CN112062561A - 一种pnnzt基多相共存弛豫铁电外延薄膜的制备方法 - Google Patents
一种pnnzt基多相共存弛豫铁电外延薄膜的制备方法 Download PDFInfo
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- 238000000151 deposition Methods 0.000 claims abstract description 51
- 238000005245 sintering Methods 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000000758 substrate Substances 0.000 claims abstract description 30
- 230000008021 deposition Effects 0.000 claims abstract description 28
- 239000013077 target material Substances 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 claims abstract description 20
- 239000008187 granular material Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
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- 239000010408 film Substances 0.000 claims description 41
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- 239000010409 thin film Substances 0.000 claims description 19
- 229910002182 La0.7Sr0.3MnO3 Inorganic materials 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 10
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- 238000000137 annealing Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000011065 in-situ storage Methods 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 6
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 6
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Abstract
本发明涉及一种PNNZT基多相共存弛豫铁电外延薄膜的制备方法,属于化学工程技术领域。一种PNNZT基多相共存弛豫铁电外延薄膜的制备方法,包括以下步骤:将同为钙钛矿结构的SrTiO3(100/111)单晶基片作为衬底,采用固相合成法和激光脉冲沉积法制备钙钛矿结构的La0.7Sr0.3MnO3(100/111)外延薄膜;采用溶胶凝胶法和固相烧结法制备PNNZT靶材,将PNNZT前驱体溶液于室温下搅拌1.5‑2h,并放置24‑30h,自然风干,制得凝胶;所得凝胶干燥、煅烧、研磨、压制制得粒料,所得粒料经过烧结,自然冷却即得所需的PNNZT靶材;制得的PNNZT靶材利用激光脉冲沉积法在底电极上外延制备出多相共存的弛豫铁电外延薄膜。本发明的有益效果是获得具有纯度高、致密性好、平均晶粒尺寸小、电场击穿强度大、电卡效应大等优点的薄膜。
Description
技术领域
本发明涉及一种PNNZT基多相共存弛豫铁电外延薄膜的制备方法,属于化学工程技术领域。
背景技术
随着电子、信息和控制技术朝着微型化、高集成化方向的发展,以及高科技领域对于快速制冷的需求,高效率的固态制冷技术的发展已经被提上日程。作为压电材料的一类分支,铁电体材料因其具有在外加电场下的电卡特性使得其成为优秀候选材料。
发明内容
本发明的目的在于提供一种PNNZT基多相共存弛豫铁电外延薄膜的制备方法。PNNZT(Pb(Ni1/3Nb2/3)xZryTi1-x-yO3,x,y=0~1)是一种多相共存弛豫铁电材料,本发明通过激光脉冲沉积法在SrTiO3和La0.7Sr0.3MnO3基底上面制备出的PNNZT多相共存弛豫铁电外延薄膜。
