CN110981468A - 一种钛酸铋钠基压电陶瓷的制备方法 - Google Patents
一种钛酸铋钠基压电陶瓷的制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 79
- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 35
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 32
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 14
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 14
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 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 claims abstract description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 14
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 235000019441 ethanol Nutrition 0.000 claims abstract description 8
- 238000005498 polishing Methods 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 26
- 239000011787 zinc oxide Substances 0.000 abstract description 13
- 239000012071 phase Substances 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 229910010252 TiO3 Inorganic materials 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
本发明公开了一种钛酸铋钠基压电陶瓷的制备方法,将氧化铋、碳酸钠、碳酸钡、二氧化钛、五氧化二铌按照化学计量比称量出BNT‑BT,再按照摩尔比为97:3称取BNT‑BT与AgNbO;将称量的各组分依次加入球磨机中,用酒精为介质,球磨混合后干燥浆料得到BNT‑BT‑3AN粉体,在冷等静压机中成型成圆片;煅烧后保温,烧结成瓷;研磨,加入适量ZnO,球磨烘干压制成陶瓷片煅烧后保温;进行打磨、抛光后用无水乙醇洗涤处理,得到钛酸铋钠基压电陶瓷。本发明通过掺杂氧化锌获得较大的非负电致应变的同时,降低钛酸铋钠陶瓷电致应变滞回性。
Description
技术领域
本发明属于陶瓷材料制备技术领域,涉及一种钛酸铋钠基压电陶瓷的制备方法。
背景技术
钛酸铋钠(Bi0.5Na0.5TiO3)陶瓷具有较大的极化强度与矫顽场,目前市场上通过掺杂钛酸钡(BaTiO3)构筑具有多重相界组分的0.94Bi0.5Na0.5TiO3-0.06BaTiO3,矫顽场降低,且具有较大的电致应变,但因较大的负电致应变对于实际应用的贡献有限。通过查阅现有的文献资料,其中“Large electrostrain and structural evolution in(1-x)[0.94Bi0.5Na0.5TiO3-0.06BaTiO3]-xAgNbO3ceramics,Journal of the European CeramicSocirty:39(2019)994-1001”公开一种最大应变值为0.50%的陶瓷的制备方法,通过进一步掺杂铌酸钾钠(K0.5Na0.5NbO3)、铌酸银(AgNbO3)调节其铁电-弛豫转变温度至室温以下,可获得较大的非负电致应变,但同时电致应变的滞回性达到了69.29%,电致应变的滞回性较大,控制比较困难,不能满足实际需要。
发明内容
