氮等离子体辅助脉冲激光沉积生长p型ZnO_N薄膜的光学和电学性质_英文_

氮等离子体辅助脉冲激光沉积生长p型ZnO_N薄膜的光学和电学性质_英文_ 32 10 Vo. 32 No. 10 l第 卷 第 期 发光学报 2011 10 年 月 Oct( ,2011 CHINESE JOURNAL OF LUMINESCENCE Article ID: 1000-7032 (2011) 10-0977-06 Optical andE lectrical Properties of p-typZen O? N Films Grown by N-plasma Assisted PulsLeads er Deposition * WANG Lei,XU Hai-yang,LI Xing-hua,LIU Yi-chun ( Centerf or Advanced Optoelectronic Functional Materials Research and Key Laboratoryf or UV Light-Emitting Materials and Technology of Ministry of Education,Northeast Normal University,Changchun 130024,China) Abstract: Nitrogen-doped ZnO ( ZnO? N) films were grownb y N-plasma assisted pulsed laser deposition, The p- type conductivities were cahieved by post low-temperature rapid thermal annealing ( RTA) , The N chemical states, optical and e lectrical properties of ZnO? N films were ysstematically studied by X-ray photoelectron spectroscopy ( XPS) ,photoluminescence ( PL) and Hall measurements, Threes ults revealed that theo btained p-type ZnO? N films are highly compensateds emiconductor,and the RTA process cana ctivate more N acceptors andre duce the self-com- pensation of intrinsic donor defects, ThreNe a cceptor-related emissions were observeind low-temperature PL spectra, Theio nization energy ofN acceptor wadset ermined as abou12t 8 meV from free-electron-to-acceptor ( FA) transition, Interestingly,donor-acceptor pair ( DAP) emission showed ali gsht redshift with increasing annealing temperature,T his phenomenon was undersitnoo ted rm s of pao tential fluctuation model, Key words: p-type; ZnO? N films; PLD; optical and electrical + + properties Document ocde: APACC: 7360F; 7855CLC number: O472 , 3; O472 , 4 PACS: 81, 15, Fg; 78, 55, Et DOI: 10, 3788/ fgxb20113210097, 7 Various groupI and V dopan,have t beene mployed--Introduction 1 to fabricate p-type ZnO, Among them,N is regar- ded as one of the moprsotm ising p-type dopantsf or With a wide band gap of3 ( 37 eV and a large ZnO becausei t has a imsilar ionic radius to O and excton bndng energy o6f 0 meV,ZnO becomes foa iii- 3 , the Nion substitution for O sublattice ( N ) cancus of ntense research as p a rom sng matera for iiiilO ,5,introduce a shallow acceptorl evel in ZnO, Nitro- short-wavelength optoelectronic devices that suitable gen gas( N) is an environmentally friendly N do- for high-temperature operation,such as ultraviolet 2 ping source, Although the Nwould inevitably intro- ( UV) photodetector,sUV light emitting diodes and 2 ,1-2,laser diodes, Howeve,rZnO still suffers fromth e duce thes ubstitutional N ,( N ) , donorsi nto ZnO2 2 O ,3,6,films,this negative effect can be inmimized by asymmetric doping limitation, The realization of a choosing suitable growth t echniques and c ondi- stable and high-quality p-type ZnO,which is crucial ,7-8,tions, Plasma assisted pulsed laser deposition for practical device applications,has be proved tboe ( PLD) ,as an onequilibrium technique,is an effec-very difficult due to the se lfcompensation effect, - ,3-4, tive method to growall oy or dopedf ilms, High-power low solubilityand high ionization energy of ac - ceptor mpurtes, In recent year,sthe researchon iiiradio-frequency ( RF) plasma sourcec an ionize the Nmolecule and generate N -plasma, which can ptype ZnO has proceeded at a more rapd pace, -i2 Received date: 2011-04-02; Revised date: 2011-05-22 Foundation item: Project