本发明的目的通过如下技术方案实现:
一种PNNZT基多相共存弛豫铁电外延薄膜的制备方法,包括以下步骤:
1)以SrTiO3(100/111)单晶基片作为衬底,以La0.7Sr0.3MnO3为靶材,采用激光脉冲沉积法制备钙钛矿结构氧化物La0.7Sr0.3MnO3(100/111)取向的薄膜底电极;
2)采用溶胶凝胶法和固相烧结法制备PNNZT靶材,将PNNZT前驱体溶液于室温下搅拌1.5-2h,并放置24-30h,自然风干,制得凝胶;
3)将步骤2)所得凝胶干燥、煅烧、研磨、压制制得粒料,所得粒料经过烧结,自然冷却即得所需的PNNZT靶材;
4)将步骤3)制得的PNNZT靶材利用激光脉冲沉积法在La0.7Sr0.3MnO3(100/111)取向的薄膜底电极上外延制备出多相共存的弛豫铁电外延薄膜。
优选的是,步骤1)所述La0.7Sr0.3MnO3靶材可通过固相烧结方法制得,所述方法包括如下步骤:将原料La2O3、SrCO3、MnO2球磨所得的混合物烘干、预烧、冷压制备块体、烧结制得所需的靶材La0.7Sr0.3MnO3。
优选的是,步骤1)所述预烧温度为1200℃~1300℃,预烧时间为10~12小时;所述烧结温度为1350~1400℃,烧结时间为24~48小时。
优选的是,步骤1)所述激光脉冲沉积法采用的沉积温度为700℃~750℃,脉冲激光能量为5Hz,单脉冲能量为350mJ,氧气氛下沉积20~30分钟,沉积完成后原位退火35~45分钟。
优选的是,所述PNNZT通式为Pb(Ni1/3Nb2/3)xZryTi1-x-yO3,其中x,y=0~1。
优选的是,步骤2)所述PNNZT前驱体溶液浓度为0.2~0.3mol/L。
优选的是,步骤3)所述凝胶干燥温度为350-400℃,干燥时间为20-30min。
优选的是,步骤3)所述煅烧包括第一次煅烧和第二次煅烧,所述第一次煅烧温度为550-600℃,煅烧时间为20-30min,第二次煅烧温度为850-900℃,煅烧时间为1.5-2h。
优选的是,步骤3)所述研磨时间为1-2h;步骤3)所述压制工艺为300Mpa冷等静压压制,压制所得粒料直径为20mm,厚度为3mm。
优选的是,步骤3)所述烧结温度为1150-1200℃,烧结时间为4-6h,烧结环境为空气氛围。
本发明的有益效果是:获得具有纯度高、致密性好、平均晶粒尺寸小、电场击穿强度大、电卡效应大等优点的薄膜;本发明可以通过基底取向控制薄膜的结构和电卡性能,是一种方便快捷的制备技术。
附图说明
图1和图2为本发明实施例1和2得到的PNNZT薄膜的XRD图和电卡性能对比图谱。
具体实施方式
下面结合具体实施例,对本发明作进一步详细的阐述,但本发明的实施方式并不局限于实施例表示的范围。这些实施例仅用于说明本发明,而非用于限制本发明的范围。此外,在阅读本发明的内容后,本领域的技术人员可以对本发明作各种修改,这些等价变化同样落于本发明所附权利要求书所限定的范围。
实施例1
1)将同为钙钛矿结构的SrTiO3(100)单晶基片作为衬底,采用激光脉冲沉积法制备钙钛矿结构氧化物La0.7Sr0.3MnO3(100)取向的薄膜底电极;
首先按照摩尔比0.7:0.3:1分别称取分析纯的La2O3、SrCO3、MnO2作为原料,利用固相烧结的方法制备La0.7Sr0.3MnO3(LSMO)。具体的步骤如下:
(1)在烧结之前,首先按照固定的摩尔比来配比这三种粉末,将粉末放在烘箱中烘干,烘干后将其倒入球磨罐中混合,然后在球磨罐中倒入适量的去离子水,球磨4小时。
(2)将步骤(1)中球磨完成后的液体倒入表面皿,放入烘箱,烘箱温度为100℃,烘干后将粉末倒入玛瑙研钵中,研磨30分钟以上,接着将研磨充分的粉末装入坩埚中,放置于高温炉内,进行预烧,预烧温度为1200℃,时间为10小时;
(3)将步骤(2)中预烧完成后的粉末冷却,之后再倒入球磨罐中,球磨4小时,然后将粉末烘干,在粉末中加入粘合剂PVA研磨30分钟,将研磨充分的粉末放置于20MPa压力下冷压成圆形块体;
(4)将步骤(3)中的块体放入高温炉中,以1350℃烧结24个小时,得到所需的靶材La0.7Sr0.3MnO3。
2)将上述制得的靶材La0.7Sr0.3MnO3利用激光脉冲沉积法制备出延薄膜,所述薄膜的厚度为100nm。具体的步骤如下:
(1)我们选择了与LSMO同为钙钛矿结构的SrTiO3(100)单晶基片作为衬底。在沉积之前,将基片分别放入去离子水,乙醇以及丙酮中用超声波清洗10分钟,重复3次;