本发明的目的是提供一种钛酸铋钠基压电陶瓷的制备方法,解决了现有方法制备的陶瓷获得较大的非负电致应变,但同时电致应变的滞回性较大,控制困难的问题。
本发明所采用的技术方案是,一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,具体步骤如下:
步骤1、将氧化铋、碳酸钠、碳酸钡、二氧化钛、五氧化二铌按照化学计量比0.94Bi0.5Na0.5TiO3-0.06BaTiO3称量出BNT-BT,再按照摩尔比为97:3称取BNT-BT与AgNbO3;
步骤2、将步骤1称量的各组分依次加入球磨机中,用酒精为介质,球磨混合后取出,干燥浆料得到BNT-BT-3AN粉体;
步骤3、将步骤2制得的BNT-BT-3AN粉体,在冷等静压机中成型成圆片;
步骤4,将步骤3成型后的圆片在氧气中煅烧后保温,烧结成瓷;
步骤5,将步骤4烧结的陶瓷取出后研磨,加入适量ZnO,再放入球磨机中球磨,烘干得到BNT-BT-3AN-xZnO(x=0~0.2)粉体;
步骤6,将步骤5制得的粉体压制成陶瓷片煅烧后保温;
步骤7,将步骤6制得陶瓷片进行打磨、抛光后用无水乙醇洗涤处理,得到钛酸铋钠基压电陶瓷。
本发明的其他特点还在于,
在步骤1中称量氧化铋10.0169g~10.1191g、碳酸钠2.2580g~2.3017g、碳酸钡1.0726g~1.0934g、二氧化钛7.3059g~7.3804g、五氧化二铌0.3721g~0.3797g和硝酸银0.4761g~0.4853g。
在步骤2中,在行星球磨机中以200~400r/min的转速球磨12~24h。
在步骤3中,在冷等静压机中,用200~220MPa的压力,保压5~10min成为直径10mm,厚度1mm的圆片。
在步骤4中,在氧气中煅烧至1100~1200℃,保温3~5h。
在步骤5中,用研钵研磨2~3h加入0~4g ZnO,放入行星式球磨机中球磨12~24h。
在步骤6中,陶瓷片煅烧至1025~1075℃,保温1h。
在步骤1中称取的氧化铋、碳酸钠、碳酸钡、二氧化钛、五氧化二铌和硝酸银纯度均不小于98.5%。
本发明的有益效果是,本发明一种钛酸铋钠基压电陶瓷的制备方法,利用固相合成法,通过成分设计引入ZnO,由于ZnO的加入,其复合含量增加使得矫顽场升高,电畴运动困难,陶瓷的滞回性降低,最低可达37.15%。本发明一种钛酸铋钠基压电陶瓷的制备方法,成本低、方法简单、可重复性好,所得材料压电性能优异,可能成为微执行器等电子元器件领域一个有希望的替代体系。
附图说明
图1是本发明一种钛酸铋钠基压电陶瓷的制备方法实施例1-4中制备的陶瓷粉体的X射线衍射图谱;
图2是本发明一种钛酸铋钠基压电陶瓷的制备方法实施例1-4中所得陶瓷的电致应变曲线。
具体实施方式
本发明一种钛酸铋钠基压电陶瓷的制备方法,通过成分设计掺杂氧化锌,从而得到低电致应变滞回性钛酸铋钠(BNT)陶瓷。
本发明一种钛酸铋钠基压电陶瓷的制备方法,具体步骤如下:
步骤1、将氧化铋、碳酸钠、碳酸钡、二氧化钛、五氧化二铌按照化学计量比0.94Bi0.5Na0.5TiO3-0.06BaTiO3称量出BNT-BT,再按照摩尔比为97:3称取BNT-BT与AgNbO3;
步骤2、将步骤1称量的各组分依次加入球磨机中,用酒精为介质,球磨混合后取出,干燥浆料得到BNT-BT-3AN粉体;
步骤3、将步骤2制得的BNT-BT-3AN粉体,在冷等静压机中成型成圆片;
步骤4,将步骤3成型后的圆片在氧气中煅烧后保温,烧结成瓷;
步骤5,将步骤4烧结的陶瓷取出后研磨,加入适量ZnO,再放入球磨机中球磨,烘干得到BNT-BT-3AN-xZnO(x=0~0.2)粉体;
步骤6,将步骤5制得的粉体压制成陶瓷片煅烧后保温;
步骤7,将步骤6制得陶瓷片进行打磨、抛光后用无水乙醇洗涤处理,得到钛酸铋钠基压电陶瓷。
在步骤1中称量氧化铋10.0169g~10.1191g、碳酸钠称2.2580g~2.3017g、碳酸钡称量1.0726g~1.0934g、二氧化钛称量7.3059g~7.3804g、硝酸银称量0.4761g~0.4853g和五氧化二铌称量0.3721g~0.3797g。
在步骤1中称取的氧化铋、碳酸钠、碳酸钡、二氧化钛、五氧化二铌和硝酸银纯度均不小于98.5%。
