CN105753467A - 一种三元材料、其制备方法及应用 - Google Patents
一种三元材料、其制备方法及应用 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims description 8
- 229910002902 BiFeO3 Inorganic materials 0.000 claims abstract description 3
- 229910003781 PbTiO3 Inorganic materials 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 26
- 239000011230 binding agent Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 239000000696 magnetic material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000005408 paramagnetism Effects 0.000 abstract description 4
- 239000003990 capacitor Substances 0.000 abstract description 2
- 230000005621 ferroelectricity Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000000634 powder X-ray diffraction Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 230000005291 magnetic effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000005690 magnetoelectric effect Effects 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000007775 ferroic material Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002902 ferrimagnetic material Substances 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920005596 polymer binder Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 206010063401 primary progressive multiple sclerosis Diseases 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
本申请公开了一种三元材料，其特征在于，所述三元材料具有钙钛矿型结构，包含BiFeO3、PbTiO3和NdFeO3三元复合体系。该三元材料稳定性强，具有压电性、铁电性和顺磁性，可应用于压电传感器、存储器、高性能电容器等相关领域。
Description
技术领域
本申请涉及一种三元材料、其制备方法及应用，属于功能材料领域。
背景技术
早在1894年P·居里就利用对称性的理论预测自然界中存在磁电效应。1960年科学家们发现了单晶Cr2O3在80K到330K的温度范围内存在磁电效应，由此引发了寻找磁电效应的热潮，并相继在混合钙钛矿型磁性铁电材料，反铁磁材料和亚铁磁材料中发现了极弱的磁电效应。1970年，Aizu根据铁电、铁磁、铁弹三种性质有一系列的相似点将其归结为一类，提出了铁性材料(Ferroics)的概念。1994年瑞士的Schmid明确提出了多铁性材料(Multi-Ferroic)的概念，指具有两种或两种以上初级铁性体特征的单相化合物。在香山科学会议第306次学术讨论会上，专家系统地介绍了铁酸铋－钛酸铅固溶体系的改性及多铁性。研究结果表明镧、镓等阳离子改性的铁酸铋－钛酸铅固溶陶瓷体系各方面性能都有明显改善和提高。在该体系的准同型相界处，其结构、电学、磁学等性能可以通过组分设计进行剪裁，同铁酸铋单晶相比表现出显著提高的极化和磁化能力。在应用方面该类材料可用于新型传感器、驱动器等电子器件。
