CN107056281A - 一种高应变钛酸铋钠基陶瓷及其制备方法 - Google Patents
一种高应变钛酸铋钠基陶瓷及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- 229910052709 silver Inorganic materials 0.000 claims description 10
- 239000004332 silver Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 5
- 229920001778 nylon Polymers 0.000 claims description 5
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
- 230000005684 electric field Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000005621 ferroelectricity Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910003237 Na0.5Bi0.5TiO3 Inorganic materials 0.000 description 1
- 229910020684 PbZr Inorganic materials 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002463 transducing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明公开了一种高应变钛酸铋钠基陶瓷及其制备方法，所述高应变钛酸铋钠基陶瓷的化学计量比为：0.8(BiNa)0.5‑x(LaLi)xTiO3‑0.2Bi0.5K0.5TiO3；x＝0.006‑0.012。本发明通过优化陶瓷配方，然后经过混合、球磨、低温预烧和高温烧结过程之后，使得环境友好型的无铅压电材料钛酸铋钠基陶瓷在较低电场下具有高的应变，室温下电场为45kV cm‑1时，其应变达0.387％，动态压电常数d33 *达860pm/V，同时材料在106次循环下保持优异的抗疲劳特性。
Description
技术领域
本发明属于压电陶瓷材料技术领域，尤其涉及一种高应变钛酸铋钠基陶瓷及其制备方法。
背景技术
利用材料电与机械位移的相互转换特性，压电陶瓷材料在传感器、制动器和换能器等方面表现出极为重要的作用，可广泛地应用于通信、家电、航空、探测和计算机等诸多领域。但是目前大规模使用的压电陶瓷以PbZr1-xTixO3(PZT)等为主的铅基压电陶瓷。铅基压电陶瓷的原料中PbO或Pb3O4约占总量的70％，并且PbO或Pb3O4在陶瓷的烧结过程中容易挥发。含铅压电陶瓷在生产、废弃以及回收过程中给自然环境带来了极大的危害，很难满足环保的使用要求。钛酸铋钠(Na0.5Bi0.5TiO3，BNT)基无铅压电陶瓷由于较高的应变性能得到了广泛的研究。通常采用与其它铁电或者非铁电钙钛矿材料形成准同型相界以进一步提高应变。虽然材料在更高场强下具有更高的应变，但是过高的场强限制了它们的实际应用。M.Acosta,et al.Core-shell lead-free piezoelectric ceramics:Current status andadvanced characterization of the Bi1/2Na1/2TiO3-SrTiO3system.J.Am.Ceram.Soc.2015,98(11):3405-3422文章中对比了不同系列的无铅压电陶瓷，发现BNT基材料在45kVcm-1电压下具有最大的动态压电常数d33 *，即Smax/Emax，约700pm/V。进一步，R.A.Malik,et al.Temperature-insensitive high strain in lead-free Bi0.5(Na0.84K0.16)0.5TiO3-0.04SrTiO3 ceramics for actuatorapplications.J.Am.Ceram.Soc.2015,98(12):3842-3848文中通过对BNT-BKT-ST体系进行Li、Nb双掺杂，使BNT基材料的压电常数d33 *提高到755pm/V。但是对于实际应用而言，无铅压电材料的应变还需要进一步提高，尤其是解决材料在较低场强下应变较低的问题。
发明内容
本发明的目的在于提供一种无铅高应变钛酸铋钠基陶瓷及其制备方法，旨在解决现有压电材料在电场诱发下应变较小的问题。
本发明是这样实现的，一种高应变钛酸铋钠基陶瓷，所述高应变钛酸铋钠基陶瓷的化学计量比为：0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3；x＝0.006-0.012。
本发明的另一目的在于提供一种所述高应变钛酸铋钠基陶瓷的制备方法，所述高应变钛酸铋钠基陶瓷的制备方法包括以下步骤：
步骤一，根据0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3化学配比称量对应量的分析纯Bi2O3，Na2CO3、TiO2、K2CO3、Li2CO3和La2O3；
步骤二，将配好的料放入以酒精为介质、锆球为磨球的尼龙罐中球磨6h-8h；
步骤三，将球磨好的料烘干过筛后并压成大块，在800℃预烧4h-6h得到预烧粉；
步骤四，将预烧粉再次放入球磨罐中研磨10h-12h，烘干后过筛；
步骤五，将过筛后的粉压成直径为12mm，厚度为2mm左右的圆柱体，在300Mpa下等静压下成型；
步骤六，将成型后的试样在1100℃-1200℃下烧结4h-6h；
步骤七，对烧结成瓷的试样进行打磨和抛光，超声清洗后涂覆银浆，在550℃下保温30min烧成银电极。
本发明的另一目的在于提供一种由所述高应变钛酸铋钠基陶瓷制造的传感器。
本发明的另一目的在于提供一种由所述高应变钛酸铋钠基陶瓷制造的制动器。
本发明的另一目的在于提供一种由所述高应变钛酸铋钠基陶瓷制造的换能器。
本发明提供的高应变钛酸铋钠基陶瓷及其制备方法，通过优化陶瓷配方，使得环境友好型的无铅压电材料钛酸铋钠基陶瓷在较低电场下具有高的应变，室温下电场为45kVcm-1时，其应变达0.387％，动态压电常数d33 *达860pm/V。同时材料在106次循环下性能没有退化，介电损耗tanδ保持在0.08以下。