在步骤2中,在行星球磨机中以200~400r/min的转速球磨12~24h。
在步骤3中,在冷等静压机中,用200~220MPa的压力,保压5~10min成为直径10mm,厚度1mm的圆片。
在步骤4中,在氧气中煅烧至1100~1200℃,保温3~5h。
在步骤5中,用研钵研磨2~3h加入0~4g ZnO,放入行星式球磨机中球磨12~24h。
在步骤6中,陶瓷片煅烧至1025~1075℃,保温1h。
下面结合附图和具体实施方式对本发明进行详细说明。
实施例1
步骤1,称量纯度为98.5%的氧化铋10.0169g、碳酸钠2.2602g、碳酸钡1.0934g、二氧化钛7.3804g、硝酸银0.4765g和五氧化二铌0.3721g。
步骤2,在行星球磨机中用80ml酒精为介质,以250r/min的转速球磨12h,干燥浆料得到BNT-BT-3AN粉体。
步骤3,将干燥粉体在冷等静压机中,用200MPa的压力压5min成为直径10mm,厚度1mm的圆片。
步骤4,将成型后的圆片在氧气中煅烧至1150℃,保温4h烧结成瓷。
步骤5,将烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤,得到钛酸铋钠基压电陶瓷进行银极测试其电致应变性能。
图1中(a)是BNT-BT-3AN陶瓷粉体的X射线衍射图谱,从图2中可以看出,样品呈单一的钙钛矿相,无第二相出现。
实施例2
步骤1,称量纯度为98.6%的氧化铋10.0169g、碳酸钠2.2602g、碳酸钡1.0934g、二氧化钛7.3804g、硝酸银0.4765g和五氧化二铌0.3721g。
步骤2,在行星球磨机中用80ml酒精为介质,以250r/min的转速球磨12h,干燥浆料得到BNT-BT-3AN粉体。
步骤3,将干燥粉体在冷等静压机中,用200MPa的压力压5min成为直径10mm,厚度1mm的圆片。
步骤4,将成型后的圆片在氧气中煅烧至1150℃,保温4h烧结成瓷。
步骤5,取出后用研钵研磨2h加入1g ZnO,放入行星式球磨机中球磨12h,然后烘干得到BNT-BT-3AN-0.05ZnO粉体。
步骤6,将制得的粉体压制成陶瓷片煅烧至1075℃,保温1h。
步骤7,将烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤,得到钛酸铋钠基压电陶瓷进行银极测试其电致应变性能。
图1中(b)是BNT-BT-3AN-0.05ZnO陶瓷粉体的X射线衍射图谱,从图中可以看出,样品呈单一的钙钛矿相,无第二相出现。图2是陶瓷在70kV/mm电压下的电致应变曲线,从图中可以计算得出电致应变滞回性降低到39.14%。
实施例3
步骤1,称量纯度为98.7%的氧化铋10.0169g、碳酸钠2.2602g、碳酸钡1.0934g、二氧化钛7.3804g、硝酸银0.4765g和五氧化二铌0.3721g。
步骤2,在行星球磨机中用80ml酒精为介质,以250r/min的转速球磨12h,干燥浆料得到BNT-BT-3AN粉体。
步骤3,将干燥粉体在冷等静压机中,用200MPa的压力压5min成为直径10mm,厚度1mm的圆片。
步骤4,将成型后的圆片在氧气中煅烧至1150℃,保温4h烧结成瓷。
步骤5,取出后用研钵研磨2h加入2g ZnO,放入行星式球磨机中球磨12h,然后烘干得到BNT-BT-3AN-0.05ZnO粉体。
步骤6,将制得的粉体压制成陶瓷片煅烧至1050℃,保温1h。
步骤7,将烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤,得到钛酸铋钠基压电陶瓷进行银极测试其电致应变性能。
图1中(c)是BNT-BT-3AN-0.1ZnO陶瓷粉体的X射线衍射图谱,从图中可以看出,样品呈单一的钙钛矿相,无第二相出现。图2是陶瓷在70kV/mm电压下的电致应变曲线,从图中可以计算得出电致应变滞回性降低到37.15%。
实施例4
步骤1,称量纯度为98.8%的氧化铋10.0169g、碳酸钠2.2602g、碳酸钡1.0934g、二氧化钛7.3804g、硝酸银0.4765g和五氧化二铌0.3721g。
