CN102392304A - 一种铜酸镧(La2CuO4)薄膜的制备方法 - Google Patents

一种铜酸镧(La2CuO4)薄膜的制备方法 Download PDF

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CN102392304A
CN102392304A CN2011103749282A CN201110374928A CN102392304A CN 102392304 A CN102392304 A CN 102392304A CN 2011103749282 A CN2011103749282 A CN 2011103749282A CN 201110374928 A CN201110374928 A CN 201110374928A CN 102392304 A CN102392304 A CN 102392304A
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黄剑锋
李意峰
侯艳超
曹丽云
吴建鹏
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Shandong Gexin Precision Co ltd
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Abstract

一种铜酸镧(La2CuO4)薄膜的制备方法,将硝酸镧加入蒸馏水中得溶液A;向A溶液中加入硝酸铜搅拌均匀后再加入草酸和乙酰丙酮得溶液B;将经双氧水和硝酸活化处理后的硅基片浸入溶液B中;将B溶液放在紫外光-微波仪中照射后取出硅基片,将硅基片用丙酮清洗后放入干燥箱中干燥得单一物相的La2CuO4薄膜。本发明采用紫外光-微波相结合的方法制备La2CuO4薄膜,反应过程易于控制,并且设备要求低,操作简单,不需要煅烧处理,大大降低了能耗,可得到高质量的La2CuO4薄膜。另外由于本发明利用草酸为螯合剂在较低温度下制备不含杂质的La2CuO4薄膜。制得的La2CuO4薄膜晶粒尺寸较小,薄膜表面平整,并且不含杂质。反应周期短,重复性好,制备简单,操作方便,原料易得,制备成本较低。

Description

一种铜酸镧(La2CuO4)薄膜的制备方法
技术领域
本发明涉及一种La2CuO4薄膜的制备方法,具体涉及一种紫外光-微波相结合制备La2CuO4薄膜的方法。
背景技术
随着高温超导研究的快速发展,尤其是液氮温度以上的超导体的发现,为超导体的广泛应用打开了方便之门,这也促使氧化物超导体薄膜物理和技术的飞速发展。就基础研究而言,在薄膜材料中,由于薄膜和基片之间晶格失配而在薄膜中产生应力(应变),而使薄膜材料的性质有别于体材料的性质。充分理解这些性能的物理含义对于揭示超导机理是十分必要的,在这一方面,由于La2CuO4体系结构和化学成份简单,可掺杂范围广,La2CuO4体系将是研究超导机理理想的材料。
同时,La2CuO4是类钙钛矿型(A2BO4)复合氧化物,它比ABO3型氧化物多了一个AO岩盐层。它的存在使层中的BO6八面体发生畸变,从而在较大的弹性范围内使结构稳定。由于其本身是一种非整比化合物,结构中可能存在着A位离子缺位和氧空位,使其具有气敏性,可以作为气体传感器,因而受到广泛的重视。
目前,关于制备La2CuO4薄膜的报道较少,汪春昌[WangChunchang.Oxygen Intercalation and Related Properties of La2CuO4Bulk Samples[D].北京:清华大学,2004.]采用脉冲激光沉积法(PLD),以LaAlO3为衬底,制备出La2CuO4薄膜,但这种方法设备要求高,工艺复杂,很难制备高质量的外延薄膜。
发明内容
本发明的目的在于克服上述现有技术的缺点,提供了一种不仅制备成本低,而且操作简单、反应周期短的单一物相的铜酸镧(La2CuO4)薄膜的制备方法。
为达到上述目的,本发明采用的技术方案是:
1)将分析纯的硝酸镧(La(NO3)3·nH2O)加入60ml~100ml蒸馏水中磁力搅拌配制成La3+浓度为0.3mol/L~0.6mol/L的透明溶液A;
2)向A溶液中加入分析纯的硝酸铜(Cu(NO3)3·3H2O),使得La3+与Cu2+的摩尔比为2∶1,并不断搅拌,然后向溶液中加入草酸,使草酸与阳离子总和的摩尔比为(0.5~3)∶1,最后加入1~8滴乙酰丙酮,搅拌均匀后静置5h~20h得溶液B;
3)将经双氧水和硝酸活化处理后的硅基片浸入溶液B中;将B溶液放在紫外光-微波仪中照射5h~20h后取出硅基片,将硅基片用丙酮清洗后放入干燥箱中,在80℃~110℃下干燥得单一物相的La2CuO4薄膜。
本发明采用紫外光-微波相结合的方法制备La2CuO4薄膜,反应过程易于控制,并且设备要求低,操作简单,不需要煅烧处理,大大降低了能耗,可得到高质量的La2CuO4薄膜。另外由于本发明利用草酸为螯合剂在较低温度下制备不含杂质的La2CuO4薄膜。制得的La2CuO4薄膜晶粒尺寸较小,薄膜表面平整,并且不含杂质。反应周期短,重复性好,制备简单,操作方便,原料易得,制备成本较低。
附图说明
图1为实施例1所制备的La2CuO4薄膜的X-射线衍射(XRD)图谱。
图2为实施例1所制备的La2CuO4薄膜的金相显微(OM)照片。
具体实施方式
下面结合附图及实施例对本发明作进一步详细说明。
实施例1:
1)将分析纯的硝酸镧(La(NO3)3·nH2O)加入80ml蒸馏水中磁力搅拌配制成La3+浓度为0.5mol/L的透明溶液A;
2)向A溶液中加入分析纯的硝酸铜(Cu(NO3)3·3H2O),使得La3+与Cu2+的摩尔比为2∶1,并不断搅拌,然后向溶液中加入草酸,使草酸与阳离子总和的摩尔比为1.2∶1,最后加入2滴乙酰丙酮,搅拌均匀后静置10h得溶液B;
3)将经双氧水和硝酸活化处理后的硅基片浸入溶液B中;将B溶液放在紫外光-微波仪中照射5h后取出硅基片,将硅基片用丙酮清洗后放入干燥箱中,在80℃下干燥得单一物相的La2CuO4薄膜。
由图1可以看出所制备的薄膜为单一相的La2CuO4,由图2可以看出,薄膜较为致密平整,孔隙较少。
实施例2:
1)将分析纯的硝酸镧(La(NO3)3·nH2O)加入70ml蒸馏水中磁力搅拌配制成La3+浓度为0.4mol/L的透明溶液A;
2)向A溶液中加入分析纯的硝酸铜(Cu(NO3)3·3H2O),使得La3+与Cu2+的摩尔比为2∶1,并不断搅拌,然后向溶液中加入草酸,使草酸与阳离子总和的摩尔比为2∶1,最后加入5滴乙酰丙酮,搅拌均匀后静置20h得溶液B;
3)将经双氧水和硝酸活化处理后的硅基片浸入溶液B中;将B溶液放在紫外光-微波仪中照射20h后取出硅基片,将硅基片用丙酮清洗后放入干燥箱中,在100℃下干燥得单一物相的La2CuO4薄膜。
实施例3:
1)将分析纯的硝酸镧(La(NO3)3·nH2O)加入100ml蒸馏水中磁力搅拌配制成La3+浓度为0.6mol/L的透明溶液A;
2)向A溶液中加入分析纯的硝酸铜(Cu(NO3)3·3H2O),使得La3+与Cu2+的摩尔比为2∶1,并不断搅拌,然后向溶液中加入草酸,使草酸与阳离子总和的摩尔比为3∶1,最后加入8滴乙酰丙酮,搅拌均匀后静置15h得溶液B;
3)将经双氧水和硝酸活化处理后的硅基片浸入溶液B中;将B溶液放在紫外光-微波仪中照射10h后取出硅基片,将硅基片用丙酮清洗后放入干燥箱中,在90℃下干燥得单一物相的La2CuO4薄膜。
实施例4:
1)将分析纯的硝酸镧(La(NO3)3·nH2O)加入60ml蒸馏水中磁力搅拌配制成La3+浓度为0.3mol/L的透明溶液A;
2)向A溶液中加入分析纯的硝酸铜(Cu(NO3)3·3H2O),使得La3+与Cu2+的摩尔比为2∶1,并不断搅拌,然后向溶液中加入草酸,使草酸与阳离子总和的摩尔比为0.5∶1,最后加入1滴乙酰丙酮,搅拌均匀后静置5h得溶液B;
3)将经双氧水和硝酸活化处理后的硅基片浸入溶液B中;将B溶液放在紫外光-微波仪中照射15h后取出硅基片,将硅基片用丙酮清洗后放入干燥箱中,在110℃下干燥得单一物相的La2CuO4薄膜。

