CN106986629B - 一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法 - Google Patents

一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法 Download PDF

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CN106986629B
CN106986629B CN201710298789.7A CN201710298789A CN106986629B CN 106986629 B CN106986629 B CN 106986629B CN 201710298789 A CN201710298789 A CN 201710298789A CN 106986629 B CN106986629 B CN 106986629B
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程兴旺
马帅
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Abstract

本发明涉及一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，属于陶瓷靶材制备领域。该方法制备的陶瓷靶材包括陶瓷块体和铜片两部分，适用于射频磁控溅射和脉冲激光沉积等物理方法制备铁电薄膜。本发明的制备方法包括称料、球磨、预烧、二次球磨、成型、排塑、冷等静压、二次预烧、磨片、烧结、抛光以及粘贴铜片等步骤。本发明制备出的靶材具有较高的整体导热性，能够及时消除热应力，克服了靶材在离子束和激光轰击过程中容易开裂的缺点，提高了靶材的质量。同时，本发明提高了钛酸铋基铋层状结构铁电陶瓷的化学纯度和结构纯度，有利于制备出高质量的铁电薄膜。

Description

一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法
技术领域
本发明涉及一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，特别涉及一种用于射频磁控溅射和脉冲激光沉积等物理方法制备铁电薄膜的钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，属于陶瓷靶材制备领域。
背景技术
铁电陶瓷材料具有多种重要的特性，如铁电极化转向特性、热释电性、高介电性、压电性、电光效应和非线性光学性能等，可用于制备电容器件、压力传感器、铁电存储器、波导管和光学存储器等一系列电子元器件。铁电陶瓷材料因其广阔的应用前景而备受关注，其中铁电薄膜和半导体材料集成得到的集成铁电体目前已成为凝聚态物理和固体电子学的热门课题之一。众多种类的铁电陶瓷材料中，含铅的铁电陶瓷材料因其优异的性能在应用中占主导地位。由于铅基铁电陶瓷材料在其制备、使用及废弃后处理的过程中都会给人类和生态环境带来严重的危害，各国纷纷加大对无铅铁电陶瓷材料的研究，希望能够逐渐在各领域中完全取代铅基铁电陶瓷材料。无铅压电陶瓷材料中，钛酸铋 (Bi4Ti3O12)基铋层状结构陶瓷材料具有居里温度高，介电击穿强度大，介电损耗低，抗疲劳特性好，电光性能优异等特点，有望在高温压电领域和铁电随机存储器中替代含铅铁电陶瓷材料，并且在电光效应、非线性光学等领域有广阔的应用前景。
钛酸铋基铋层状结构铁电陶瓷材料是在Bi4Ti3O12陶瓷材料的基础上对钙钛矿结构中的A位Bi离子和B位中的Ti离子进行掺杂取代得到铋层状结构陶瓷材料，其化学通式为AxBi4-xByTi3-yO12,其中A和B均为稀土元素或/和过渡金属元素的一种或两种组合，0≤x<1，0≤y<1。随着系统向集成化、轻量化和小型化方向的发展，对铁电薄膜的需求持续提高。通过射频磁控溅射法和脉冲激光沉积法等物理方法制备钛酸铋基铋层状结构薄膜时，需要钛酸铋基铋层状结构陶瓷靶材具有很高的致密度以及良好的散热能力，以防止在溅射过程中发生开裂，同时还需要靶材具有很高的纯度，以保证铁电薄膜的质量。