(2)薄膜的沉积工作。沉积过程中,采用的沉积温度为700℃,脉冲激光能量为5Hz,单脉冲能量为350mJ,在40Pa的氧气氛下沉积20分钟,沉积完成后原位退火35分钟。之后就得到了优质的LSMO(100)取向外延薄膜;
3)采用溶胶凝胶法和固相烧结法制备PNNZT靶材;
首先采用溶胶凝胶法制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液,溶液浓度为0.2mol/L,两种方法的步骤如下:
(1)按照摩尔比1:(1/3×0.5):(2/3×0.5):0.15:0.35分别称取Pb(CH3COO)2、Ni(CH3COO)2、C10H25NbO5、Zr(OC3H7)4和Ti(OC4H9)4制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;
将原料Pb(CH3COO)2、Ni(CH3COO)2和C10H25NbO5于120℃溶解在冰醋酸和去离子水的混合液体中,然后将Zr(OC3H7)4和Ti(OC4H9)4于室温溶解在冰醋酸和CH3COCH2COCH3的混合液体中,最后将前面两种混合液再次混合并搅拌0.5h,得到浓度为0.2mol/L的Pb(Ni1/ 3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;
(2)将步骤(1)制得的前驱体溶液在室温下继续搅拌1.5h,并放置24h,风干该溶液,得到天然干燥的凝胶;
(3)将步骤(2)得到的凝胶首先在350℃干燥20min,然后在550℃下第一次煅烧20min,最后在850℃于空气氛围中第二次煅烧1.5h,在玛瑙研钵中研磨1h,将该粉末在300Mpa冷等静压下压制成直径为20mm,厚度为3mm的粒料,然后在1150℃的空气氛围中烧结4h,之后自然冷却到室温,得到所需的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3;
4)将上述制得的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3利用激光脉冲沉积法在La0.7Sr0.3MnO3(100)取向的薄膜底电极上制备出多相共存的弛豫铁电外延薄膜,所述激光脉冲沉积法除了靶材、衬底与步骤2)不同,其它步骤及参数与步骤2)一致,所述薄膜的厚度为300nm~400nm。本发明提供了一种铁电性能优异的弛豫外延薄膜制备方法。
实施例2
1)将同为钙钛矿结构的SrTiO3(111)单晶基片作为衬底,采用激光脉冲沉积法制备钙钛矿结构氧化物La0.7Sr0.3MnO3(111)取向的薄膜底电极;
首先按照摩尔比0.7:0.3:1分别称取分析纯的La2O3、SrCO3、MnO2作为原料,利用固相烧结的方法制备La0.7Sr0.3MnO3。具体的步骤如下:
(1)在烧结之前,首先按照固定的摩尔比来配比这三种粉末,将粉末放在烘箱中烘干,烘干后将其倒入球磨罐中混合,然后在球磨罐中倒入适量的去离子水,球磨5小时。
(2)将步骤(1)中球磨完成后的液体倒入表面皿,放入烘箱,烘箱温度为110℃,烘干后将粉末倒入玛瑙研钵中,研磨30分钟以上,接着将研磨充分的粉末装入坩埚中,放置于高温炉内,进行预烧,预烧温度为1250℃,时间为11小时;
(3)将步骤(2)中预烧完成后的粉末冷却,之后再倒入球磨罐中,球磨5小时,然后将粉末烘干,在粉末中加入粘合剂PVA研磨40分钟,将研磨充分的粉末放置于20MPa压力下冷压成圆形块体;
(4)将步骤(3)中的块体放入高温炉中,以1360℃烧结30个小时,得到所需的靶材La0.7Sr0.3MnO3。
2)将上述制得的靶材La0.7Sr0.3MnO3利用激光脉冲沉积法制备出延薄膜,所述薄膜的厚度为150nm。具体的步骤如下:
(1)我们选择了与LSMO同为钙钛矿结构的SrTiO3(111)单晶基片作为衬底。在沉积之前,将基片分别放入去离子水,乙醇以及丙酮中用超声波清洗15分钟,重复4次;
(2)薄膜的沉积工作。沉积过程中,采用的沉积温度为720℃,脉冲激光能量为5Hz,单脉冲能量为350mJ,在40Pa的氧气氛下沉积25分钟,沉积完成后原位退火40分钟。之后就得到了优质的LSMO(111)取向外延薄膜。
3)采用溶胶凝胶法和固相烧结法制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3靶材;
首先采用溶胶凝胶法制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液,溶液浓度为0.2mol/L,两种方法的步骤如下:
