CN110877978B - 氧化物(Na0.5Bi0.5)1-xMexTiO3稀磁铁电半导体陶瓷及其制备方法 - Google Patents
氧化物(Na0.5Bi0.5)1-xMexTiO3稀磁铁电半导体陶瓷及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 77
- 239000004065 semiconductor Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 75
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 60
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 54
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000002156 mixing Methods 0.000 claims abstract description 43
- 238000001035 drying Methods 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 30
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 50
- 230000003287 optical effect Effects 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 24
- 239000000243 solution Substances 0.000 description 13
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 12
- 238000011056 performance test Methods 0.000 description 12
- 230000002194 synthesizing effect Effects 0.000 description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- 229910003237 Na0.5Bi0.5TiO3 Inorganic materials 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种氧化物(Na0.5Bi0.5)1‑ x Me x TiO3稀磁铁电半导体陶瓷及其制备方法,其组成通式为:(Na0.5Bi0.5)1‑x Me x TiO3,其中0.02≤x≤0.1,Me为Ni、Co、Fe、Mn中的一种,该陶瓷的制备方法步骤为:1)按(1‑x)/2:(1‑x)/2:x:1的摩尔比例称取高纯度的Bi2O3:Na2CO3:MeO:TiO2粉体原料,以无水乙醇为介质置于行星球磨机中充分混合后取出干燥、研磨,再煅烧合成(Na0.5Bi0.5)1‑x Me x TiO3粉体;2)将(Na0.5Bi0.5)1‑ x Me x TiO3粉体与质量浓度为5%的PVA溶液混合均匀,烘干,研磨成粉末,将粉末压制成陶瓷坯体;3)将陶瓷坯体高温烧结,即得到氧化物(Na0.5Bi0.5)1‑x Me x TiO3稀磁铁电半导体陶瓷。该(Na0.5Bi0.5)1‑x Me x TiO3稀磁铁电半导体陶瓷可用于制造光电器件、光传感器、光探测器、光伏器件和多功能电磁器件等领域中。
Description
技术领域
本发明属于功能陶瓷制造领域,具体涉及到一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷及其制备方法。
背景技术
氧化物稀磁铁电半导体陶瓷是指非磁性氧化物铁电半导体陶瓷中部分原子被过渡金属元素取代后的功能陶瓷,它同时具有磁性、铁电性和半导体特性。可应用于集成电路、存储器、光电器件、光传感器等高新技术领域。要想获得稀磁铁电半导体材料,常采用磁性材料、铁电体和半导体组合构成,而这带来了复杂的器件设计。钙钛矿结构的Na0.5Bi0.5TiO3是一种优良的氧化物铁电体,在室温下为三方结构,它具有较高的居里温度(约320℃)以及较好的铁电性等优点,一直被认为是铅基铁电材料的替代品之一。然而,纯的Na0.5Bi0.5TiO3仅具有铁电压电性和高达3.2eV以上的光学带隙,对太阳光的可见光波段不具有响应性;同时,纯的Na0.5Bi0.5TiO3没有磁性,不具有磁调节功能。为解决这个问题,因而有了如下发明。
发明内容
本发明的目的在于克服现有技术的不足,而提供一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷及其制备方法,该陶瓷采用MeTiO3(Me = Ni、Co、Fe、Mn)与纯Na0.5Bi0.5TiO3进行固溶,通过的固相烧结法制备得(Na0.5Bi0.5)1-x Me x TiO3氧化物稀磁铁电半导体功能陶瓷。
实现本发明目的的技术方案是:
一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷,其组成通式为:(Na0.5Bi0.5)1-x Me x TiO3,其中x为摩尔分数,0.02≤x≤0.1,Me为Ni、Co、Fe、Mn中的至少一种。
一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷的制备方法,包括如下步骤:
1)按(1-x)/2:(1-x)/2:x:1的摩尔比例称取高纯度的Bi2O3、Na2CO3、MeO、TiO2粉体原料,以无水乙醇为介质置于行星球磨机中充分混合后取出干燥、研磨,再煅烧合成(Na0.5Bi0.5)1-x Me x TiO3粉体;
2)将(Na0.5Bi0.5)1-x Me x TiO3粉体与质量浓度为5%的PVA溶液混合均匀,烘干,研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体高温烧结,即得到氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷。
步骤1)中,所述的煅烧,是850℃下保温2小时。
步骤3)中,所述的高温烧结,是1075~1125℃下保温2小时。
本发明提供的一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷及其制备方法,将Na0.5Bi0.5TiO3与MeTiO3(Me = Ni、Co、Fe、Mn)固溶能形成稀磁铁电半导体,经测试具有一定的光伏效应,其铁电剩余极化(P r )介于29.2~51.8μC/cm2,光学带隙值(E g)介于1.12~2.76eV,短路光电流密度(J sc)介于0.74~2.70 nA/cm2,饱和磁化强度(M)介于35.4~100.8menu/g。这种单一物相就具有稀磁铁电半导体特征的氧化物材料,在当前各种氧化物铁电材料中并不多见,该(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷可用于制造光电器件、光传感器、光探测器、光伏器件和多功能电磁器件等领域中。
具体实施方式
下面结合具体实施例对本发明内容做进一步阐述,但不是对本发明的限定。
实施例1:
1)选择高纯度的NiO(98%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:NiO:TiO2=0.49:0.49:0.02:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.49Bi0.49Ni0.02TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀,烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1075℃下保温2小时,即得到Na0.49Bi0.49Ni0.02TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.49Bi0.49Ni0.02TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例2:
1)选择高纯度的NiO(98%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:NiO:TiO2=0.47:0.47:0.06:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.47Bi0.47Ni0.06TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1100℃下保温2小时,即得到Na0.47Bi0.47Ni0.06TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.47Bi0.47Ni0.06TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例3:
1)选择高纯度的NiO(98%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:NiO:TiO2=0.45:0.45:0.1:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.45Bi0.45Ni0.1TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1125℃下保温2小时,即得到Na0.45Bi0.45Ni0.1TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.45Bi0.45Ni0.1TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例4:
