CN110015893A - 一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料、制备方法及其应用 - Google Patents
一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料、制备方法及其应用 Download PDFInfo
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- CN110015893A CN110015893A CN201910420021.1A CN201910420021A CN110015893A CN 110015893 A CN110015893 A CN 110015893A CN 201910420021 A CN201910420021 A CN 201910420021A CN 110015893 A CN110015893 A CN 110015893A
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- barium titanate
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- composite mixed
- ceramics material
- bismuth ferrite
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- 239000000919 ceramic Substances 0.000 title claims abstract description 72
- 239000000463 material Substances 0.000 title claims abstract description 46
- 229910002056 binary alloy Inorganic materials 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 35
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 34
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 38
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000003990 capacitor Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 27
- 150000002500 ions Chemical class 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 18
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 15
- 229910052593 corundum Inorganic materials 0.000 claims description 11
- 229910000859 α-Fe Inorganic materials 0.000 claims description 11
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 9
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 9
- 150000002736 metal compounds Chemical class 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 239000010431 corundum Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000003129 oil well Substances 0.000 claims description 3
- ZUJVZHIDQJPCHU-UHFFFAOYSA-N [Ba].[Bi] Chemical compound [Ba].[Bi] ZUJVZHIDQJPCHU-UHFFFAOYSA-N 0.000 claims description 2
- 239000000295 fuel oil Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 238000004513 sizing Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 8
- 239000007787 solid Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 description 2
- 230000005621 ferroelectricity Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 229910002902 BiFeO3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 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
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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Abstract
一种复合掺杂铁酸铋‑钛酸钡二元系无铅铁电陶瓷材料、制备方法及其应用，本发明属于无铅铁电陶瓷材料领域，具体涉及一种复合掺杂铁酸铋‑钛酸钡二元系无铅铁电陶瓷材料、制备方法及其应用。本发明要解决传统固相合成法制备的BFO陶瓷铁电性能较差、漏电严重的问题。陶瓷材料的化学通式为(1‑y)BiFeO3‑yBa1‑x(Li+ 0.5A3+ 0.5)xTiO3。本发明采用SPS快速低温烧结和固相合成相结合的烧结方式制备获得陶瓷材料，该体系为钙钛矿相，无杂相，所制备的陶瓷材料具有优良的电学性能和较高的居里温度，其制备工艺稳定，有较好的应用前景。所制备的陶瓷材料作为电子元器件用于温度稳定型电容器及高温应用领域。
Description
技术领域
本发明属于无铅铁电陶瓷材料领域，具体涉及一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料、制备方法及其应用。
背景技术