然而到目前为止，与铁酸铋－钛酸铅相关的三元体系的报道却少之又少，并且这些离子的改性对磁学和电学的提高也是有限的，因此，探索新的对铁酸铋－钛酸铅二元体系的改性方法来提高其电学和磁学性能是必要的。
发明内容
本申请的目的在于提供一种新型的三元材料，该材料稳定性强，具有压电性、铁电性和顺磁性，可应用于压电传感器、存储器、高性能电容器等相关领域。
所述三元材料，其特征在于，所述三元材料具有钙钛矿型结构，包含BiFeO3、PbTiO3和NdFeO3三元复合体系。
优选地，所述三元材料的化学组成为：
xBiFeO3—yNdFeO3—zPbTiO3
其中，x代表三元材料中BiFeO3所占的摩尔分数，x＝0.14～0.58；
y代表三元材料中NdFeO3所占的摩尔分数，y＝0.08～0.2；
z代表三元材料中PbTiO3所占的摩尔分数，x+y+z＝1。
进一步优选地，x＝0.20～0.58；y＝0.08～0.2。更进一步优选地，x＝0.48～0.58；y＝0.08～0.2。
本申请的又一目的在于提供一种制备所述三元材料的方法，采用固相方法，能够简单、高收率地制备得到高纯度产品。
所述制备三元材料的方法，其特征在于，至少包括以下步骤：
a)将铅的氧化物、铋的氧化物、铁的氧化物、钕的氧化物和钛的氧化物混合均匀，得到具有如下摩尔配比的混合物I：
Pb：Bi：Fe：Nd：Ti＝z：x：(x+y)：y：z
其中，x＝0.14～0.58，y＝0.08～0.2，x+y+z＝1；
b)将步骤a)所得混合物I压片后，于750℃～950℃下焙烧后，得到前驱体；
c)将步骤b)所得的前驱体研磨后，加入粘结剂混合均匀，得到混合物II；
d)将步骤c)所得混合物II压片后，于400℃～600℃下排胶；
e)将步骤d)所得排胶后样品置于1000℃～1100℃焙烧，即得所述三元材料。
优选地，步骤a)中铅的氧化物是PbO；铋的氧化物是Bi2O3；铁的氧化物是Fe2O3；钕的氧化物是Nd2O3；钛的氧化物是TiO2。
本领域技术人员可以根据实际需要选择步骤a)中的混合方式，如机械混合、球磨混合、研磨混合等。作为一种实施方式，所述混合均匀是加入酒精混合研磨1～3小时。
优选地，步骤b)是将步骤a)所得混合物I与5MPa～12MPa压片后，于800℃～900℃下焙烧3～10小时后，即得所述三元材料。进一步优选地，所述焙烧时间为4～6小时。
作为一种实施方式，步骤b)中研磨前驱体的方式为加入酒精研磨1～3小时。
优选地，步骤c)所述粘结剂选自高分子聚合物粘结剂中的至少一种。本领域技术人员可以根据实际需要选择步骤c)中粘结剂的种类和加入量。优选地，所述粘结剂是聚乙烯醇(简写为PVA)粘结剂。粘结剂在固相中所占的重量百分含量为2％～5％。
优选地，步骤d)所述混合物II压片的压力为10～20MPa。进一步优选地，所述混合物II压片的压力为10～15MPa。
优选地，步骤d)所述排胶的时间不低于1小时。进一步优选地，步骤d)所述排胶时间是1～3小时。
优选地，步骤e)所述焙烧的时间不低于2小时。进一步优选地，步骤e)所述焙烧的时间是3～5小时。
本申请的又一目的在于提供一种压电材料，其特征在于，包含上述的三元材料、根据上述任意方法制备得到的三元材料中的至少一种。
本申请的又一目的在于提供一种磁性材料，其特征在于，包含上述的三元材料、根据上述任意方法制备得到的三元材料中的至少一种。
本申请的又一目的在于提供一种弛豫型铁电材料，其特征在于，包含上述的三元材料、根据上述任意方法制备得到的三元材料中的至少一种。
本申请的有益效果包括但不限于：
(1)本申请提供了一种新型的三元材料，具有很好的研究价值和实用价值。
(2)本申请提供的三元材料，稳定性强。
(3)本申请提供的三元材料，居里温度从246℃～411℃；三元材料的矫顽场得到有效降低，从9.12kV/cm～45.31kV/cm；压电系数达到143pC/N。
(4)本申请提供的三元材料的制备方法，采用固体合成方法，能够简单和高收率的得到高纯度样品。
附图说明
图1是样品F1#～F6#的XRD衍射图谱。
图2是样品P1#的介电温谱。
