以氯化鈉/氯化銅為氯離子源之化學浴沉積法製備氯化亞銅薄膜特性研究

梁菀婷

doi:10.6840/cycu201600873

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以氯化钠/氯化铜为氯离子源之化学浴沉积法制备氯化亚铜薄膜特性研究

Fabrication of cuprous chloride films by chemical bath deposition using sodium chloride / cupric chloride as the source of chloride ions

梁菀婷 , 硕士　　导师：温武义　　

英文 DOI： 10.6840/cycu201600873

氯化钠；氯化铜；氯化亚铜；化学浴沉积法；铜基板； NaCl ； CuCl2 ； CuCl ； chemical bath deposition ； copper substrate

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摘要 │ 参考文献 (56) │ 国际计量

摘要〈TOP〉

本研究是以氯化钠和氯化铜化合物共同作为氯离子的前驱物，而氯化铜亦同时为铜离子的前驱物，使用化学浴沉积法在铜基板上制备氯化亚铜薄膜。藉由改变实验参数，如：掺入浓度、沉积时间、盐酸浸渍...等，制备不同条件下沉积的氯化亚铜薄膜，通过分析它们的导电型态、光学特性、晶相结构、表面形貌、元素组成以及结构层，进行有系统地比较，寻找出最适当沉积参数及其特性研究，并且与使用单一氯化铜化合物为前驱物所制备出的氯化亚铜薄膜作比较。
首先是研究在不同浓度氯化钠的掺入下对氯化亚铜薄膜之影响，并且与未掺入时所制备出的薄膜进行比较。所制备的薄膜之发光特性、晶相结构、表面形貌以及元素组成已经过详细审查。从分析结果得知以氯化钠与氯化铜化合物为两种离子源前驱物下的良好品质之氯化亚铜薄膜已经通过化学浴沉积法实现，并且确认掺入比未掺入氯化钠所制备出的薄膜之品质更好。藉此结果可证实以氯化钠化合物增加氯离子源的理论是成功，有达成改善氯化亚铜薄膜中氯原子相对比率之状况。
然後是研究改变薄膜沉积时间与盐酸浸渍次数对氯化亚铜薄膜之影响。所制备的薄膜之发光特性、晶相结构、表面形貌、元素组成以及结构层已经过详细审查。从分析结果发现未改变样品所制备出的是平坦连续的氯化亚铜覆盖层，薄膜厚度约为2微米，比未掺入氯化钠所制备出的薄膜厚约1微米，并且其薄膜层是纯的氯化亚铜结晶，与其相应的元素分布是均匀的。另外，虽然延长薄膜沉积时间与增加盐酸浸渍次数所制备出的是不连续的氯化亚铜覆盖层（60min-3dipping、80min-4dipping），但是其品质并不输於未掺入氯化钠所制备出的薄膜，所以如此改变所制备出的氯化亚铜薄膜可以依照往後所要制成的元件之需求调整其结构层。藉此结果可证实增厚薄膜以减少Cu^+离子的形成的理论是成功，亦有达成改善氯化亚铜薄膜中氯原子相对比率之状况。
另一方面为了改善薄膜之晶相品质，本研究也调查了在不同温度与时间的热退火处理下对氯化亚铜薄膜之影响。所制备的薄膜之导电型态、发光特性、晶相结构、表面形貌以及元素组成已经过详细审查。从分析结果得知回火前、後所制备出的皆是n型氯化亚铜薄膜，并且发现薄膜的发光强度、结晶性、表面氯元素含量会随着温度提升而增加（150℃-1hr、200℃-1hr），再加上其表面形貌会也随着温度与时间的提升而更趋於平整，藉由上述分析结果证实热退火处理是有助於提升氯化亚铜薄膜品质。值得一提的是於光激萤光光谱图中观察到在5.7K低温下激子和双激子的发光机制，特别是於室温下明显地观察到自由激子的发射，而此特性意谓薄膜品质佳。以上分析结果对於氯化亚铜未来用以制备二极体元件有着重大的意义。