步骤2,在行星球磨机中用80ml酒精为介质,以250r/min的转速球磨12h,干燥浆料得到BNT-BT-3AN粉体;
步骤3,将干燥粉体在冷等静压机中,用200MPa的压力压5min成为直径10mm,厚度1mm的圆片;
步骤4,将成型后的圆片在氧气中煅烧至1150℃,保温4h烧结成瓷;
步骤5,取出后用研钵研磨2h加入4g ZnO,放入行星式球磨机中球磨12h,然后烘干得到BNT-BT-3AN-0.05ZnO粉体;
步骤6,将制得的粉体压制成陶瓷片煅烧至1025℃,保温1;
步骤7,将步骤6制得陶瓷片进行打磨、抛光后用无水乙醇洗涤处理,得到钛酸铋钠基压电陶瓷进行银极测试其电致应变性能。
图1中(d)是BNT-BT-3AN-0.2ZnO陶瓷粉体的X射线衍射图谱,从图中可以看出,样品呈单一的钙钛矿相,无第二相出现。图2是陶瓷在70kV/mm电压下的电致应变曲线,从图中可以计算得出电致应变滞回性降低到45.12%。
本发明一种钛酸铋钠基压电陶瓷的制备方法,制备出BNT-BT-3AN-0.1ZnO陶瓷,通过成分设计,获得了电致应变滞回性较低的钛酸铋钠基陶瓷。
Claims (8)
1.一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,具体步骤如下:
步骤1、将氧化铋、碳酸钠、碳酸钡、二氧化钛、五氧化二铌按照化学计量比0.94Bi0.5Na0.5TiO3-0.06BaTiO3称量出BNT-BT,再按照摩尔比为97:3称取BNT-BT与AgNbO3;
步骤2、将步骤1称量的各组分依次加入球磨机中,用酒精为介质,球磨混合后取出,干燥浆料得到BNT-BT-3AN粉体;
步骤3、将步骤2制得的BNT-BT-3AN粉体,在冷等静压机中成型成圆片;
步骤4,将步骤3成型后的圆片在氧气中煅烧后保温,烧结成瓷;
步骤5,将步骤4烧结的陶瓷取出后研磨,加入适量ZnO,再放入球磨机中球磨,烘干得到BNT-BT-3AN-xZnO粉体,其中,x=0~0.2;
步骤6,将步骤5制得的粉体压制成陶瓷片煅烧后保温;
步骤7,将步骤6制得陶瓷片进行打磨、抛光后用无水乙醇洗涤处理,得到钛酸铋钠基压电陶瓷。
2.根据权利要求1所述的一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,在所述步骤1中称量氧化铋10.0169g~10.1191g、碳酸钠2.2580g~2.3017g、碳酸钡1.0726g~1.0934g、二氧化钛7.3059g~7.3804g、五氧化二铌0.3721g~0.3797g和硝酸银0.4761g~0.4853g。
3.根据权利要求1所述的一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,在所述步骤2中,在行星球磨机中以200~400r/min的转速球磨12~24h。
4.根据权利要求1所述的一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,在所述步骤3中,在冷等静压机中,用200~220MPa的压力,保压5~10min成为直径10mm,厚度1mm的圆片。
5.根据权利要求1所述的一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,在所述步骤4中,在氧气中煅烧至1100~1200℃,保温3~5h。
6.根据权利要求2所述的一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,在所述步骤5中,用研钵研磨2~3h加入0~4g ZnO,放入行星式球磨机中球磨12~24h。
7.根据权利要求1所述的一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,在所述步骤6中,陶瓷片煅烧至1025~1075℃,保温1h。
8.根据权利要求1所述的一种钛酸铋钠基压电陶瓷的制备方法,其特征在于,在所述步骤1中称取的氧化铋、碳酸钠、碳酸钡、二氧化钛、五氧化二铌和硝酸银纯度均不小于98.5%。
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