PLD法制备Ni_（1-x）Co_xO_（4/3）透明导电氧化物薄膜的研究
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摘要
透明导电氧化物(TCO)薄膜因为其良好的光电性能,广泛应用于平面显示器、太阳能电池、节能视窗、透明电磁屏蔽等领域。但由于光电性能良好的p型TCO薄膜的缺乏导致透明电子器件难以制备,因此TCO薄膜的p型掺杂成为了目前半导体材料领域的研究热点之一,制备出具有良好的光电性能的p型TCO薄膜成为了国际上的热门研究课题。
NiO和Co3O4都是p型导电材料,据报道将它们按照不同的比例组合制备而成的Ni1-xCoxO4/3氧化物薄膜也是一种p型导电薄膜,并且具有良好的光电性能。本文采用传统的陶瓷烧结工艺制备了不同比例的镍钴氧化物靶材,为薄膜的制备提供条件。利用脉冲激光沉积(PLD)系统在CVDZnS衬底上制备了一系列Ni1-xCoxO4/3薄膜,采用AFM、SEM、XPS、轮廓仪等表征手段对薄膜进行了成分分析和结构分析,并对薄膜的电学性能和光学性能进行了测试分析。
采用PLD法制备的Ni1-xCoxO4/3薄膜表面非常平整,薄膜粗糙度较小,薄膜与衬底结合较好,薄膜的厚度约50nm。XPS分析结果显示,薄膜中Ni元素和Co元素的比例和靶材中的比例吻合较好,但O原子所占比例较小,和预想化学计量比相差较大。薄膜中Ni和Co都同时存在二价和三价,薄膜主要以尖晶石结构存在。电学性能结果分析显示,采用PLD法制备的Ni1-xCoxO4/3薄膜具有优良的电学性能,其电阻率较低,最低的电阻率达到了1.22×10-4?·cm。但薄膜的光学性能较差,在可见光波段和红外波段透过率都较低。在保持薄膜具有高的电导率的同时,通过改变工艺参数,制备出高透过率的薄膜需要进一步的研究。
Transparent conductive oxide (TCO) films have been widely used in graphic LCD,solar battery electrodes,and other energy-saving window due to their outstanding photoelectric properties.However,the lack of p-type TCO films with good photoelectric properties lead to difficult to prepare transparent electronic devices.Therefor p-type TCO films have been the focus in the field of semiconductor materials,and preparing p-type TCO films with good photoelectric properties have been the hot research topic in the international world.
Both NiO and Co3O4 are p-type conductive materials,it is reported that the Ni1-xCoxO4/3 films prepared by them with different ratio are also p-type conductive films, and have good optical performance.In this paper, nickel cobalt oxide targets are prepared by using traditional ceramic sintering process,which can be used in the following experiment.Ni1-xCoxO4/3 films are prepared on CVDZnS substrate by using pulse laser deposition(PLD)method. AFM,SEM,XPS and profilometer are used to characterize the films,what’s more, both their electrical properties and their optical properties are studied.
It is found that the surfaces of Ni1-xCoxO4/3 films prepared by PLD method are very flat,and the films combine well with substrate,the thickness of films is 50nm or so.The XPS analysis results indicate that the ratio of element Ni and Co in the films match well with that in the target,however the proportion of O atoms is small,which is much different from the expected stoichiometric.Element Ni and Co in the films are bivalent and trivalency,and the structure of films is mainly spinel.The Ni1-xCoxO4/3 films prepared by PLD method have excellent electrical properties,their resistivitity value are very small,the smallest resistivitity value is 1.22×10-4?·cm.However,the optical properties of films are bad,the transmittance of films are very small both in the visible light range and in the infrared light range.The films with better optical properties can be prepared by changing the process parameters.In a word,it need further research to prepare films with both excellent electrical properties and outstanding optical properties.
NiO和Co3O4都是p型导电材料,据报道将它们按照不同的比例组合制备而成的Ni1-xCoxO4/3氧化物薄膜也是一种p型导电薄膜,并且具有良好的光电性能。本文采用传统的陶瓷烧结工艺制备了不同比例的镍钴氧化物靶材,为薄膜的制备提供条件。利用脉冲激光沉积(PLD)系统在CVDZnS衬底上制备了一系列Ni1-xCoxO4/3薄膜,采用AFM、SEM、XPS、轮廓仪等表征手段对薄膜进行了成分分析和结构分析,并对薄膜的电学性能和光学性能进行了测试分析。
采用PLD法制备的Ni1-xCoxO4/3薄膜表面非常平整,薄膜粗糙度较小,薄膜与衬底结合较好,薄膜的厚度约50nm。XPS分析结果显示,薄膜中Ni元素和Co元素的比例和靶材中的比例吻合较好,但O原子所占比例较小,和预想化学计量比相差较大。薄膜中Ni和Co都同时存在二价和三价,薄膜主要以尖晶石结构存在。电学性能结果分析显示,采用PLD法制备的Ni1-xCoxO4/3薄膜具有优良的电学性能,其电阻率较低,最低的电阻率达到了1.22×10-4?·cm。但薄膜的光学性能较差,在可见光波段和红外波段透过率都较低。在保持薄膜具有高的电导率的同时,通过改变工艺参数,制备出高透过率的薄膜需要进一步的研究。
Transparent conductive oxide (TCO) films have been widely used in graphic LCD,solar battery electrodes,and other energy-saving window due to their outstanding photoelectric properties.However,the lack of p-type TCO films with good photoelectric properties lead to difficult to prepare transparent electronic devices.Therefor p-type TCO films have been the focus in the field of semiconductor materials,and preparing p-type TCO films with good photoelectric properties have been the hot research topic in the international world.