supportedby National Natural Science Foundation of China ( 50725205,60907016) ,Science Foundation for YoungS choars of Jn Provnce,Chna ( 20080102) ,and Cutvaton Fund of NENU ( NENUSTC08001) , liliiilii-Biography: WANG Lei,born in 1982,male,Jilin Province, His work focuses oni dwe-band-gap semiconductor materials and devices, E-mail: wangl055@ nenu, edu, cn * : Corresponding Author; E-mail: hyxu@ nen,u edu, cn increase the solubility of N in ZnO over 8 orders of espectively( The chemical states of theel ements in r magnitude,as reportedi n Ref, ,8,, However,re- ZnO? N fms were dentfed by Xray photoeectron iliii-lports onPL D growth ofp -type ZnO? N film are very spectroscopy( XPS,VG ESCALAB MKsystem, -? ,9,limited, In this work,we usedN plasma assisted -UK) , The eectrca property wasex amned by Halilill PLD technique to grow Z nO ? N films,their ptype -measurement(s Lakeshore7704 system) in the van conductivities were a chieved just via post l ow-tem- der Pauw co nfiguration, Their optical properties peraturer apd therma anneang ( RTA ) , Detaed illiilwere investigated by temperature-dependent photolu- studies have been g iven on the c hemical states, minescence ( PL )measuremen ts( JobinYvon-electrical and optical properties of thep type ZnO? N - HR800 UV spectromete) r,in which the 325 nm He-films, Cd aser ne was used as thexc teaton source, lliii Experiments Results and Discussion 2 3 Table 1 lists the resistivity,net carrier concen- grown on c sapphire sub --ZnO ? N films were stratesby N-plasma assisted PLD technique( A ation and mobility of ZnO? N films( The tr Nd? resistance of the as-grown ZnO? N film was soh igh as to YAG pulsed laser ( 355 nm,5 ns,10 Hz) wase m- exceed the de tecton limit of Ha system( After illpoyed to abate a ZnO ceramc target ( 4N lli the RTA treatmen,tthe fms show weak p type il-purty) , Pror to the d eposton, the growth iiii conduction, As the annealing temperature in crease chamber was evacuated to a base pressure7, of 5 × , 5 from 200 to 10 Pa with a turbo molecular pump, And then,13 15 , to 2( 68 × 10 cm ,but the mobility3( 24 × 10 3 400 ? ,the net carrier concentration increase sfrom ultrapure OandN gases werein troduced into the 2 2 decreases ignsificantly( The low carrier chamber, The totapressure was kept 20at Pa,and concentraton l i the parta pressurera to of Nto Os 9 ? 1, The and mobty are attrbuted to the strongse fcompeniliiiliil-- 2 2 sation effect( The observation of RTA-induced Npasma,whch was generated by an RF pasma -lil p- type conversion indicated that the low-source with a power of temperature RTA process helps to activate more N 100 W,serves as the do ping source, Thes ubstrate acceptors and decrease the donor specie s adsorbed temperature was a mntaned at 500 ? , The fm iiil on the g rain boundaries and f ilm surface,which will thckness was about 120 nm, To actvate more N ii be further demonstratedby the following XPS acceptor,sthe asgrown ZnO ? N films are rapidly -Table 1 H all measurement results of as-grownan d RTA-treated ZnO? N films results, annealed at 200 and 400 ? in Natmosphere, 2 , 32 , 1 , t/ ? Resistivity / ( cm)Type ? C / cm Mobility / ( cmV s ??