CN110128139A - 一种具有高压电和高铁电性能的knn基陶瓷及其制备方法 - Google Patents
一种具有高压电和高铁电性能的knn基陶瓷及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 11
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 10
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims 2
- 230000005611 electricity Effects 0.000 claims 2
- 238000003801 milling Methods 0.000 claims 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 2
- 108010010803 Gelatin Proteins 0.000 claims 1
- 229920000159 gelatin Polymers 0.000 claims 1
- 239000008273 gelatin Substances 0.000 claims 1
- 235000019322 gelatine Nutrition 0.000 claims 1
- 235000011852 gelatine desserts Nutrition 0.000 claims 1
- 229910052808 lithium carbonate Inorganic materials 0.000 claims 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims 1
- 230000010287 polarization Effects 0.000 abstract description 18
- 230000002269 spontaneous effect Effects 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 150000002739 metals Chemical class 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 41
- 238000001228 spectrum Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
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Abstract
本发明公开了一种具有高压电和高铁电性能的KNN基陶瓷及其制备方法，属于压电材料的技术领域。本发明要解决现有KNN基陶瓷压电性能和铁电性能差的技术问题。本发明所述KNN基陶瓷的通式为(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2。本发明在KNN陶瓷中掺杂了Li2CO3、Ta2O5、MnO2金属，通过在1126℃下烧结下制成。本发明中的(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的压电性能d33＝251pC/N，自发极化强度为Ps＝25.525μC/cm2，矫顽场Ec＝10.77kV/cm。
Description
技术领域
本发明属于压电材料的技术领域；具体涉及一种具有高压电和高铁电性能的KNN基陶瓷及其制备方法。
背景技术
压电材料主要应用在医疗、工业检测、铁路运输、海洋通讯与探测、核电站安全、航天航空精密传动等领域。由于之前人们所研究的大部分是铅基压电材料，但铅基压电材料会对环境造成严重的污染，使得无铅压电陶瓷成为了当今社会研究的主流。无铅压电材料主要包括BaTiO3基、Bi1/2Na1/2TiO3(BNT)基、铋层状结构、(K,Na)NbO3基(KNN)材料。
其中，铌酸钾钠(KNN)基陶瓷是由反铁电体NaNbO3和铁电体KNbO3固溶而成的具有钙钛矿结构的压电材料。当K：Na＝1：1时，为该体系的准同型相界。其室温下为正交相。KNN陶瓷具有居里温度高(约为420℃)，压电常数高(约为120～160pC/N)，机电耦合性能高等优点，但是它也有一系列的缺点：压电性能无法达到商业化的要求，烧结温区较窄(约为10℃～20℃)，难以成瓷，导致普通的烧结制备困难；高温烧结KNN陶瓷时，K+与Na+容易挥发，导致陶瓷的铁电性较差，同时还导致陶瓷的致密性较差，影响陶瓷的漏电流较大。
虽然二元体系KNLNT陶瓷的压电性能虽然比纯KNN基陶瓷的有了一些提高，但是与实际应用还是有着相当的距离的。
发明内容
本发明要解决现有KNN基陶瓷压电性能和铁电性能差从而导致其很难实际应用的技术问题；而提供了一种具有高压电和高铁电性能的KNN基陶瓷及其制备方法。
了解决上述技术问题，本发明中一种具有高压电和高铁电性能的KNN基陶瓷的通式为(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2；所述KNN基陶瓷制备方法是通过下述步骤进行的：
步骤一、按照(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3的化学计量比分别称量原料Na2CO3、K2CO3、Nb2O5、Li2CO3、Ta2O5，然后用无水乙醇湿法球磨，烘干后研磨，压片；
步骤二、然后置于氧化铝坩埚中，在900℃条件下保温4h，研碎；
步骤三、然后加入K2CO3、Na2CO3、MnO2，研磨至均匀，再加入无水乙醇，湿法球磨，烘干；
步骤四、加入PVA胶液后研磨至均匀，在干燥环境下放置，依次过100目和160目筛，选取100目～160目的粉体进行压片处理，得到料片A；
步骤五、向氧化铝坩埚中均匀地铺上一层步骤四通过160目筛的粉料，然后放入步骤四获得的料片A，再在料片A的上表面上均匀地铺上一层步骤四通过160目筛的粉料；