附图说明
图1是本发明实施例提供的高应变钛酸铋钠基陶瓷的制备方法流程图。
图2是本发明实施例提供的0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3，x＝0.01时陶瓷的X射线衍射和扫描电镜图谱示意图。
图3是本发明实施例提供的0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3，x＝0.01时陶瓷不同频率的介电常数和介电损耗随温度的变化图谱示意图；
图中：虚线箭头方向表示频率增大。
图4是本发明实施例提供的0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3，x＝0.01时陶瓷室温下45kVcm-1电场下的电滞回线和应变曲线图谱示意图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
下面结合附图对本发明的应用原理作详细的描述。
本发明实施例提供的高应变钛酸铋钠基陶瓷的化学计量比为：0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3(x＝0.006-0.012)。
如图1所示，本发明实施例提供的高应变钛酸铋钠基陶瓷的制备方法包括以下步骤：
S101：根据0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3(x＝0.006-0.012)化学配比称量对应量的分析纯Bi2O3，Na2CO3、TiO2、K2CO3、Li2CO3和La2O3；
S102；将配好的料放入以酒精为介质、锆球为磨球的尼龙罐中球磨6h-8h；
S103：将球磨好的料烘干过筛后并压成大块，在800℃预烧4h-6h得到预烧粉；
S104：将预烧粉再次放入球磨罐中研磨10h-12h，烘干后过筛；
S105：将过筛后的粉压成直径为12mm，厚度为2mm左右的圆柱体，在300Mpa下等静压下成型；
S106：将成型后的试样在1100℃-1200℃下烧结4h-6h；
S107：对烧结成瓷的试样进行打磨和抛光，超声清洗后涂覆银浆，在550℃下保温30min烧成银电极。
下面结合具体实施例对本发明的应用原理作进一步的描述。
实施例1，根据化学计量比称量22.9252g的Bi2O3，4.1548g的Na2CO3、1.3821g的K2CO3、7.987g的TiO2、0.0591g的LiCO3和0.2606g的La2O3，将配好的料放入以酒精为介质、锆球为磨球的尼龙罐中球磨6-8h；将球磨好的料烘干过筛后并压成大块，在800℃预烧4h得到预烧粉；将预烧粉再次放入球磨罐中研磨10-12h，烘干后过筛；将过筛后的粉压成直径为12mm，厚度为2mm左右的圆柱体，在300Mpa下等静压下成型；将成型后的试样在1100-1200℃下烧结4h；对烧结成瓷的试样进行打磨和抛光，超声清洗后涂覆银浆，在550℃下保温30min烧成银电极。采用安捷伦精密阻抗分析仪(4294A，Agilent，CA，USA)测试样品的介电谱。采用TF2000型铁电参数测试仪(aixACCT,Aachen,Germany)测试样品的电滞回线、应变曲线和电流密度曲线。从图2可以看出样品属于赝立方钙钛矿相，并没有出现杂相，从扫描图谱可以看出样品比较致密、均一且呈多边形分布。从图3可以看出材料具有典型的弛豫特性，其介电损耗保持在0.08以下。图4为材料的电滞回线和应变曲线图谱，可以看出材料具有典型的束腰型电滞回线，它在45kV cm-1电场下具有非常大的应变，其动态压电常数d33 *提高到860pm/V，且样品在106次循环下具有优异的抗疲劳特性。
实施例2，根据化学计量比称量22.8506g的Bi2O3，4.1378g的Na2CO3、1.3821g的K2CO3、7.987g的TiO2、0.0709g的LiCO3和0.3128g的La2O3，将配好的料放入以酒精为介质、锆球为磨球的尼龙罐中球磨6-8h；将球磨好的料烘干过筛后并压成大块，在800℃预烧4h得到预烧粉；将预烧粉再次放入球磨罐中研磨10-12h，烘干后过筛；将过筛后的粉压成直径为12mm，厚度为2mm左右的圆柱体，在300Mpa下等静压下成型；将成型后的试样在1100-1200℃下烧结4h；对烧结成瓷的试样进行打磨和抛光，超声清洗后涂覆银浆，在550℃下保温30min烧成银电极。通过测试材料在45kV cm-1电场下动态压电常数d33 *可达810pm/V。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种高应变钛酸铋钠基陶瓷，其特征在于，所述高应变钛酸铋钠基陶瓷的化学计量比为：0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3；x＝0.006-0.012。
2.一种如权利要求1所述高应变钛酸铋钠基陶瓷的制备方法，其特征在于，所述高应变钛酸铋钠基陶瓷的制备方法包括以下步骤：
步骤一，根据0.8(BiNa)0.5-x(LaLi)xTiO3-0.2Bi0.5K0.5TiO3化学配比称量一定量的分析纯Bi2O3，Na2CO3、TiO2、K2CO3、Li2CO3和La2O3；
步骤二，将配好的料放入以酒精为介质、锆球为磨球的尼龙罐中球磨6h-8h；
步骤三，将球磨好的料烘干过筛后并压成大块，在800℃预烧4h-6h得到预烧粉；
步骤四，将预烧粉再次放入球磨罐中研磨10h-12h，烘干后过筛；
步骤五，将过筛后的粉压成直径为12mm，厚度为2mm的圆柱体，在300Mpa下等静压下成型；
步骤六，将成型后的试样在1100℃-1200℃下烧结4h-6h；
步骤七，对烧结成瓷的试样进行打磨和抛光，超声清洗后涂覆银浆，在550℃下保温30min烧成银电极。
3.一种由权利要求1所述高应变钛酸铋钠基陶瓷制造的传感器。
4.一种由权利要求1所述高应变钛酸铋钠基陶瓷制造的制动器。
5.一种由权利要求1所述高应变钛酸铋钠基陶瓷制造的换能器。
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| CN112341192B (zh) * | 2020-11-20 | 2022-07-22 | 西安合容新能源科技有限公司 | 一种高储能密度钛酸铋钠基无铅介质材料及其制备方法 |
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