ΩRTA 1 ), as-grown , , High ρ 200 p 26( 8( 05 × 3( 24 × 3130 10 10 1( 4400 p 9 1( 57 × 2( 68 × 31510 10 ,12, Fg( 1 shows theN 1s andO 1s coreeve XPS i-llXPSand is an effective acceptor dopan, t Thel at-spectra of theas -grown and annealed ZnO? N films, ter is associated with N—O species, such a s , ,10, ( NO) , They may be adsorbed thon e respectvey, The bndng energys cae was cabrailiilli- 2 grain ted by using the C 1s line at 284, 6 eV, In boundary,and impose a negative effect onp type -Fg, 1 iconductivity, With the increasing annealing tempera- ( a) ,a broad band at about400 eV dominates allture,the ntegrated ntensty rato of Nto NO peak iiii—O the N 1s core-level XPS spectra,which can bed e- increase,s This confirms that the RTA treatment can convoluted into two Gaussian peaks at about399 and 3 , ,1011,-decrease the undesirable N—O species and activate more N acceptor(s As ar esut,the ptype conducl--Nion ( N ) ,which has beeni nvestigated inO O 401 eV, The formers attrbuted to thes ubsttutona iiiil our previous report by temperature-dependent tivity of ZnO ? N films is achieved( Another weak N 10 979 第 期WANG Lei,et al: Optical and Electrical Properties of ptype ZnO? N Films …- 1s peak at405 eV wasa lso observe(d The origin and suggesting a relative reduction in the a dsorbed of oxygen species,which partly contributes to ptype -ths peak can beco nsdered as the N moecue ociill- 2 converson, Smar phenomenon of RTAnduced iiil-icupying O site ,( N) ,,which is a shallow double 2 O oxygend esorption has also been observedi n the pre- ,14,donor andu sually exists in the heavily dopedZ nO ? ,3,13,vious reports, To s tudy Ndoping effects on the - Howeve,rthe XPSr esults indicate that it is,N optical properties of ZnO films,PL spectra ofR TA- difficult to remove the( N) componentv ia a low- 2 O treated ZnO? N fms were measured at 80 K,as iltemperature R TA treatmen(t The of the presence shown n Fg, 2 ( a) , The UV emsson band can iiiiaccep- N) donors p artly compensateshe ( Nt O2 O ,3,13,be we ftted by fve peaks, By comparng the lliiitors,which leading to a very low net carrier reported peak positions,we tentatively assign the concentration in the ZnO? N exhib- three mfilms( Fig( 1( b)ain peaks at about3 , 35,3, 31 and 3, 25 its the O 1s core-level XPS spectr(a Obviously,the0 eV to neutral acceptor bounde xciton ( AX) O 1s band is overlapped by two peaks iwth binding emission,freeelectrontoacceptor transition ( FA) -- --energies of 530, 5 and 532, 2 eV,which correspon- and donoracceptor par ( DAP) recombnaton,-iiiding to the O-Zn bond and theloo sely bound oxygen ,16-17,respectively, An- other two weak peaks at about adsorbed on the gran boundares and fm surface, iiil ,14,3, 17 and 3, 10 eV are attributed to the longitudinal respectvey, The atter was abeed as Ads, O, In illll optical ( LO) phononsr eplicas of DAP emission,general,they play a negative role in p-type conducti- ,15,since their energy separa- tions are close to the LO vity, After ZnO ? N films were R TA-treated in 2 phonon energy ZofnO ( 72 meV ) , The appearance N atmospher,ethe intensity ratio of the adsorbeodxy gen of these acceptorrelated emissions further confirms -peak to thela ttice O peak decreasessig nificantly the N incorporation, One can d etermine the ionization energy of N acceptor (a) N 1 s No ( E ) from the F A emissionenergy ( E ) ,usingA FA —NO,16,400 ?