图3是样品P1#～P6#的电滞回线。
图4是样品F1#～F5#的磁滞回线。
图5是样品F1#～F4#的M-T曲线；其中(a)是磁化率与温度的曲线；(b)是磁化率的倒数与温度的曲线。
具体实施方式
下面结合实施例，进一步阐述本申请。应理解，这些实施例仅用于说明本发明而不用于限制本申请的范围。下列实施例中未注明具体条件的实验方法，通常按照常规条件或按照制造厂商所建议的条件。未做特殊说明的情况下，本申请所使用原料，均通过商业途径购买，不经特殊处理直接使用。
实施例1样品P1#～P9#和F1#～F9#的制备
样品P1#～P9#的制备过程如下
a)将PbO、Bi2O3、Fe2O3、Nd2O3和TiO2加入酒精混合研磨两小时，得到具有如下摩尔配比的混合物I：Pb：Bi：Fe：Nd：Ti＝z：x：(x+y)：y：z，z＝1-x-y；
b)将步骤a)所得混合物I压片和焙烧后，得到前驱体；
c)将步骤b)所得的前驱体加入酒精混合研磨两小时，加入5％PVA粘结剂混合均匀，得到混合物II；
d)将步骤c)所得混合物II在12MPa下压片后，于400℃～600℃下排胶；
e)将步骤d)所得排胶后样品置于1000℃～1100℃焙烧4小时，即得所述三元材料的陶瓷样品片，分别记为样品P1#～P9#。
样品的配料比例、具体制备条件与样品编号的关系如表1所示。
将步骤e)所得陶瓷样品片P1#～P9#分别研磨成粉，所得粉状样品分别记为样品F1#～F9#。
表1
a:PVA在混合物II固相的中所占的重量百分含量。
实施例2样品的结构表征
采用X－射线粉末衍射(XRD)方法对样品F1#～F9#的结构进行表征。所用仪器为日本RIGAKU－DMAX2500粉末衍射仪(Cu靶，λ＝0.154056nm，石墨单色仪)，具体测试条件为室温下，测量角度范围为10-80°，采用的步长为0.02°(2θ)，时间2s每步长。
样品F1#～F6#的XRD图谱如图1所示。由图可以看出，样品F1#～F6#的XRD图谱上具有钙钛矿型结构的特征衍射峰，样品F1#～F6#均是具有钙钛矿型结构的高纯度样品。样品F7#～F9#的XRD图谱与样品F1#的图谱类似，即峰位置基本相同，依据合成条件不同，峰强度在±10％的范围内变化。
实施例3样品的电学性能测定
将陶瓷样品片P1#～P9#磨薄为0.4～0.6mm，抛光后两面涂银胶，用于电学性能的测定。
样品介电性的测量在阿尔法介电/阻抗高分辨率分析仪(Novolcontrol,German)上进行，测温范围30～500℃，频率范围1～10kHz，小信号测试电压1Vrms。
样品铁电性的测量在德国aixACCT公司生产的TF2000标准铁电测量系统，温度条件为室温，所加频率为10Hz。
结果如图2和图3所示，图2是样品P1#的介电温谱；图3是样品P1#～P6#的电滞回线。由图可以看出，此三元体系具有典型的弛豫铁电体特征。
实施例4样品的磁学性能测定
样品F1#～F5#的磁滞回线在美国QuantumDesign公司生产的PPMS-10T系统上测试，测试在2K下进行，结果如图4所示。由图可以看出，此三元体系具有顺磁性
样品F1#～F4#的M-T曲线在美国QuantumDesign公司生产的MPMS-XL仪器上测试，温度范围是从0K-300K。
结果如图5所示，图5(a)是磁化率与温度的曲线；图5(b)是磁化率的倒数与温度的曲线。由图可以看出，此三元体系具有顺磁性。
以上所述，仅是本申请的几个实施例，并非对本申请做任何形式的限制，虽然本申请以较佳实施例揭示如上，然而并非用以限制本申请，任何熟悉本专业的技术人员，在不脱离本申请技术方案的范围内，利用上述揭示的技术内容做出些许的变动或修饰均等同于等效实施案例，均属于技术方案范围内。
Claims (10)
1.一种三元材料，其特征在于，所述三元材料具有钙钛矿型结构，包含BiFeO3、PbTiO3和NdFeO3三元复合体系。
2.根据权利要求1所述的三元材料，其特征在于，所述三元材料的化学组成为：
xBiFeO3—yNdFeO3—zPbTiO3
其中，x代表三元材料中BiFeO3所占的摩尔分数，x＝0.14～0.58；
y代表三元材料中NdFeO3所占的摩尔分数，y＝0.08～0.2；
z代表三元材料中PbTiO3所占的摩尔分数，x+y+z＝1。