BaTiO3(BT)陶瓷是应用得最早最广泛的铁电陶瓷材料，具有良好的介电和铁电性能，在多层陶瓷电容器和微波介质等领域有较好的应用前景。然而，BT最大的问题是其居里温度很低(TC～120℃)，而且经过元素掺杂后的BT，其居里温度一般会降至室温附近甚至更低，因此这一致命缺点极大的限制了BT在其他领域的应用。相比之下，BiFeO3(BFO)的居里温度(TC～830℃)很高，尽管BFO是唯一一个在室温下同时具有铁电性和反铁磁性的多铁材料，但是BFO本征介电常数很低～60，导致其压电系数d33很小<100pC/N，远远低于其他无铅压电材料。此外BFO漏电问题严重，因此很难测到饱和的电滞回线。目前对BFO陶瓷制备主要采用的方法是传统的固相合成，应用其他特殊烧结方法比较少见。纯相BFO陶瓷存在漏电流大、矫顽场大、剩余极化小等一系列缺点。
发明内容
本发明是要解决传统固相合成法制备的BFO陶瓷铁电性能较差、漏电严重的问题，而提供一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料、制备方法及其应用。
本发明一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3，其中x和y为摩尔分数，0.005≤x≤0.06，0.1≤y≤0.35，A3+离子为Al3+、Ga3+、In3+或Er3+离子。
本发明一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法是按以下步骤完成的：
一、按化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3配比称取Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和A3+离子金属化合物，其中x和y为摩尔分数，0.005≤x≤0.06，0.1≤y≤0.35，A3+离子为Al3+、Ga3+、In3+或Er3+离子；然后将称取的Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和A3+离子金属化合物混合，得到混合料；所述A3+离子金属化合物为Al2O3、Ga2O3、Er2O3或In2O3；
二、将混合料置于球磨机中，以无水乙醇和氧化锆磨球作为球磨介质在转速为300～350r/min的条件下球磨10～15h，得到浆料，将浆料置于温度为80～120℃的条件下烘干，得到干燥粉体；
三、将干燥粉体在温度为750～800℃的条件下预烧4～6h，得到(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体；
四、将(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体过200目筛，放入直径为20mm的石墨模具中进行SPS烧结，压制成直径为20mm的圆片；
五、将步骤四得到的直径为20mm的圆片放入刚玉陶瓷坩埚中，采用步骤三相同成分的(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体进行掩埋，然后以5℃/min的升温速率将刚玉陶瓷坩埚升温至900～1050℃，在温度为900～1050℃的条件下保温1～3h，然后随炉冷却，得到(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3陶瓷。
本发明有益效果：本发明通过SPS烧结和固相合成相结合的方式制备复合掺杂铁酸铋-钛酸钡(BFO-BT)二元系无铅铁电陶瓷材料，利用SPS低温快速烧结可以明显减少Bi元素的挥发，并在相对较低的烧结温度下，获得致密的电学性能优良的BFO-BT二元系陶瓷。所制备的陶瓷材料具有优良的电学性能和较高的居里温度，制备工艺稳定，特别适合在自动燃油喷射、石油测井及航空加速度计等高温应用领域中使用。
附图说明
图1为实施例1、实施例2和实施例3制备的复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的XRD谱图；其中1为实施例1，2为实施例2，3为实施例3；
图2为实施例一、实施例二和实施例三制备的复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的室温电滞回线；其中1为实施例1，2为实施例2，3为实施例3。
具体实施方式
本发明技术方案不限于以下所列举的具体实施方式，还包括各具体实施方式之间的任意组合。
具体实施方式一：本实施方式一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3，其中x和y为摩尔分数，0.005≤x≤0.06，0.1≤y≤0.35，A3+离子为Al3+、Ga3+、In3+或Er3+离子。
具体实施方式二：本实施方式与具体实施方式一不同的是：复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3，其中x和y为摩尔分数，0.01≤x≤0.06，0.15≤y≤0.3，A3+离子为Al3+、Ga3+、In3+或Er3+离子。其他与具体实施方式一相同。
具体实施方式三：本实施方式与具体实施方式一或二不同的是：复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3，其中x和y为摩尔分数，0.02≤x≤0.04，0.2≤y≤0.25，A3+离子为Al3+、Ga3+、In3+或Er3+离子。其他与具体实施方式一或二相同。
具体实施方式四：本实施方式一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法是按以下步骤完成的：
一、按化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3配比称取Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和A3+离子金属化合物，其中x和y为摩尔分数，0.005≤x≤0.06，0.1≤y≤0.35，A3+离子为Al3+、Ga3+、In3+或Er3+离子；然后将称取的Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和A3+离子金属化合物混合，得到混合料；所述A3+离子金属化合物为Al2O3、Ga2O3、Er2O3或In2O3；
二、将混合料置于球磨机中，以无水乙醇和氧化锆磨球作为球磨介质在转速为300～350r/min的条件下球磨10～15h，得到浆料，将浆料置于温度为80～120℃的条件下烘干，得到干燥粉体；
三、将干燥粉体在温度为750～800℃的条件下预烧4～6h，得到(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体；