关键字：氯化钠、氯化铜、氯化亚铜、化学浴沉积法、铜基板

*：作者
**：指导老师

并列摘要〈TOP〉

This research is taking both sodium chloride (NaCl) and copper (II) chloride (CuCl_2) compound as precursor of chloride ions, while CuCl_2 is also taken as precursor of copper ions, and using chemical bath deposition (CBD) to prepare copper (I) chloride (CuCl) films on a copper (Cu) substrate. We prepare CuCl films deposited under different conditions by changing the parameters of the experiment, such as adding concentration, deposition time, hydrochloric acid (HCl) dip, etc. By analyzing their electrical properties, optical properties, phase structure, morphology of the surface, elemental composition and structure layer, we can conduct a systematic comparison to find out the most suitable deposition parameters and researches of their characteristics. Then we compare with the CuCl films prepared by using single CuCl_2 compound as precursor.
First, we study the effect on the CuCl film grown with adding different concentrations of NaCl, and compared with the one grown with not adding NaCl. The light emission characteristics, phase structure, morphology of the surface and elemental composition of prepared films have detailed investigated. We can know from the analysis result that a good-quality CuCl film was achieved by CBD via taking NaCl and CuCl_2 compound as precursor of two kinds of ions source. And we confirmed the quality of the film grown with adding NaCl is better than the one without adding NaCl. We can prove the theory that using NaCl compound to increase chloride ions is successful by this result and we have achieved that improving relative ratio of chloride atoms in CuCl film.
Next, we study the effect on the CuCl film grown with changing the deposition time of the film and HCl dip times. The light emission characteristics, phase structure, morphology of the surface, elemental composition and structure layer of prepared films have detailed investigated. We found the prepared CuCl-covered layer of simples without changing is flat and continuous from the analysis result. The thickness of the film is about 2 microns and about 1 micron thicker than the one without adding NaCl. Its film layer is pure CuCl crystallites and corresponding elemental distribution is uniform. In addition, although the film grown with extending deposition time of the film and increasing HCl dip times is discontinuous CuCl-covered layer (60min-3dipping and 80min-4dipping), its quality is not worse than the one without adding. So the CuCl film prepared by this changing can adjust its structure layer depending on the demand of devices need to fabricate afterwards. We can prove the theory that increasing the thickness of the film to decrease the formation of Cu^+ is successful by this result and also have achieved that improving relative ratio of chloride atoms in CuCl film.
On the other hand, in order to improve the quality of phases of the film, this research also investigated the effect on the CuCl film under different temperature and time of the thermal annealing treatment. The light emission characteristics, phase structure, morphology of the surface, elemental composition and structure layer of prepared films have detailed investigated. We can know from the analysis result that the CuCl films prepared before- and after-annealing are all n-type and find the intensity of light emission, crystalline and contents of chloride on the surface of the film will increase with the temperature increasing (150℃-1hr and 200℃-1hr). And plus, its morphology of the surface also tends to be more flat with temperature and time increasing. We can prove the thermal annealing treatment is helpful to enhance the quality of CuCl film by the analysis results described above. Noticeably, we observed light emission mechanism of exciton and bi-exciton in low temperature photoluminescence (PL) spectra at 5.7K, especially, clearly observed the free exciton related emission at room temperature and this property means the quality of the film is good. The analysis results above have great significance for CuCl used in the fabrication of the diode elements in the future.

Keywords: Sodium chloride (NaCl), copper (II) chloride (CuCl_2), copper (I) chloride (CuCl), chemical bath deposition (CBD), copper (Cu) substrate.

*: The author
**: The advisors

参考文献 ( 56 ) 〈TOP〉

[3] S. C. Hung, K. J. Wang, S. M. Lan, T. N. Yang, W. Y. Uen, and G. C. Chi, Phys. Status Solidi A 209 (2012) 1053-1058.
连结：
[4] Y. C. Huang, L. W. Weng, W. Y. Uen, S. M. Lan, Z. Y. Li, S.-M. Liao, T. Y. Lin, and T. N. Yang, J. Alloys Compd. 509 (2011) 1980-1983.
连结：
[8] Y. C. Huang, Z. Y. Li, H. H. Chen, W. Y. Uen, S. M. Lan, S. M. Liao, Y. H. Huang, C. T. Ku, M. C. Chen, T. N. Yang, and C. C. Chiang, Thin Solid Films 517 (2009) 5537-5542.
连结：
[11] Z. Y. Li, C. Y. Lee, D. W. Lin, B. C. Lin, K. C. Shen, C. H. Chiu, P. M. Tu, H. C. Kuo, W. Y. Uen, R. H. Horng, G. C. Chi, and C. Y. Chang, IEEE Journal of Quantum Electronics 50 (2014) 354-363.
连结：
[12] C. H. Chiu, C. C. Lin, P. M. Tu, S. C. Huang, C. C. Tu, J. C. Li, Z. Y. Li, and W. Y. Uen, IEEE Journal of Quantum Electronics 48 (2012) 175-181.
连结：

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引用含有DOI的文献

DOI可强化引用精确性、增强学术圈连结，并给予使用者跨平台的良好使用经验，目前在全世界已有超过五千万个对象申请DOI。 如想对DOI的使用与概念有进一步了解，请参考 （ ） 。

DOI可强化引用精确性、增强学术圈连结，并给予使用者跨平台的良好使用经验，目前在全世界已有超过五千万个对象申请DOI。如想对DOI的使用与概念有进一步了解，请参考（）。