3.根据权利要求2所述的三元材料，其特征在于，x＝0.20～0.58；y＝0.08～0.20。
4.制备权利要求1至3任一项所述三元材料的方法，其特征在于，至少包括以下步骤：
a)将铅的氧化物、铋的氧化物、铁的氧化物、钕的氧化物和钛的氧化物混合均匀，得到具有如下摩尔配比的混合物I：
Pb：Bi：Fe：Nd：Ti＝z：x：(x+y)：y：z
其中，x＝0.14～0.58，y＝0.08～0.2，x+y+z＝1；
b)将步骤a)所得混合物I压片后，于750℃～950℃下焙烧后，得到前驱体；
c)将步骤b)所得的前驱体研磨后，加入粘结剂混合均匀，得到混合物II；
d)将步骤c)所得混合物II压片后，于400℃～600℃下排胶；
e)将步骤d)所得排胶后样品置于1000℃～1100℃焙烧，即得所述三元材料。
5.根据权利要求4所述的方法，其特征在于，步骤b)是将步骤a)所得混合物I与5MPa～12MPa压片后，于800℃～900℃下焙烧3～10小时后，即得所述三元材料。
6.根据权利要求4所述的方法，其特征在于，步骤c)所述混合物II中，粘结剂在固相中所占的重量百分含量为2％～5％。
7.根据权利要求4所述的方法，其特征在于，步骤d)所述排胶的时间不低于1小时；步骤e)所述焙烧的时间不低于3小时。
8.一种压电材料，其特征在于，包含权利要求1至3任一项所述的三元材料、根据权利要求4至7任一项所述方法制备得到的三元材料中的至少一种。
9.一种磁性材料，其特征在于，包含权利要求1至3任一项所述的三元材料、根据权利要求4至7任一项所述方法制备得到的三元材料中的至少一种。
10.一种弛豫型铁电材料，其特征在于，包含权利要求1至3任一项所述的三元材料、根据权利要求4至7任一项所述方法制备得到的三元材料中的至少一种。
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| CN106866144A (zh) * | 2017-02-27 | 2017-06-20 | 西安交通大学 | 一种低温烧结超低温宽温稳定性电容器陶瓷及制备方法 |
| CN109704765A (zh) * | 2019-03-07 | 2019-05-03 | 哈尔滨工业大学 | 具有准同型晶相结构的高致密化铁电陶瓷及其制备方法 |
| JP2020522878A (ja) * | 2017-05-12 | 2020-07-30 | ザール テクノロジー リミテッドＸａａｒ Ｔｅｃｈｎｏｌｏｇｙ Ｌｉｍｉｔｅｄ | セラミック |
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| CN113173783A (zh) * | 2021-04-28 | 2021-07-27 | 桂林电子科技大学 | 钙钛矿结构的铁氧体吸波材料与制备方法 |
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| CN106866144B (zh) * | 2017-02-27 | 2020-03-17 | 西安交通大学 | 一种低温烧结超低温宽温稳定性电容器陶瓷及制备方法 |
| JP2020522878A (ja) * | 2017-05-12 | 2020-07-30 | ザール テクノロジー リミテッドＸａａｒ Ｔｅｃｈｎｏｌｏｇｙ Ｌｉｍｉｔｅｄ | セラミック |
| JP7297680B2 (ja) | 2017-05-12 | 2023-06-26 | ザール テクノロジー リミテッド | セラミック |
| CN109704765A (zh) * | 2019-03-07 | 2019-05-03 | 哈尔滨工业大学 | 具有准同型晶相结构的高致密化铁电陶瓷及其制备方法 |
| CN112745115A (zh) * | 2021-01-11 | 2021-05-04 | 电子科技大学 | 低磁场域下高应变灵敏度的磁致伸缩材料及其制备方法 |
| CN113173783A (zh) * | 2021-04-28 | 2021-07-27 | 桂林电子科技大学 | 钙钛矿结构的铁氧体吸波材料与制备方法 |
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