Both NiO and Co3O4 are p-type conductive materials,it is reported that the Ni1-xCoxO4/3 films prepared by them with different ratio are also p-type conductive films, and have good optical performance.In this paper, nickel cobalt oxide targets are prepared by using traditional ceramic sintering process,which can be used in the following experiment.Ni1-xCoxO4/3 films are prepared on CVDZnS substrate by using pulse laser deposition(PLD)method. AFM,SEM,XPS and profilometer are used to characterize the films,what’s more, both their electrical properties and their optical properties are studied.
It is found that the surfaces of Ni1-xCoxO4/3 films prepared by PLD method are very flat,and the films combine well with substrate,the thickness of films is 50nm or so.The XPS analysis results indicate that the ratio of element Ni and Co in the films match well with that in the target,however the proportion of O atoms is small,which is much different from the expected stoichiometric.Element Ni and Co in the films are bivalent and trivalency,and the structure of films is mainly spinel.The Ni1-xCoxO4/3 films prepared by PLD method have excellent electrical properties,their resistivitity value are very small,the smallest resistivitity value is 1.22×10-4?·cm.However,the optical properties of films are bad,the transmittance of films are very small both in the visible light range and in the infrared light range.The films with better optical properties can be prepared by changing the process parameters.In a word,it need further research to prepare films with both excellent electrical properties and outstanding optical properties.
引文
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2徐慢,夏冬林和赵修建,透明导电氧化物薄膜材料及其制备技术研究进展.材料导报,2006. 20:312~322;
3 ZC.Jin, I.Hamberg, and CG.Granqvist, Optical Properties of Sputter-deposited ZnO:Al Thin Film. Journal of Applied physics, 1988. 64:5117~5131;
4吴广明,吴永刚,倪星元等,一种性能可调的新型节能材料—电致变色膜。材料科学与工程,1996. 14(3):11~17;
5 T.Schuler and M.A.Aegerter, Optical,Electrical and Structural Properties of Sol-Gel ZnO:Al Coatings. Thin Solid Films, 1999. 351:125~131;
6陈新亮,薛俊明,赵颖等, ZnO-TCO薄膜及其在太阳电池中的应用。材料导报,2006. 20(5):22~25;
7姜燮昌和胡勇,ITO膜透明导电玻璃的应用前景及工业化生产。真空, 1995. 6:1~8;
8 H.Kawazoe, M.Yasukawa, H.Hvoda, et al., P-type Electrical Conduction in Transparent Thin Films of CuAlO2. Nature, 1997. 389:939~942;
9 H.Yanagi, S.Inoue, K.Ueda, et al., Electronic Structure and Optoelectronic Properties of Transparent p-type Conducting CuAlO2. Journal of Applied physics, 2000. 88(7):4159~4163;
10 K.Ueda, T.Hase, H.Yanagi, et al., Epitaxial Growth of Transparent p-type Conducting CuGaO2 Thin Films on Sapphire (001) Substrates by Pulsed Laser Deposition. Journal of Applied physics, 2001. 89(3):1790~1793;
11孟扬,沈杰,和蒋益明,透明导电氧化物薄膜的新进展.光电子技术, 2002. 22(3):125~130,144;
12 Kudo, H.Yanagi, K.Ueda, et al., Fabrication of Transparent p-n Heterojunction Thin Film Diodes Based Entirely on Oxide Semiconductors. Applied Physics Letters, 1999. 75(18):2851~2853;
13 H.Ohta, K.I.Kawamura, M.Orita, et al., Current Injection Emission From a Transparent p-n Junction Composed of p-SrCu2O2/n-ZnO. Applied Physics Letters, 2000. 77(4): 475~477;
14 H.Hosono, H.Ohta, K.Hayashi, et al., Near-UV Emitting Diodes Based on Transparent p-n Junction Composed of Heteroepitaxially Grown p-SrCu2O2 and n-ZnO. Crystal Growth & Design, 2002. 237:496~502;
15 K.Nomura, H.Ohta, K.Ueda, et al., All Oxide Transparent MISFET Using High-kDielectrics Gates. Microelectronic Engineering, 2004. 72:294~298;
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