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 PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910002282 La2CuO4 Inorganic materials 0.000 title abstract 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010949 copper Substances 0.000 claims description 15
- 150000002500 ions Chemical class 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 150000002978 peroxides Chemical class 0.000 claims description 6
- JRLTTZUODKEYDH-UHFFFAOYSA-N 8-methylquinoline Chemical group C1=CN=C2C(C)=CC=CC2=C1 JRLTTZUODKEYDH-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 2
- 239000012535 impurity Substances 0.000 abstract 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000002738 chelating agent Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 abstract 1
- 239000012153 distilled water Substances 0.000 abstract 1
- 238000005242 forging Methods 0.000 abstract 1
- 230000001678 irradiating effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 23
- 239000000463 material Substances 0.000 description 4
- 239000002887 superconductor Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical class CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000010442 halite Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005088 metallography Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
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。
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| 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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| 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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