步骤六、然后在1126℃下烧结，保温5h，随炉冷却至室温，得到KNN基陶瓷；
其中，步骤三中K2CO3加入量是步骤一所述原料总重量的1.5％，Na2CO3加入量是步骤一所述原料总重量的1.5％，MnO2加入量是步骤一所述原料总重量的0.1％。
进一步地限定，步骤一中球磨工艺参数：转速为300r/min，球磨时间为12h，球料比1:3。
进一步地限定，步骤一在80℃条件下烘干。
进一步地限定，步骤三中球磨工艺参数：转速为300r/min，球磨时间为12h，球料比1:3。
进一步地限定，步骤三所述PVA胶液浓度为5wt％，是由PVA和水配置的。
进一步地限定，步骤三按1g粉体加入1滴PVA胶液配比加入PVA胶液。
进一步地限定，步骤三中在干燥环境下放置12h。
本发明中的(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的压电性能d33＝251pC/N，自发极化强度为Ps＝25.525μC/cm2，而(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的d33＝150pC/N，自发极化强度为Ps＝19.862μC/cm2。本发明改善了(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的压电性能并提高了其铁电性能。同时，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的矫顽场也出现了一定程度的减小，Ec＝10.77kV/cm，进一步缓解了该体系陶瓷极化困难的问题。
附图说明
图1是(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3的P-E曲线；
图2是(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2的P-E曲线；
图3是(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的XRD图谱；
图4是(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的XRD图谱；
图5是(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷极化后的介电温谱；
图6是(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷极化后的介电温谱，图6中1——εr，2——tanδ。
具体实施方式
实施例1：本实施例中一种具有高压电和高铁电性能的KNN基陶瓷的通式为(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2；其具体是通过下述步骤制备的：
步骤一、按照(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3的化学计量比分别称量原料质量纯度为99.50％Na2CO3、质量纯度为99.00％的K2CO3、质量纯度为99.90％Nb2O5、质量纯度为99.99％的Li2CO3、质量纯度为99.50％的Ta2O5，然后用无水乙醇湿法球磨，在80℃下烘干10h后研磨10min，压片；
步骤一中球磨工艺参数：转速为300r/min，球磨时间为12h，球料比1:3。
步骤二、然后置于氧化铝坩埚中，在900℃条件下保温4h，研碎；
步骤三、然后加入质量纯度为99.00％的K2CO3、质量纯度为99.50％的Na2CO3、质量纯度为99.9％的MnO2，研磨至均匀，再加入无水乙醇，湿法球磨，在80℃下烘干10h；
步骤一中球磨工艺参数：转速为300r/min，球磨时间为12h，球料比1:3。
步骤四、按1g粉体(是指步骤三处理后的粉体)加入1滴PVA胶液配比加入PVA胶液加入浓度为5wt％的PVA胶液后研磨至均匀，在干燥环境下放置12h，依次过100目和160目筛，选取100目～160目的粉体(即粒径在0.097～0.15mm的粉体)进行压片处理，得到料片A；
步骤五、向氧化铝坩埚中均匀地铺上一层步骤四通过160目筛的粉料，然后放入步骤四获得的料片A，再在料片A的上表面上均匀地铺上一层步骤四通过160目筛的粉料；
步骤六、然后在1126℃下烧结，保温5h，随炉冷却至室温，得到KNN基陶瓷；
其中，步骤三中K2CO3加入量是步骤一所述原料总重量的1.5％，Na2CO3加入量是步骤一所述原料总重量的1.5％，MnO2加入量是步骤一所述原料总重量的0.1％。
不同KNN基陶瓷的压电性能如表1所示：
表1各陶瓷的压电性能
| Ceramics | KNN | KNLNT | KNLNT-0.1MnO<sub>2</sub> |
| d<sub>33</sub>(pC/N) | 80 | 165 | 251 |
由表1可知纯的KNN陶瓷的压电性能为d33＝80pC/N，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的压电性能为d33＝165pC/N，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的压电性能为d33＝251pC/N，通过对比这几个陶瓷的压电常数，我们可以看出(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3的压电性能是要高于KNN陶瓷的，而在掺杂了0.1mol％MnO2之后，它的压电性能有了进一步的提高。
不同KNN基陶瓷的压电性能如表2所示：
表2各陶瓷的铁电性能
| Ceramics | KNN | KNLNT | KNLNT-0.1MnO<sub>2</sub> |
| P<sub>s</sub>(μC/cm<sup>2</sup>) | 10.464 | 15.622 | 25.525 |
| P<sub>r</sub>(μC/cm<sup>2</sup>) | 8.625 | 12.007 | 20.591 |
