混合配体配合物胍基脒基镧的合成及性能

Synthesis and Properties of Ligand Complex Guanidine Lanthanum

La_(2)O_(3)薄膜材料应用广泛,而制备La_(2)O_(3)薄膜的前驱体合成面临着挑战,多数现有前驱体热稳定性差、合成路线复杂或者成本高等问题。因此,本文报道了混配型和均配型的胍基、脒基镧配合物二(N,N′-二异丙基-甲胺基胍基)一(N,N′-二异丙基戊基脒基)合镧(配合物1)和三(N,N′-二异丙基-甲胺基胍基)合镧(配合物2),通过1H NMR,13C NMR表征结构;通过热重分析(TGA)研究所有配合物的热稳定性和挥发性。结果表明:配合物1在加热至170.0℃时,其蒸气压会急剧上升;在202.0℃能产生1.0 Torr的蒸气压;在260.0℃以下该配合物有良好的热稳定性。以上数据说明:该配合物比较好地满足CVD工艺条件,是一种潜在的化学气相沉积前驱体;通过CVD技术,在源加热温度210℃、沉积温度为260.0℃、沉积时间为10.0 min的条件下得到约11.9 nm薄膜,SEM和XPS分析了薄膜的形貌和成分,实验结果表明沉积的纳米薄膜为高纯的La_(2)O_(3)薄膜。

La_(2)O_(3)thin films are widely used,but the synthesis of precursors to prepare La_(2)O_(3)thin films faces challenges.Most of the existing precursors have poor thermal stability,complex synthesis route or high cost.Therefore,the structure of guanidine and amidinolanthanum complexes(N,N′-diisopropyl-methylaminoguanidine)(N,N′-diisopropyl-aminoguanidine)(lanthanum)(complex 1)and(N,N′-diisopropyl-methylaminoguanidine)(complex 2)was characterized by 1 H NMR and^(13)C NMR.The thermal stability and volatility of all complexes were investigated by thermogravimetric analysis(TGA).The results show that the vapor pressure of complex 1 increases sharply when it is heated to 170.0℃.The vapor pressure of 1 Torr can be produced at 202.0℃.The complex has good thermal stability below 260.0℃.The above data indicate that the complex satisfies the CVD process conditions well,and is a potential precursor of chemical vapor deposition.By CVD technique,about 11.9 nm thin films were prepared under the conditions of source heating temperature of 210.0℃,deposition temperature of 260.0℃and deposition time of 10.0 min.The morphology and composition of the thin films were analyzed by SEM and XPS.The experimental results show that the deposited thin films are high purity La_(2)O_(3)films.