(N) 2O the foowng equaton: llii E= E,E + kT /2,( 1)u. A g FA B 200 ? a. / 0X A80 K (a)400? RTA FA 3.351 DAP 3.312 as-grown 3.244 DAP-1LO 3.167 DAP-2LO 3.108 u. 410 405 400 395 a. /Binding energy / eV (b)200? RTA 3.351 3.252 (b) O 1 s O—Zn 3.312 3.175 3.103 Ads. O 3.4 3.0 3.1 3.2 3.3 u. I Photon energy / eV a. /400 ? I Fig( 2 Low-temperature ( 80 K) PL spectrao f RTA- 200 ? treated ZnO? N films, ( a) 400 ? and ( b) as-grown 200 ? , TheU V emission bands are ewll fitted by 537 534 531 528 five Gaussian peaks, Binding energy / eV With intrinsic band gapE = 3, 377 eV,Ecan g A Fig( 1 ( a) N 1s and ( b) O 1s core-level XPS spectra be calculated to be about128 meV at80 K, It I ofZnO? N films( The rectangle ( ) ,circle and ?is very agreementi thw the theoretical value of 132 ( )? trange ( )expermenta data corresponds to the ilil? meV predicted by a hydrogen-like acceptor omdel as-grown,200 and 400 ? annealed ZnO ? N films,and the expermenta vaue of about 120 meV ill respectvey, The XPS spectra have beesmnoo thed n ilireported n i order to reduce the noise level, ZnO? N fms grown by moecuar beam eptaxyillli,18,, acceptor natur(e It was worth n oting that the 400 ? RTA 0AX DAP yFA tisDAP nemission slightly redshifts from 3( 252 to 3( 244 eDAP-1LO tnieV PL wth ncreasng RTAtemperature from 200 to 400 iii-80 K d110 K ze141 K li? ( Ths DAP shft suggests ha gh compensaton iiiia170 K m 201K ro231 K in the heavily doped ZnO? N films,and can be N262 K 290 K under- stood in terms of ap otential fluctuation model3.0 3.1 3.2 3.3 3.4 ,19-20,, In a heavy doped,strongy compensated illPhoto energy / eV semconductor,a hgh densty of charged donors i- iiFg( 3 Temperaturedependent PL spectra ofZ nO ? N i- and acceptors can creatse tr ong oca eectrca - lllilfilms annealed at 400 ? feds,whch nducng Couombpotenta fuctuatons iliiil-illi0 whch may bea ttrbuted to thed ssocaton of A X to iiiiiof the band edgesand impurity levels, In this E,( E+ E),2 , ( 2)= Efree exciton( Moreove,rthe FA emission gradually σ DAPg D A case,the photon energofy DAP recombination ( E) is DAP whereE ,Eand Eare the band gap ZofnO ,theshifts to the low energys ide with the temperaturien - g D A expressed :a sdonor and acceptioron ization energies,respectively, creasing, This redshift is dominated by the ordinary temperature-induced band gaps hrinkage, The represents th eaverage po tential-well depth,σ whch s proportona to the chargedm purtes con iiiliii- Conclusion 4 centration and the s creening radius( Hall and XPS studies have revealed that increasing RTA-The p-type ZnO? N films were fabricated by N- plasma assisted PLD technique combined with a tempera- ture cana ctivate more N acceptors( The lowtemperature RTA proces(s Different types of -increase in ionized acceptorc oncentration deepens N oca states,ncudng Naccepto,r( N) donor lliliO 2 O the potential and NO speces,were observed n the ZnO? N -iiwell ( ) ,thus leading to ther edshift of DAP emis- σ films, Though the weapkt ype conductivity is real-- sion, Similar observation has laso been r eported in ,19-ized,the strongs elfcompensation of ( N) and n-- 2 O heavily doped ZnS?e N and GaAs? Li films 20,atve donorsr esuts n the ow net carrer concentrailili- , To support the PL assignments, the ton and mobty, N acceptorreated emssons iili-liitemperature- dependentP L spectra of thetw o RTA- dominate the lowtemperature PL spectra of ZnO? -treated ZnO? N films were measured in the range N films, The ionization energy oNf acceptor was of 80 : 290 K, Both films exhibit similar estimated to be abou12t 8 meV from the PL - temperatureev olution, studies, The mechanisms of DAP redshift were