在常压下烧结制备钛酸铋基铋层状结构陶瓷靶材的过程中，由于粉体成型时与模具在高压力下接触，陶瓷生坯上下表面很容易引入模具剥落下的杂质，杂质在烧结过程中会与陶瓷材料发生反应，并扩散至靶材内部，降低靶材的纯度。另一方面，在制备过程中，生坯表面容易吸附空气中的尘埃等杂质，降低靶材的纯度。在公开号为CN 102167585A的发明专利中，公开了一种多元素掺杂钛酸铋基无铅压电陶瓷材料的制备方法，但该方法得到的陶瓷片如果直接用于靶材，容易在高能离子束和激光轰击过程中产生热应力而出现开裂问题，同时没有解决陶瓷片表面杂质的问题，不利于制备高质量的铁电薄膜。假若在压片成型后，简单的磨去陶瓷生坯片表面层，则很容易使陶瓷生坯片破裂，并降低生坯片的密实度，产生内部裂纹等缺陷。烧结后得到的陶瓷靶材杂质通过反应已扩散致内部，无法用磨片的方式消除。
发明内容
本发明的目的在于解决钛酸铋基铋层状陶瓷靶材容易在高能离子束和激光轰击过程中开裂的问题以及制备过程中表面层引入杂质的问题，提供一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，该方法制备的陶瓷靶材适用于射频磁控溅射和脉冲激光沉积等物理方法制备铁电薄膜。
为了达到上述目的，本发明的技术方案是：
一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，该钛酸铋基铋层状结构铁电陶瓷靶材由陶瓷块体和铜片两部分组成，陶瓷块体组分包括Bi4Ti3O12体系和以Bi4Ti3O12为基础，过渡金属元素氧化物或/和稀土金属元素氧化物为掺杂剂的多元素掺杂钛酸铋基铁电陶瓷体系，制备方法包括以下步骤：
步骤一、按照钛酸铋基铋层状结构铁电陶瓷靶材的化学计量比称取原料，原料包括Bi2O3、TiO2和掺杂的过渡金属元素氧化物或/和稀土金属元素氧化物；需保证称取的Bi2O3比其理论重量多2～4wt％；
步骤二、将称取的原料在无水乙醇介质中球磨至混合均匀，球磨后得到浆料在70～100℃下烘干，得到粉体；
步骤三、将烘干后的粉体，在750～850℃下预烧1～4h；然后在无水乙醇介质中球磨，球磨后得到浆料在70～100℃下烘干，得到粉体A；
步骤四、在烘干后的粉体A中加入1～5wt％的聚乙烯醇粘结剂，在 40～100MPa下压制成型，然后在600～700℃下保温至少4h，进行排塑，得到陶瓷坯体；
步骤五、将步骤四得到的陶瓷坯体，采用冷等静压方式，在150～250MPa 压力下保压3～10min进行致密化处理，得到致密化的陶瓷坯体；再在750～800℃下预烧0.5～2h，得到预烧后的陶瓷坯体；
步骤六、将步骤五所得的预烧后的陶瓷坯体上下表面分别磨去一层，并将上下表面处理干净后，在1050～1120℃下保温1～4h进行烧结，得到陶瓷块体；
步骤七、将步骤六的陶瓷块体上下表面进行抛光处理，然后选择其中一面用导电银浆粘贴铜片，铜片的面积与陶瓷块体表面面积等大，并使陶瓷块体表面和铜片完全吻合，将银浆烘干后得到钛酸铋基铋层状结构铁电陶瓷靶材。
上述步骤三中的粉体的预烧温度为800℃，保温2h。
上述步骤四中的排塑温度为650℃，保温6h。
上述步骤六中所述的陶瓷坯体上下表面分别磨去的一层厚度大于0.05mm；
上述步骤六中的烧结温度为1100℃，保温2h。
上述步骤七中的铜片材质为紫铜，厚度为0.3～1.5mm。
有益效果
1、按照本发明获得的钛酸铋基铋层状结构铁电陶瓷靶材整体导热性高于单纯的铁电陶瓷块体，该靶材在陶瓷体受到高能粒子束和激光的轰击时，能够将轰击产生的热量通过铜片进行传导散热，在射频磁控溅射和脉冲激光沉积等物理方法制备铁电薄膜过程中，克服了因热应力集中而出现开裂的缺点。
2、本发明通过将陶瓷坯体在低于杂质与陶瓷基体的反应温度的温度下进行热处理，再磨去上下表面层的技术手段，解决了在制备过程中靶材的陶瓷块体上下表面容易引入杂质的问题，提高了陶瓷靶材的纯度，有利于制备出高质量的钛酸铋基铋层状结构铁电薄膜，为铁电薄膜的科研和商业化应用带来积极影响。
附图说明
图1是实施例1制备的钛酸铋基铋层状结构铁电陶瓷靶材陶瓷块体的XRD 图；