四、将(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体过200目筛，放入直径为20mm的石墨模具中进行SPS烧结，压制成直径为20mm的圆片；
五、将步骤四得到的直径为20mm的圆片放入刚玉陶瓷坩埚中，采用步骤三相同成分的(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体进行掩埋，然后以5℃/min的升温速率将刚玉陶瓷坩埚升温至900～1050℃，在温度为900～1050℃的条件下保温1～3h，然后随炉冷却，得到(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3陶瓷。
具体实施方式五：本实施方式与具体实施方式四不同的是：步骤四中所述SPS烧结中冷压压力为200MPa，保压时间为3～5min，烧结温度为850～900℃。其他与具体实施方式四相同。
具体实施方式六：本实施方式与具体实施方式或五不同的是：步骤一中x和y为摩尔分数，0.005≤x≤0.05，0.1≤y≤0.3。。其他与具体实施方式四或五相同。
具体实施方式七：本实施方式与具体实施方式四至六之一不同的是：步骤一中x和y为摩尔分数，0.005≤x≤0.03，0.1≤y≤0.25。其他与具体实施方式四至六之一相同。
具体实施方式八：本实施方式与具体实施方式四至七之一不同的是：步骤一中x和y为摩尔分数，0.005≤x≤0.02，0.1≤y≤0.2。其他与具体实施方式四至七之一相同。
具体实施方式九：本实施方式一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料作为电子元器件用于温度稳定型电容器及高温应用领域。
具体实施方式十：本实施方式与具体实施方式九不同的是：复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料作为电子元器件用于自动燃油喷射、石油测井或航空加速度计。其他与具体实施方式九相同。
采用下述实施例验证本发明的有益效果：
实施例1：一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，它是按照以下步骤进行的：
一、按化学通式(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3中元素的化学计量比称取原料：Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和Al2O3，其中A3+为Al3+，x＝0.01，y＝0.25；
二、将步骤一中称取的原料放入球磨机中以无水乙醇和氧化锆磨球为球磨介质进行混料，球料比为5:1，转速为300r/min，球磨时间为12h；
三、将球磨所得浆料于80℃下保温烘干12h；
四、将步骤三得到的粉体在800℃预烧5h，得到0.75BiFeO3-0.25Ba0.99(Li+ 0.5Al3 + 0.5)0.01TiO3粉体；
五、将步骤四得到的粉体过200目筛，放入直径为20mm的石墨模具中进行SPS烧结，冷压200MPa，烧结温度为900℃，保压5min，压制成直径为20mm的圆片；
六、将经过步骤五的圆片，放入刚玉陶瓷坩埚中，埋入0.75BiFeO3-0.25Ba0.99(Li+ 0.5Al3+ 0.5)0.01TiO3粉体中，以5℃/min的升温速率升温至1050℃，保温2h，然后随炉冷却，得到0.75BiFeO3-0.25Ba0.99(Li+ 0.5Al3+ 0.5)0.01TiO3陶瓷。
对获得的0.75BiFeO3-0.25Ba0.99(Li+ 0.5Al3+ 0.5)0.01TiO3二元系陶瓷样品表面进行抛光处理，样品厚度磨至1mm左右，超声清洗后双面被银电极，陶瓷样品浸入100℃的硅油中，极化20min，极化电场为2kV/mm，然后测试陶瓷样品的电学性能参数。
图1给出了陶瓷样品的XRD图，由图可见陶瓷材料为单一钙钛矿相结构，无杂相。图2为室温下陶瓷样品的电滞回线，由回线形状可知，BFO的漏电性能明显改善。部分电学性能参数见表1。
实施例2：
本实施例的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，它是按照以下步骤进行的：
一、按化学通式(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3中元素的化学计量比称取原料：Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和Ga2O3，其中A3+为Ga3+，x＝0.02，y＝0.25；
二、将步骤一中称取的原料放入球磨机中以无水乙醇和氧化锆磨球为球磨介质进行混料，球料比为5:1，转速为350r/min，球磨时间为15h；
三、将球磨所得浆料于80℃下保温烘干12h；
四、将步骤三得到的粉体在800℃预烧4h，得到0.75BiFeO3-0.25Ba0.98(Li+ 0.5Ga3 + 0.5)0.02TiO3粉体；
五、将步骤四得到的粉体过200目筛，放入直径为20mm的石墨模具中进行SPS烧结，冷压200MPa，烧结温度为900℃，保压5min，压制成直径为20mm的圆片；
六、将经过步骤五的圆片，放入刚玉陶瓷坩埚中，埋入0.75BiFeO3-0.25Ba0.98(Li+ 0.5Ga3+ 0.5)0.02TiO3粉体中，以5℃/min的升温速率升温至1000℃，保温2h，然后随炉冷却，得到0.75BiFeO3-0.25Ba0.98(Li+ 0.5Ga3+ 0.5)0.02TiO3陶瓷。
对获得的0.75BiFeO3-0.25Ba0.98(Li+ 0.5Ga3+ 0.5)0.02TiO3二元系陶瓷样品表面抛光，样品厚度磨至1mm左右，超声清洗后双面被银电极，陶瓷样品浸入100℃的硅油中，极化20min，极化电场为2kV/mm，然后测试陶瓷样品的电学性能参数。
图1给出了陶瓷样品的XRD图，由图可见陶瓷材料为单一钙钛矿相结构，无杂相。图2为室温下陶瓷样品的电滞回线，由回线形状可知，BFO的漏电性能明显改善。部分电学性能参数见表1。
实施例3：
本实施例的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，它是按照以下步骤进行的：
一、按化学通式(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3中元素的化学计量比称取原料：Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和In2O3，其中A3+为In3+，x＝0.02，y＝0.15；
