片的方法，所述方法以Pb3O4，Nb2O5，ZnO，ZrO2 ，TiO2 ，BaCO3 ，In2Se3为初始原料，按照重量比Pb3O4︰Nb2O5︰ZnO︰ZrO2︰TiO2︰BaCO3︰In2Se3为137.11︰10.63︰3.26︰30.76︰18.4︰5.26︰(0.2-0.8)，采用固相法制备而成。
优选的，所述固相法包括如下步骤：
将各初始原料按重量比称量，经一次球磨后，煅烧，经过二次球磨，烘干过筛，加入PVA造粒压片得到陶瓷片，陶瓷片排胶后在1250℃下烧结，经印银、烧银的陶瓷片最后放入120℃的硅油中，在直流电压30~50 kV/cm下保压15min进行极化处理，得到压电陶瓷。
优选的，所述一次球磨和二次球磨均为行星球磨，球磨时间为12 h。
优选的，所述煅烧为850℃煅烧2 h。
优选的，其特征在于，所述过筛指过100目筛。
优选的，所述造粒压片得到的陶瓷片直径为10 mm，成型压力200 MPa。
优选的，所述排胶是在90~120℃烧结210min，然后在210~450℃烧结180min，再在450~860℃烧结30min。
优选的，所述印银厚度为0.003mm，所述烧银制度为820℃下15min。
优选的，所述陶瓷片排胶后在1250℃下烧结4h，保温3h。
优选的，所述压电陶瓷为窝型压电片。
本发明所述原料除五氧化二铌纯度为99.5w%外，其他原料纯度均在99w%。
本发明的技术方案所获得的技术效果为：本发明以Pb3O4，Nb2O5，ZnO，ZrO2 ，TiO2 ，BaCO3 ，In2Se3为原料，采用传统固相法，即混料、混合、成型、排胶、烧成、印银、烧银、极化等工序，合成的一种4M压电陶瓷（聚能换能片）。该压电陶瓷的制备方法工艺简单、易控，换能片频率由3MHz提升到4MHz，制作雾化效果得到显著提升。
现今各个体系中都只能制备出3M的聚能换能片，本发明通过加入硒化铟以及对铌锌锆钛酸铅材料配方体系的调控将聚能换能片功率提升到4M，在降低材料能耗的同时，实现了5V的低压驱动；在材料直径不变的条件下厚度减小，驱动电压降低的情况下，尤其是将平面压电片工艺改进为窝型压电片，达到聚能的效果，雾化量更大，雾化颗粒更细。
具体实施方式
下面结合具体实施例对本发明作进一步的详细描述。但不应将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明内容所实现的技术均属于本发明的范围。
实施例1
配方：
四氧化三铅:137.11 g
五氧化二铌:10.63 g
氧化锌:3.26g
氧化锆:30.76 g
氧化钛:18.4 g
碳酸钡:5.26g
硒化铟:0.2g
除五氧化二铌纯度为99.5w%外，其他原料纯度均在99w%。
制备工艺过程为：
将各初始原料称量，经行星球磨12h后，850℃煅烧2 h，经过二次行星球磨12h后，烘干过100目筛，加入PVA造粒压片得到陶瓷片(直径10 mm, 成型压力200 MPa)，陶瓷片排胶后在1250℃下烧结，经印银、烧银的陶瓷片最后放入120℃的硅油中，在直流电压30 kV/cm下保压15min进行极化处理，得到压电陶瓷。
其中，各工艺参数如下：
成型方式： 扎膜
排胶制度： 90~120℃烧结210min，210~450烧结180min，450~860烧30min；
烧成温度： 1250℃
烧成时间： 4h
保温时间： 3h
印银厚度：0.003mm
烧银制度：820℃/15min
制备的压电陶瓷主要性能指标测定为：
d33=271pC/N ，kp=0.52 ，Qm=275 ，TC=265℃，εr=2150，tanδ=0.31%，Pr=39.45μC/cm2，Ec=18.98KV/cm
实施例2
配方：
四氧化三铅:137.11 g
五氧化二铌:10.63 g
氧化锌:3.26g
氧化锆:30.76 g
氧化钛:18.4 g
碳酸钡:5.26g
硒化铟:0.4g
除五氧化二铌纯度为99.5w%外，其他原料纯度均在99w%
制备工艺过程为：
将各初始原料称量，经行星球磨12h后，850℃煅烧2 h，经过二次行星球磨12h后，烘干过100目筛，加入PVA造粒压片得到陶瓷片(直径10 mm, 成型压力200 MPa)，陶瓷片排胶后在1250℃下烧结，经印银、烧银的陶瓷片最后放入120℃的硅油中，在直流电压50 kV/cm下保压15min进行极化处理，得到压电陶瓷。
其中，各工艺参数如下：
成型方式： 扎膜
排胶制度： 90~120℃烧结210min，210~450烧结180min，450~860烧30min；
烧成温度： 1250℃
烧成时间： 4h
保温时间： 3h
印银厚度：0.003mm