图2是实施例1制备的钛酸铋基铋层状结构铁电陶瓷靶材陶瓷块体的电滞回线图。
具体实施方式
下面结合实施例和附图对本发明方案进行进一步描述，但保护范围不被此限制。
实施例1
一种钛酸铋基铋层状结构铁电陶瓷靶材制备方法，该钛酸铋基铁电陶瓷掺杂剂为La2O3和TaO2，化学式为Bi3.25La0.75Ta0.09Ti2.91O12，按照该化学式计量比称取Bi2O3，TiO2，La2O3和TaO2，纯度分别为99.99wt％，99.99wt％，99.99wt％和 99.5wt％，其中Bi2O3过量3wt％，即Bi2O3＝34.316g，TiO2＝10.229g，La2O3＝5.376g 和TaO2＝0.880g。将称取的原料粉体加入无水乙醇介质中，球磨2h后，放入烘箱中80℃烘干，然后在800℃下保温2h进行预烧。预烧后得到的粉体二次球磨 1h，在80℃下烘干后，加入2wt％，即1.01g的聚乙烯醇粘结剂，其中聚乙烯醇粘结剂中的聚乙烯醇质量浓度为10％，在70MPa压力下压制成型。得到的陶瓷素坯在650℃下保温4h进行排塑，随后采用冷等静压的方式，在200MPa压力下保压5min进行致密化，将致密化的陶瓷坯体，在800℃下预烧1h。将预烧后的陶瓷坯体用细砂纸上下表面磨去一层，磨去层的厚度为0.1mm，将得到的陶瓷坯体放入无水乙醇中超声清洗，将上下表面处理干净后，在1100℃下进行烧结，保温时间2h，得到陶瓷块体。将陶瓷块体上下表面在抛光机上进行抛光处理，然后选择其中一面用导电银浆粘贴一片厚度为0.8mm的紫铜铜片，铜片的面积与陶瓷块体表面面积等大，并使陶瓷表面和铜片完全吻合，将银浆放入烘箱中150℃烘干，最终得到钛酸铋基铋层状结构铁电陶瓷靶材。将该靶材用于射频磁控溅射制备铁电薄膜的过程中，在不同的工作射频功率下，均未出现开裂的情况。
图1是实施例1制备的钛酸铋基铋层状结构铁电陶瓷靶材陶瓷块体的XRD 图，由图中可以看到该陶瓷为单一的Bi层状结构，没有杂质相出现。图2是实施例1制备的钛酸铋基铋层状结构铁电陶瓷靶材陶瓷块体的电滞回线图，由图可以看出该陶瓷的电滞回线矩形度较好，具有较好的铁电性能。
实施例2
一种钛酸铋基铋层状结构铁电陶瓷靶材制备方法，该钛酸铋基铁电陶瓷掺杂剂为La2O3化学式为Bi3.25La0.75Ti3O12，按照该化学式称取分析纯Bi2O3，TiO2和 La2O3，纯度均为99.99wt％，其中Bi2O3过量2wt％，即Bi2O3＝16.991g， TiO2＝5.271g，La2O3＝2.688g。将称取的原料粉体加入无水乙醇介质中，球磨2h 后，放入烘箱中80℃烘干，然后在800℃下保温2h进行预烧。预烧后得到的粉体二次球磨1h，在80℃下烘干后，加入3wt％，即0.75g的聚乙烯醇粘结剂，的聚乙烯醇粘结剂，其中聚乙烯醇粘结剂中的聚乙烯醇质量浓度为10％，在100MPa压力下压制成型。得到的陶瓷素坯在650℃下保温6h进行排塑，随后采用冷等静压的方式，在200MPa压力下保压5min进行致密化，将致密化的陶瓷坯体，在800℃下预烧1h。将预烧后的陶瓷坯体用细砂纸上下表面磨去一层，磨去层的厚度为0.1mm，将得到的陶瓷坯体上下表面用洗耳球吹干净后，放入氧化炉坩埚中在1100℃下进行烧结，保温时间2h，得到陶瓷块体。将陶瓷块体上下表面用抛光砂纸进行抛光处理，然后选择其中一面用导电银浆粘贴一片厚度为1mm的紫铜铜片，铜片的面积与陶瓷块体表面面积等大，并使陶瓷表面和铜片完全吻合，将银浆放入烘箱中150℃烘干，最终得到钛酸铋基铋层状结构铁电陶瓷靶材。靶材的XRD测试表明该陶瓷为纯的铋层状结构，没有杂质相出现。将该靶材用于脉冲激光沉积制备铁电薄膜的过程中，未出现开裂的情况。
实施例3
一种钛酸铋基铋层状结构铁电陶瓷靶材制备方法，该钛酸铋基铁电陶瓷化学式为Bi4Ti3O12，按照该化学式称取Bi2O3和TiO2，纯度均为99.99wt％，其中 Bi2O3过量4wt％即Bi2O3＝42.648g，TiO2＝10.543g，其余条件同实施例1。最终得到钛酸铋基铋层状结构铁电陶瓷靶材。靶材的XRD测试表明该陶瓷为纯的铋层状结构，没有杂质相出现。将该靶材用于射频磁控溅射制备铁电薄膜的过程中，未出现开裂的情况。