Fig, 3 show thet emperature-dependent PL spec- discussed, It is expected thatt h e detailed tra of thef ilm annealed at 400 ? , As the tempera- nvestgatons on theph ysca propertes of ZnO ? iiiiliture increasing,the DAP emission loses its intensity N fms are h epfu for achevng reproducbe,hghillliiili-rapidly,and mergesi nto the FA emission peak,due to quality and s toble p- type ZnO films, the relatively lower donor ionization energy, This 0 featurei s typical for DAP recombination, The AX emission also shows athermal quenching behavior, References: ys, Status So, B,200724,4( 9) : 30273073,Phl-,1, Klingshirn C, ZnO: From basics towardsa pplications ,J,, ,2, Bagnall D M,ChenY F,Zhu Z,et al, Optically pumpedl asing of ZnO at room temperature,J,, Appl, Phys, Lett, , 1997,70( 17) : 2230-2232, ,3, Lee E C,Kim Y S,Jin Y G,et al, Compensation mechanism for N acceptorsi n ZnO, J,, Phys, Rev, B,20016,4( 8) : 085120-1-5, ,4, Gao Xiaoqi,Guo Zhiyou,Zhang Yufei,et al, The electronic structure ando ptical properties of Al-N codoped ZnO,J ,, 10 981 第 期WANG Lei,et al: Optical and Electrical Properties of ptype ZnO? 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N ? Cl ,J,, Phys,R ev, B,19985,7( 20) : 1286912873, - ,20,Gislason H P,YangB H,Linnarsson M, Shifting photoluminescence bands in highresistivity Licompensated GaAs, J,, -- Phys, Rev, B,19934,7( 15) : 94189424,- 氮等离子体辅助脉冲激光沉积生长 p ZnO? N 型 薄膜的光学和电学性 质 * ,,,王雷徐海阳李兴华刘益春 ( 东北师范大学 先进光电子功能材料研究中心 紫外光发射材料与技术教育部重点实验室,吉林 长春 130024) ZnO? N) 。: ( PLD) ( 摘要通过氮气等离子体辅助脉冲激光沉积技术制备了氮掺杂氧化锌薄膜经过低温快 速 ( RTA) ,ZnO? N p 。XPS) 、( PL) X ( 热退火处理后薄膜呈现 型导电特性利用 射线光电子能谱光致发光和霍尔 ZnO? N N 。: p ZnO? 测量对 薄膜中 的化学状态及其光学和电学性质进行了系列的研究结果明所制得的 型 N ; RTA N ,薄膜为高度补偿半导体工艺不仅可以激活薄膜中更多的 受主还可以弱化由薄膜中的施主缺陷造成 。-( FA) PL 3 ,的自补偿效应在低温 光谱中观察到了 种与氮受主相关的光发射并且通过自由电子受主辐射 N ( 128 meV) 。-,复合光发射确定了薄膜中 受主的离化能随着退火温度的升高施主受主对发射峰呈现了略 ,。微的红移现象这可以通过势能波动模型加以理解 PLD;: p ; ZnO? N 光学和电学性质关 键 词型薄 ;膜 81, 15, Fg; 78, 55, Et; 73, 61, Ga PACC: : APACS: 文献标识码+ : O472 ( 3; O472 中图分类号7360F; 7855 : 1000-7032 (2011) 10-0977-06+文章编号 , 4 DOI: 10, 3788/ fgxb20113210097, 7 收稿日期: 20110402; 修订日期: 20110522---- 基金项目: 国家自然学基金 ( 50725205 /60907016) ; 吉林省青年学者科学基金 ( 20080102 ) ; 东北师范大学培养 基 金 ( NENU- STC0800)1 资助项目 作者简介: 王雷( 1982 , ) ,男,吉林德惠人,主要从事宽带隙半导体材料与器件的研究。 E-mail: wangl055@ nenu, edu, cn * : 通讯联系人; E-mail: hyxu@ nen,u edu, cn,ycliu@ nenu, edu, cn 櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬櫬 《》发 光 学 报 ——— (; EI、)核心期刊 物理学类无线电电子学电信技术类 《》发光学报是中国物理学会发光分会与中国科学院长春光学精密机械与物理研究所共同主办的 。、中国物理学会发光分会的学术会刊该刊是以发光学凝聚态物质中的激发过程为专业方向的综合性 。学术刊物 《》1980 1992 ,1996 2004 《,,2000 发光学报于 年创刊曾于 年年年和 年连续四次被中文核心期刊要 目》“”,2000 “、”。总览评为物理学类核心期刊并于 年同时被评为无线电电子学电信技术类核心期刊 2000 。、《( ) 》《》“年获中国科学院优秀期刊二等奖现已被中国学术期刊光盘版中国期刊网和万方数据资 ”。《》( SA) 1999 ; 《》( CA) 《》 源系统等列为源期刊英国科学文摘自 年美国化学文摘和俄罗斯文摘杂志( AJ) 2000 ; 《》2002 ; 《》( CBST,JICST) 2003 自 年美国剑桥科学文摘社网站自 年日本科技文献速报自 年 2008 Esever Bbographc Databases 2010 ;“liilii”;已定期收录检索该刊论文年被荷兰确定为源期刊年被美国 EI。2001 “”“”,《》“确定为源期刊年在国家科技部组织的中国期刊方阵的评定中发光学报被评为双效期 ”。2002 2001 ， 2002 “”。2004 《刊年获中国科学院 年度科学出版基金择重资助年被选入中国知识资源 ?》。、,,总库中国科技精品库本刊丰富信息量大主要反映本学科专业领域的科研和技术成就及 ,,。时报道国内外的学术动态开展学术讨论和交流为提高我国该学科的学术水平服务 《》2011 。: 40 ,480,A4 ,144 ,发光学报自 年改为月刊开本页国内外公开发行国内定价元全年 ,。《》、,。元全国各地邮局均可订阅发光学报欢迎广大作者读者广为利用踊跃投稿 : 3888 22-1116 / O4: CN 地 址长春市东南湖大路 号国内统一刊号 : ISSN 1000-7032 国际刊号《》发光学报编辑部 12-312 : 国内邮发代号国外发行: 130033邮 编 : 4863BM代号 : ( 0431) 86176862,84613407电 话 http: / / www, fgxb, org E-mail: fgxbt@ 12,6 com