(1)按照摩尔比1:(1/3×0.5):(2/3×0.5):0.15:0.35分别称取Pb(CH3COO)2、Ni(CH3COO)2、C10H25NbO5、Zr(OC3H7)4和Ti(OC4H9)4制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;
将原料Pb(CH3COO)2、Ni(CH3COO)2和C10H25NbO5于120℃溶解在冰醋酸和去离子水的混合液体中,然后将Zr(OC3H7)4和Ti(OC4H9)4于室温溶解在冰醋酸和CH3COCH2COCH3的混合液体中,最后将前面两种混合液再次混合并搅拌0.6h,得到浓度为0.2mol/L的Pb(Ni1/ 3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;
(2)将步骤(1)制得的前驱体溶液在室温下继续搅拌1.6h,并放置26h,风干该溶液,得到天然干燥的凝胶;
(3)将步骤(2)得到的凝胶首先在380℃干燥25min,然后在580℃下第一次煅烧25min,最后在860℃于空气氛围中第二次煅烧1.6h,在玛瑙研钵中研磨1.5h,将该粉末在300Mpa冷等静压下压制成直径为20mm,厚度为3mm的粒料,然后在1160℃的空气氛围中烧结5h,之后自然冷却到室温,得到所需的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3;
4)将上述制得的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3利用激光脉冲沉积法在La0.7Sr0.3MnO3(111)取向的薄膜底电极上制备出多相共存的弛豫铁电外延薄膜,所述激光脉冲沉积法除了靶材、衬底与步骤2)不同,其它步骤及参数与步骤2)一致,所述薄膜的厚度为300nm~400nm。本发明提供了一种铁电性能优异的弛豫外延薄膜制备方法。
实施例3
1)将同为钙钛矿结构的SrTiO3(100)单晶基片作为衬底,采用激光脉冲沉积法制备钙钛矿结构氧化物La0.7Sr0.3MnO3(100)取向的薄膜底电极;
首先按照摩尔比0.7:0.3:1分别称取分析纯的La2O3、SrCO3、MnO2作为为原料,利用固相烧结的方法制备La0.7Sr0.3MnO3。具体的步骤如下:
(1)在烧结之前,首先按照固定的摩尔比来配比这三种粉末,将粉末放在烘箱中烘干,烘干后将其倒入球磨罐中混合,然后在球磨罐中倒入适量的去离子水,球磨6小时。
(2)将步骤(1)中球磨完成后的液体倒入表面皿,放入烘箱,烘箱温度为120℃,烘干后将粉末倒入玛瑙研钵中,研磨30分钟以上,接着将研磨充分的粉末装入坩埚中,放置于高温炉内,进行预烧,预烧温度为1300℃,时间为12小时;
(3)将步骤(2)中预烧完成后的粉末冷却,之后再倒入球磨罐中,球磨6小时,然后将粉末烘干,在粉末中加入粘合剂PVA研磨60分钟,将研磨充分的粉末放置于20MPa压力下冷压成圆形块体;
(4)将步骤(3)中的块体放入高温炉中,以1400℃烧结48个小时,得到所需的靶材La0.7Sr0.3MnO3。
2)将上述制得的靶材La0.7Sr0.3MnO3利用激光脉冲沉积法制备出(100)取向的延薄膜,所述薄膜的厚度为200nm。具体的步骤如下:
(1)我们选择了与LSMO同为钙钛矿结构的SrTiO3(100)单晶基片作为衬底。在沉积之前,将基片分别放入去离子水,乙醇以及丙酮中用超声波清洗20分钟,重复5次;
(2)薄膜的沉积工作。沉积过程中,采用的沉积温度为750℃,脉冲激光能量为5Hz,单脉冲能量为350mJ,在40Pa的氧气氛下沉积30分钟,沉积完成后原位退火45分钟。之后就得到了优质的LSMO(100)取向外延薄膜。
3)采用溶胶凝胶法和固相烧结法制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3靶材;
首先采用溶胶凝胶法制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液,溶液浓度为0.3mol/L,两种方法的步骤如下:
(1)按照摩尔比1:(1/3×0.5):(2/3×0.5):0.15:0.35分别称取Pb(CH3COO)2、Ni(CH3COO)2、C10H25NbO5、Zr(OC3H7)4和Ti(OC4H9)4制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;将原料Pb(CH3COO)2、Ni(CH3COO)2和C10H25NbO5于120℃溶解在冰醋酸和去离子水的混合液体中,然后将Zr(OC3H7)4和Ti(OC4H9)4于室温溶解在冰醋酸和CH3COCH2COCH3的混合液体中,最后将前面两种混合液再次混合并搅拌1h,得到浓度为0.3mol/L的Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;