Claims (1)

1.一种铜酸镧(La2CuO4)薄膜的制备方法,其特征在于:
1)将分析纯的硝酸镧(La(NO3)3·nH2O)加入60ml~100ml蒸馏水中磁力搅拌配制成La3+浓度为0.3mol/L~0.6mol/L的透明溶液A;
2)向A溶液中加入分析纯的硝酸铜(Cu(NO3)3·3H2O),使得La3+与Cu2+的摩尔比为2∶1,并不断搅拌,然后向溶液中加入草酸,使草酸与阳离子总和的摩尔比为(0.5~3)∶1,最后加入1~8滴乙酰丙酮,搅拌均匀后静置5h~20h得溶液B;
3)将经双氧水和硝酸活化处理后的硅基片浸入溶液B中;将B溶液放在紫外光-微波仪中照射5h~20h后取出硅基片,将硅基片用丙酮清洗后放入干燥箱中,在80℃~110℃下干燥得单一物相的La2CuO4薄膜。
CN 201110374928 2011-11-23 2011-11-23 一种铜酸镧(La2CuO4)薄膜的制备方法 Expired - Fee Related CN102392304B (zh)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101186328A (zh) * 2007-12-07 2008-05-28 北京工业大学 单晶类钙钛矿型氧化物La2CuO4纳微米棒的制备方法
CN101798103A (zh) * 2010-01-29 2010-08-11 北京工业大学 一种制备三维大孔结构的正交晶相La2CuO4的胶质晶模板法
JP2011051826A (ja) * 2009-09-01 2011-03-17 Nippon Telegr & Teleph Corp <Ntt> 複合酸化物及びその製造方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101186328A (zh) * 2007-12-07 2008-05-28 北京工业大学 单晶类钙钛矿型氧化物La2CuO4纳微米棒的制备方法
JP2011051826A (ja) * 2009-09-01 2011-03-17 Nippon Telegr & Teleph Corp <Ntt> 複合酸化物及びその製造方法
CN101798103A (zh) * 2010-01-29 2010-08-11 北京工业大学 一种制备三维大孔结构的正交晶相La2CuO4的胶质晶模板法

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