1)选择高纯度的Co2O3(99.9%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:Co2O3:TiO2=0.49:0.49:0.02:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.49Co0.49Ni0.02TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1075℃下保温2小时,即得到Na0.49Co0.49Ni0.02TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.49Co0.49Ni0.02TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例5:
1)选择高纯度的Co2O3(99.9%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:Co2O3:TiO2=0.48:0.48:0.04:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.46Bi0.46Co0.04TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1105℃下保温2小时,即得到Na0.46Bi0.46Co0.04TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.46Bi0.46Co0.04TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例6:
1)选择高纯度的Co2O3(99.9%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:Co2O3:TiO2=0.45:0.45:0.1:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.45Bi0.45 Co 0.1TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1125℃下保温2小时,即得到Na0.45Bi0.45Co0.1TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.45Bi0.45Co0.1TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例7:
1)选择高纯度的Fe2O3(99.9%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:Fe2O3:TiO2=0.49:0.49:0.02:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.49Fe0.49Ni0.02TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1075℃下保温2小时,即得到Na0.49Fe0.49Ni0.02TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.49Fe0.49Ni0.02TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例8:
1)选择高纯度的Fe2O3(99.9%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:Fe2O3:TiO2=0.47:0.47:0.06:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.47Bi0.47Fe0.06TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1095℃下保温2小时,即得到Na0.47Bi0.47Fe0.06TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.47Bi0.47Fe0.06TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例9:
1)选择高纯度的Fe2O3(99.9%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:Fe2O3:TiO2=0.45:0.45:0.1:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.45Bi0.45Fe0.1TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1125℃下保温2小时,即得到Na0.45Bi0.45Fe0.1TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.45Bi0.45Fe0.1TiO33稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例10:
1)选择高纯度的MnO2(85%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:MnO2:TiO2=0.49:0.49:0.02:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.49Mn0.49Ni0.02TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1075℃下保温2小时,即得到Na0.49Mn0.49Ni0.02TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.49Mn0.49Ni0.02TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例11:
1)选择高纯度的MnO2(85%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:MnO2:TiO2=0.47:0.47:0.06:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.47Bi0.47Mn0.06TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1110℃下保温2小时,即得到Na0.47Bi0.47Mn0.06TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.47Bi0.47Mn0.06TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
实施例12:
1)选择高纯度的MnO2(85%)、TiO2(99.9%)、Na2CO3(99.9%)、Bi2O3(99.9%)粉末为原料,按照Bi2O3:Na2CO3:MnO2:TiO2=0.45:0.45:0.1:1的摩尔比例配料,以无水乙醇为介质将原料置于行星球磨机中充分混合24h后取出烘干、研磨,再经过850℃保温2小时合成Na0.45Bi0.45Mn0.1TiO3粉体;
2)将所得粉体与质量浓度为5%的PVA溶液混合均匀, 烘干、研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体于1125℃保温2小时,即得到Na0.45Bi0.45Mn0.1TiO3稀磁铁电半导体陶瓷;
4)将所得Na0.45Bi0.45Mn0.1TiO3稀磁铁电半导体陶瓷进行铁电性能、光学带隙、光电流和磁性能测试,性能测试结果如表1所示。
表1 各实施例制得的陶瓷性能
Claims (3)
1.一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷,其特征在于,其组成通式为:(Na0.5Bi0.5)1-x Me x TiO3,其中x为摩尔分数,0.02≤x≤0.1,Me为Ni、Co、Fe、Mn中的一种。
2.根据权利要求1所述的一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷,其特征在于,其制备方法包括如下步骤:
1)按(1-x)/4:(1-x)/4:x:1的摩尔比例称取Bi2O3、Na2CO3、MeO、TiO2粉体原料,以无水乙醇为介质置于行星球磨机中充分混合后取出干燥、研磨,再煅烧合成(Na0.5Bi0.5)1-x Me x TiO3粉体;
2)将(Na0.5Bi0.5)1-x Me x TiO3粉体与质量浓度为5%的PVA溶液混合均匀,烘干,研磨成粉末,将粉末压制成陶瓷坯体;
3)将陶瓷坯体烧结,即得到氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷;
所述的烧结,是1075~1125℃下保温2小时。
3.根据权利要求2所述的一种氧化物(Na0.5Bi0.5)1-x Me x TiO3稀磁铁电半导体陶瓷,其特征在于,步骤1)中,所述的煅烧,是850℃下保温2小时。
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