| E<sub>c</sub>(kV/cm) | 21.39 | 11.21 | 10.77 |
由表2可知，纯的KNN陶瓷的自发极化强度为Ps＝10.464μC/cm2，剩余极化强度Pr＝8.625μC/cm2，矫顽场为Ec＝21.39kV/cm。(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的自发极化强度为Ps＝15.622μC/cm2，剩余极化强度Pr＝12.007μC/cm2，矫顽场为Ec＝11.21kV/cm。而(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的自发极化强度为Ps＝25.525μC/cm2，剩余极化强度Pr＝20.591μC/cm2,矫顽场为Ec＝10.77kV/cm。MnO2有着优异的软化特性，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的铁电性能好。
(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3的P-E曲线如图1所示，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2的P-E曲线如图2所示；可知，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的自发极化强度为Ps＝15.622μC/cm2，剩余极化强度Pr＝12.007μC/cm2，矫顽场为Ec＝11.21kV/cm。而(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的自发极化强度为Ps＝25.525μC/cm2，剩余极化强度Pr＝12.20.591μC/cm2,矫顽场为Ec＝10.77kV/cm。可以看到，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷比K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的铁电性能好。
(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷的XRD图谱如图3所示；从图3中可以看出，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷无杂峰且为钙钛矿结构。样品的正交相与四方相共存。(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷的XRD图谱如图4所示；从图4中可以看出，(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷无杂峰且为钙钛矿结构。在室温时，样品的正交相与四方相共存，但正交相占据主导位置。
(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3陶瓷(KNLNT陶瓷)极化后的介电温谱如图5所示；从图5中可以看出，KNLNT陶瓷的相变温度在室温以下，居里温度在320℃左右。(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷极化后的介电温谱如图6所示。从图6中可以看出，K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2陶瓷(KNLNT-0.1MnO2陶瓷)的相变温度在60℃左右，居里温度在350℃左右，可以看到，相较KNLNT陶瓷，它的温区均向右位移。
Claims (8)
1.一种具有高压电和高铁电性能的KNN基陶瓷，其特征在于所述KNN基陶瓷的通式为(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3:0.1％MnO2。
2.如权利要求1所述的一种具有高压电和高铁电性能的KNN基陶瓷的制备方法，其特征在于所述制备方法是通过下述步骤实现的：
步骤一、按照(K0.48Na0.48Li0.04)(Nb0.8Ta0.2)O3的化学计量比分别称量原料Na2CO3、K2CO3、Nb2O5、Li2CO3、Ta2O5，然后用无水乙醇湿法球磨，烘干后研磨，压片；
步骤二、然后置于氧化铝坩埚中，在900℃条件下保温4h，研碎；
步骤三、然后加入K2CO3、Na2CO3、MnO2，研磨至均匀，再加入无水乙醇，湿法球磨，烘干；
步骤四、加入PVA胶液后研磨至均匀，在干燥环境下放置，依次过100目和160目筛，选取100目～160目的粉体进行压片处理，得到料片A；
步骤五、向氧化铝坩埚中均匀地铺上一层步骤四通过160目筛的粉料，然后放入步骤四获得的料片A，再在料片A的上表面上均匀地铺上一层步骤四通过160目筛的粉料；
步骤六、然后在1126℃下烧结，保温5h，随炉冷却至室温，得到KNN基陶瓷；
其中，步骤三中K2CO3加入量是步骤一所述原料总重量的1.5％，Na2CO3加入量是步骤一所述原料总重量的1.5％，MnO2加入量是步骤一所述原料总重量的0.1％。
3.根据权利要求2所述制备方法，其特征在于步骤一中球磨工艺参数：转速为300r/min，球磨时间为12h，球料比1:3。
4.根据权利要求2所述制备方法，其特征在于步骤一在80℃条件下烘干。
5.根据权利要求2所述制备方法，其特征在于步骤三中球磨工艺参数：转速为300r/min，球磨时间为12h，球料比1:3。
6.根据权利要求2所述制备方法，其特征在于步骤三所述PVA胶液浓度为5wt％，是由PVA和水配置的。
7.根据权利要求2所述制备方法，其特征在于步骤三按1g粉体加入1滴PVA胶液配比加入PVA胶液。
8.根据权利要求2所述制备方法，其特征在于步骤三中在干燥环境下放置12h。
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