(2)将步骤(1)制得的前驱体溶液在室温下继续搅拌2h,并放置30h,风干该溶液,得到天然干燥的凝胶;
(3)将步骤(2)得到的凝胶首先在400℃干燥30min,然后在600℃下第一次煅烧30min,最后在900℃于空气氛围中第二次煅烧2h,在玛瑙研钵中研磨2h,将该粉末在300Mpa冷等静压下压制成直径为20mm,厚度为3mm的粒料,然后在1200℃的空气氛围中烧结6h,之后自然冷却到室温,得到所需的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3;
4)将上述制得的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3利用激光脉冲沉积法在La0.7Sr0.3MnO3(100)取向的薄膜底电极上制备出多相共存的弛豫铁电外延薄膜,所述激光脉冲沉积法除了靶材、衬底与步骤2)不同,其它步骤及参数与步骤2)一致,所述薄膜的厚度为300nm~400nm。本发明提供了一种铁电性能优异的弛豫外延薄膜制备方法。
实施例4
1)将同为钙钛矿结构的SrTiO3(100)单晶基片作为衬底,采用激光脉冲沉积法制备钙钛矿结构氧化物La0.7Sr0.3MnO3(100)取向的薄膜底电极;
首先按照摩尔比0.7:0.3:1分别称取分析纯的La2O3、SrCO3、MnO2作为为原料,利用固相烧结的方法制备La0.7Sr0.3MnO3。具体的步骤如下:
(1)在烧结之前,首先按照固定的摩尔比来配比这三种粉末,将粉末放在烘箱中烘干,烘干后将其倒入球磨罐中混合,然后在球磨罐中倒入适量的去离子水,球磨6小时。
(2)将步骤(1)中球磨完成后的液体倒入表面皿,放入烘箱,烘箱温度为120℃,烘干后将粉末倒入玛瑙研钵中,研磨30分钟以上,接着将研磨充分的粉末装入坩埚中,放置于高温炉内,进行预烧,预烧温度为1300℃,时间为12小时;
(3)将步骤(2)中预烧完成后的粉末冷却,之后再倒入球磨罐中,球磨6小时,然后将粉末烘干,在粉末中加入粘合剂PVA研磨60分钟,将研磨充分的粉末放置于20MPa压力下冷压成圆形块体;
(4)将步骤(3)中的块体放入高温炉中,以1400℃烧结48个小时,得到所需的靶材La0.7Sr0.3MnO3。
2)将上述制得的靶材La0.7Sr0.3MnO3利用激光脉冲沉积法制备出La0.7Sr0.3MnO3(100)取向的延薄膜,所述薄膜的厚度为200nm。具体的步骤如下:
(1)我们选择了与LSMO同为钙钛矿结构的SrTiO3(100)单晶基片作为衬底。在沉积之前,将基片分别放入去离子水,乙醇以及丙酮中用超声波清洗20分钟,重复5次;
(2)薄膜的沉积工作。沉积过程中,采用的沉积温度为750℃,脉冲激光能量为5Hz,单脉冲能量为350mJ,在40Pa的氧气氛下沉积30分钟,沉积完成后原位退火45分钟。之后就得到了优质的LSMO(100)取向外延薄膜。
3)采用溶胶凝胶法和固相烧结法制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3靶材;
首先采用溶胶凝胶法制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液,溶液浓度为0.25mol/L,两种方法的步骤如下:
(1)按照摩尔比1:(1/3×0.5):(2/3×0.5):0.15:0.35分别称取Pb(CH3COO)2、Ni(CH3COO)2、C10H25NbO5、Zr(OC3H7)4和Ti(OC4H9)4制备Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;
将原料Pb(CH3COO)2、Ni(CH3COO)2和C10H25NbO5于120℃溶解在冰醋酸和去离子水的混合液体中,然后将Zr(OC3H7)4和Ti(OC4H9)4于室温溶解在冰醋酸和CH3COCH2COCH3的混合液体中,最后将前面两种混合液再次混合并搅拌0.6h,得到浓度为0.25mol/L的Pb(Ni1/ 3Nb2/3)0.5Zr0.15Ti0.35O3前驱体溶液;
(2)将步骤(1)制得的前驱体溶液在室温下继续搅拌1.6h,并放置26h,风干该溶液,得到天然干燥的凝胶;