烧银制度：820℃/15min
制备的压电陶瓷主要性能指标测定为：
d33=365pC/N ，kp=0.63 ，Qm=308 ，TC=265℃，εr=2560，tanδ=0.23%，Pr=41.45μC/cm2，Ec=19.18KV/cm。
实施例3
配方：
四氧化三铅:137.11 g
五氧化二铌:10.63 g
氧化锌:3.26g
氧化锆:30.76 g
氧化钛:18.4 g
碳酸钡:5.26g
硒化铟:0.6g
除五氧化二铌纯度为99.5w%外，其他原料纯度均在99w%
将各初始原料称量，经行星球磨12h后，850℃煅烧2 h，经过二次行星球磨12h后，烘干过100目筛，加入PVA造粒压片得到陶瓷片(直径10 mm, 成型压力200 MPa)，陶瓷片排胶后在1250℃下烧结，经印银、烧银的陶瓷片最后放入120℃的硅油中，在直流电压50 kV/cm下保压15min进行极化处理，得到压电陶瓷。
其中，各工艺参数如下：
成型方式： 扎膜
排胶制度： 90~120℃烧结210min，210~450烧结180min，450~860烧30min；
烧成温度： 1250℃
烧成时间： 4h
保温时间： 3h
印银厚度：0.003mm
烧银制度：820℃/15min
制备的压电陶瓷主要性能指标测定为：
d33=382pC/N ，kp=0.71 ，tanδ=0.18%，Qm=452 ，TC=265℃，εr=2800，Pr=47.21μC/cm2，Ec=19.98KV/cm。
实施例4
配方：
四氧化三铅:137.11 g
五氧化二铌:10.63 g
氧化锌:3.26g
氧化锆:30.76 g
氧化钛:18.4 g
碳酸钡:5.26g
硒化铟:0.8g
除五氧化二铌纯度为99.5w%外，其他原料纯度均在99w%
将各初始原料称量，经行星球磨12h后，850℃煅烧2 h，经过二次行星球磨12h后，烘干过100目筛，加入PVA造粒压片得到陶瓷片(直径10 mm, 成型压力200 MPa)，陶瓷片排胶后在1250℃下烧结，经印银、烧银的陶瓷片最后放入120℃的硅油中，在直流电压50 kV/cm下保压15min进行极化处理，得到压电陶瓷。
其中，各工艺参数如下：
成型方式： 扎膜
排胶制度： 90~120℃烧结210min，210~450烧结180min，450~860烧30min；
烧成温度： 1250℃
烧成时间： 4h
保温时间： 3h
印银厚度：0.003mm
烧银制度：820℃/15min
制备的压电陶瓷主要性能指标测定为：
d33=276pC/N ，kp=0.59 ，tanδ=0.26%，Qm=326 ，TC=265℃，εr=2390，Pr=42.23μC/cm2，Ec=19.68KV/cm。
Claims (10)
1.利用硒化铟改性铌锌锆钛酸铅体系并制得4M聚能换能片的方法，其特征在于，所述方法以Pb3O4，Nb2O5，ZnO，ZrO2 ，TiO2 ，BaCO3 ，In2Se3为初始原料，按照重量比Pb3O4︰Nb2O5︰ZnO︰ZrO2︰TiO2︰BaCO3︰In2Se3为137.11︰10.63︰3.26︰30.76︰18.4︰5.26︰(0.2-0.8)，采用固相法制备而成。
2.根据权利要求1所述的方法，其特征在于，所述固相法包括如下步骤：
将各初始原料按重量比称量，经一次球磨后，煅烧，经过二次球磨，烘干过筛，加入PVA造粒压片得到陶瓷片，陶瓷片排胶后在1250℃下烧结，经印银、烧银的陶瓷片最后放入120℃的硅油中，在直流电压30~50 kV/cm下保压15min进行极化处理，得到压电陶瓷。
3.根据权利要求2所述的方法，其特征在于，所述一次球磨和二次球磨均为行星球磨，球磨时间为12 h。
4.根据权利要求2所述的方法，其特征在于，所述煅烧为850℃煅烧2 h。
5.根据权利要求2所述的方法，其特征在于，所述过筛指过100目筛。
6.根据权利要求2所述的方法，其特征在于，所述造粒压片得到的陶瓷片直径为10 mm，成型压力200 MPa。
7.根据权利要求2所述的方法，其特征在于，所述排胶是在90~120℃烧结210min，然后在210~450℃烧结180min，再在450~860℃烧结30min。
8.根据权利要求2所述的方法，所述印银厚度为0.003mm，所述烧银制度为820℃下15min。
9.根据权利要求2所述的方法，其特征在于，所述陶瓷片排胶后在1250℃下烧结4h， 保温3h。
10.根据权利要求1-9任一项所述的方法，其特征在于，所述压电陶瓷为窝型压电片。
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