二、将步骤一中称取的原料放入球磨机中以无水乙醇和氧化锆磨球为球磨介质进行混料，球料比为5:1，转速为300r/min，球磨时间为10h；
三、将球磨所得浆料于80℃下保温烘干12h；
四、将步骤三得到的粉体在780℃预烧4h，得到0.85BiFeO3-0.15Ba0.98(Li+ 0.5In3 + 0.5)0.02TiO3粉体；
五、将步骤四得到的粉体过200目筛，放入直径为20mm的石墨模具中进行SPS烧结，冷压200MPa，烧结温度为850℃，保压5min，压制成直径为20mm的圆片；
六、将经过步骤五的圆片，放入刚玉陶瓷坩埚中，埋入0.85BiFeO3-0.15Ba0.98(Li+ 0.5In3+ 0.5)0.02TiO3粉体中，以5℃/min的升温速率升温至950℃，保温2h，然后随炉冷却，得到0.85BiFeO3-0.15Ba0.98(Li+ 0.5In3+ 0.5)0.02TiO3陶瓷。
对获得的0.85BiFeO3-0.15Ba0.98(Li+ 0.5In3+ 0.5)0.02TiO3二元系陶瓷样品表面抛光，样品厚度磨至1mm左右，超声清洗后双面被银电极，陶瓷样品浸入100℃的硅油中，极化20min，极化电场为2kV/mm，然后测试陶瓷样品的电学性能参数。
图1给出了陶瓷样品的XRD图，由图可见陶瓷材料为单一钙钛矿相结构，无杂相。图2为室温下陶瓷样品的电滞回线，由回线形状可知，BFO的漏电性能明显改善。部分电学性能参数见表1。
表1实施例1至实施例3所得陶瓷样品部分电学性能参数
Claims (10)
1.一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料，其特征在于复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3，其中x和y为摩尔分数，0.005≤x≤0.06，0.1≤y≤0.35，A3+离子为Al3+、Ga3+、In3+或Er3+离子。
2.根据权利要求1所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料，其特征在于复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3，其中x和y为摩尔分数，0.01≤x≤0.06，0.15≤y≤0.3，A3+离子为Al3+、Ga3+、In3+或Er3+离子。
3.根据权利要求1所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料，其特征在于复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3，其中x和y为摩尔分数，0.02≤x≤0.04，0.2≤y≤0.25，A3+离子为Al3+、Ga3+、In3+或Er3+离子。
4.如权利要求1所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，其特征在于复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法是按以下步骤完成的：
一、按化学通式为(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3配比称取Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和A3+离子金属化合物，其中x和y为摩尔分数，0.005≤x≤0.06，0.1≤y≤0.35，A3+离子为Al3+、Ga3+、In3+或Er3+离子；然后将称取的Bi2O3、Fe2O3、BaCO3、TiO2、Li2O和A3+离子金属化合物混合，得到混合料；所述A3+离子金属化合物为Al2O3、Ga2O3、Er2O3或In2O3；
二、将混合料置于球磨机中，以无水乙醇和氧化锆磨球作为球磨介质在转速为300～350r/min的条件下球磨10～15h，得到浆料，将浆料置于温度为80～120℃的条件下烘干，得到干燥粉体；
三、将干燥粉体在温度为750～800℃的条件下预烧4～6h，得到(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体；
四、将(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体过200目筛，放入直径为20mm的石墨模具中进行SPS烧结，压制成直径为20mm的圆片；
五、将步骤四得到的直径为20mm的圆片放入刚玉陶瓷坩埚中，采用步骤三相同成分的(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3粉体进行掩埋，然后以5℃/min的升温速率将刚玉陶瓷坩埚升温至900～1050℃，在温度为900～1050℃的条件下保温1～3h，然后随炉冷却，得到(1-y)BiFeO3-yBa1-x(Li+ 0.5A3+ 0.5)xTiO3陶瓷。
5.根据权利要求4所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，其特征在于步骤四中所述SPS烧结中冷压压力为200MPa，保压时间为3～5min，烧结温度为850～900℃。
6.根据权利要求4所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，其特征在于步骤一中x和y为摩尔分数，0.005≤x≤0.05，0.1≤y≤0.3。
7.根据权利要求4所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，其特征在于步骤一中x和y为摩尔分数，0.005≤x≤0.03，0.1≤y≤0.25。
8.根据权利要求4所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的制备方法，其特征在于步骤一中x和y为摩尔分数，0.005≤x≤0.02，0.1≤y≤0.2。
9.如权利要求1所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的应用，其特征在于复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料作为电子元器件用于温度稳定型电容器及高温应用领域。
10.根据权利要求9所述的一种复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料的应用，其特征在于复合掺杂铁酸铋-钛酸钡二元系无铅铁电陶瓷材料作为电子元器件用于自动燃油喷射、石油测井或航空加速度计。
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