(3)将步骤(2)得到的凝胶首先在380℃干燥25min,然后在580℃下第一次煅烧25min,最后在860℃于空气氛围中第二次煅烧1.6h,在玛瑙研钵中研磨1.5h,将该粉末在300Mpa冷等静压下压制成直径为20mm,厚度为3mm的粒料,然后在1160℃的空气氛围中烧结5h,之后自然冷却到室温,得到所需的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3;
4)将上述制得的靶材Pb(Ni1/3Nb2/3)0.5Zr0.15Ti0.35O3利用激光脉冲沉积法在La0.7Sr0.3MnO3(100)取向的薄膜底电极上制备出多相共存的弛豫铁电外延薄膜,所述激光脉冲沉积法除了靶材、衬底与步骤2)不同,其它步骤及参数与步骤2)一致,所述薄膜的厚度为300nm~400nm。本发明提供了一种铁电性能优异的弛豫外延薄膜制备方法。
Claims (10)
1.一种PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,所述方法包括以下步骤:
1)以SrTiO3(100/111)单晶基片作为衬底,以La0.7Sr0.3MnO3为靶材,采用激光脉冲沉积法制备钙钛矿结构氧化物La0.7Sr0.3MnO3(100/111)取向的薄膜底电极;
2)采用溶胶凝胶法和固相烧结法制备PNNZT靶材,将PNNZT前驱体溶液于室温下搅拌1.5-2h,并放置24-30h,自然风干,制得凝胶;
3)将步骤2)所得凝胶干燥、煅烧、研磨、压制制得粒料,所得粒料经过烧结,自然冷却即得所需的PNNZT靶材;
4)将步骤3)制得的PNNZT靶材利用激光脉冲沉积法在La0.7Sr0.3MnO3(100/111)取向的薄膜底电极上外延制备出多相共存的弛豫铁电外延薄膜。
2.根据权利要求1所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤1)所述La0.7Sr0.3MnO3靶材可通过固相烧结方法制得,所述方法包括如下步骤:将原料La2O3、SrCO3、MnO2球磨所得的混合物烘干、预烧、冷压制备块体、烧结制得所需的靶材La0.7Sr0.3MnO3。
3.根据权利要求2所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤1)所述预烧温度为1200℃~1300℃,预烧时间为10~12小时;所述烧结温度为1350~1400℃,烧结时间为24~48小时。
4.根据权利要求1所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤1)所述激光脉冲沉积法采用的沉积温度为700℃~750℃,脉冲激光能量为5Hz,单脉冲能量为350mJ,氧气氛下沉积20~30分钟,沉积完成后原位退火35~45分钟。
5.根据权利要求1所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,所述PNNZT通式为Pb(Ni1/3Nb2/3)xZryTi1-x-yO3,其中x,y=0~1。
6.根据权利要求5所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤2)所述PNNZT前驱体溶液浓度为0.2~0.3mol/L。
7.根据权利要求1-6任一所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤3)所述凝胶干燥温度为350-400℃,干燥时间为20-30min。
8.根据权利要求1-6任一所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤3)所述煅烧包括第一次煅烧和第二次煅烧,所述第一次煅烧温度为550-600℃,煅烧时间为20-30min,第二次煅烧温度为850-900℃,煅烧时间为1.5-2h。
9.根据权利要求1-6任一所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤3)所述研磨时间为1-2h;步骤3)所述压制工艺为300Mpa冷等静压压制,压制所得粒料直径为20mm,厚度为3mm。
10.根据权利要求1-6任一所述的PNNZT基多相共存弛豫铁电外延薄膜的制备方法,其特征在于,步骤3)所述烧结温度为1150-1200℃,烧结时间为4-6h,烧结环境为空气氛围。
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