Claims (6)

1.一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，其特征在于：所述钛酸铋基铋层状结构铁电陶瓷靶材由陶瓷块体和铜片两部分组成，陶瓷块体组分包括Bi4Ti3O12体系和以Bi4Ti3O12为基础，过渡金属元素氧化物或/和稀土金属元素氧化物为掺杂剂的多元素掺杂钛酸铋基铁电陶瓷体系；
具体步骤如下：
步骤一、按照钛酸铋基铋层状结构铁电陶瓷靶材的化学计量比称取原料，原料包括Bi2O3、TiO2和掺杂的过渡金属元素氧化物或/和稀土金属元素氧化物；需保证称取的Bi2O3比其理论重量多2～4wt％；
步骤二、将称取的原料在无水乙醇介质中球磨至混合均匀，球磨后得到浆料在70～100℃下烘干，得到粉体；
步骤三、将烘干后的粉体，在750～850℃下预烧1～4h；然后在无水乙醇介质中球磨，球磨后得到浆料在70～100℃下烘干，得到粉体A；
步骤四、在烘干后的粉体A中加入1～5wt％的聚乙烯醇粘结剂，在40～100MPa下压制成型，然后在600～700℃下保温至少4h，进行排塑，得到陶瓷坯体；
步骤五、将步骤四得到的陶瓷坯体，采用冷等静压方式，在150～250MPa压力下保压3～10min进行致密化处理，得到致密化的陶瓷坯体；再在750～800℃下预烧0.5～2h，得到预烧后的陶瓷坯体；
步骤六、将步骤五所得的预烧后的陶瓷坯体上下表面分别磨去一层，并将上下表面处理干净后，在1050～1120℃下保温1～4h进行烧结，得到陶瓷块体；
步骤七、将步骤六的陶瓷块体上下表面进行抛光处理，然后选择其中一面用导电银浆粘贴铜片，铜片的面积与陶瓷块体表面面积等大，并使陶瓷块体表面和铜片完全吻合，将银浆烘干后得到钛酸铋基铋层状结构铁电陶瓷靶材。
2.如权利要求1所述的一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，其特征在于：所述步骤三中的粉体的预烧温度为800℃，保温2h。
3.如权利要求1所述的一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，其特征在于：所述步骤四中的排塑温度为650℃，保温6h。
4.如权利要求1所述的一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，其特征在于：所述步骤六中所述的陶瓷坯体上下表面分别磨去的一层厚度大于0.05mm。
5.如权利要求1所述的一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，其特征在于：所述步骤六中的烧结温度为1100℃，保温2h。
6.如权利要求1所述的一种钛酸铋基铋层状结构铁电陶瓷靶材的制备方法，其特征在于：所述步骤七中的铜片材质为紫铜，厚度为0.3～1.5mm。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005001987A (ja) * 2003-05-21 2005-01-06 Japan Science & Technology Agency ビスマスを構成元素に含む多元系酸化物単結晶の製造方法
CN104529435A (zh) * 2014-12-26 2015-04-22 中国科学院声学研究所 铋层状结构压电陶瓷材料及其制备方法
CN104529447A (zh) * 2014-12-26 2015-04-22 中国科学院声学研究所 铋层状复合结构压电陶瓷材料及其制备方法
CN105461303A (zh) * 2014-09-25 2016-04-06 Tdk株式会社 压电组合物、压电元件和溅射靶材

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005001987A (ja) * 2003-05-21 2005-01-06 Japan Science & Technology Agency ビスマスを構成元素に含む多元系酸化物単結晶の製造方法
CN105461303A (zh) * 2014-09-25 2016-04-06 Tdk株式会社 压电组合物、压电元件和溅射靶材
CN104529435A (zh) * 2014-12-26 2015-04-22 中国科学院声学研究所 铋层状结构压电陶瓷材料及其制备方法
CN104529447A (zh) * 2014-12-26 2015-04-22 中国科学院声学研究所 铋层状复合结构压电陶瓷材料及其制备方法

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