脉冲激光沉积制备一维有序氧化物纳米结构的研究进展 
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1 引言
一维有序纳米材料是指横向方向为纳米尺度(1~100 nm)、长度方向为宏观尺度的结构材料,其主要结构形式包括纳米管[1-4]、纳米线[5-7]、纳米柱[8-10]和纳米带[11-13]等。一维有序纳米材料不仅具有大的比表面积,而且具有取向有序性,为研究电、光、热等特性的尺寸效应和量子效应提供了一个完美的研究主体[14]。此外,一维有序纳米结构作为一个整体,可以体现纳米结构单元的集体效应,具有单一纳米结构单元所不具备的协同效应和耦合效应等,可直接被应用于多种功能器件(如光子晶体、光栅、存储单元等[15-20])。
功能氧化物具有比半导体和金属复杂得多的化学配比、离子价态和晶体结构,呈现出了丰富的、奇异的物理特性,如离子导体、多铁性、电致电阻效应、光电效应、磁光效应和非线性光学等[21-28]。功能氧化物的一维有序纳米结构由于维度降低,相应的电子态被限制在尺度小于电子平均自由程的体系中,电子电荷、自旋、轨道、晶格之间的关联作用加强,从而表现出了与块体材料行为特征相关却又截然不同的新奇的物理特性。除了众所周知的纳米结构能级量化外[29],这些奇特的物理特性还包括熔点和热导率的降低、量化的电导/电阻率、高度的磁各向异性、较低的激发阈值,以及沿一维纳米结构纵轴的光偏振调制[30-35]。除此之外,将具有不同电学、磁学、光学等性质的功能氧化物在原子尺度上精确地堆叠外延生长在一起,形成具有周期性结构的一维纳米超晶格或有序的纳米复合材料,在功能交叉耦合和量子尺寸效应的协同效应下,就可制备出具有特殊光、磁、电学特性的人工复合“超材料”[36-39]。近年来,功能氧化物一维有序纳米材料的控制精确合成和控制组装技术已成为学术研究和工业应用的前沿热点。
目前,功能氧化物一维有序纳米材料可控可靠的制备方法有多种多样,包括水热法[40-41]、热蒸发法[11,42]、化学气相沉积(CVD)法[43-45]、磁控溅射法[46-47]、熔盐法[48]、模板法[49-50]和一些复合方法[51-54]。作为制备氧化物一维有序纳米结构的重要方法之一,脉冲激光沉积(PLD)法具有许多优点,如:良好的保成分性、原子级的生长精度控制、工艺参数任意调节、极大的工艺兼容性,已广泛应用于原位生长高质量、低缺陷密度、成分复杂的氧化物材料[55-58]。PLD法制备氧化物一维有序纳米结构主要是通过与基于模板或催化剂阵列的常规纳米制造工艺相结合来实现的。同时,PLD过程是一个热动力学高度非平衡的过程,具有易于控制、快速凝聚、低压、高能量等特点,通过精确控制多维度制备参数,可在不采用模板或催化剂的情况下,利用晶体生长模式的改变实现氧化物一维有序纳米结构的自组装制备。PLD技术从过程复杂、容易引入杂质的传统模板/催化剂辅助纳米结构制备形式,转向控制方便、结构有序的自组装制备形式,顺应了当前该领域的发展趋势,是研究人员关注的重要方向之一。
本文首先概述了PLD技术的原理和特点,系统介绍了PLD制备氧化物一维有序纳米结构的方法和机理,着重分析了PLD自组装一维有序纳米结构技术的原理和应用实例;然后总结了近年来PLD应用于典型氧化物一维有序纳米结构制备的研究进展;最后指出了PLD制备一维有序纳米结构面临的挑战,并展望了超快激光在该技术中的应用前景。
2 PLD制备有序纳米结构的方法和机理
PLD系统主要由激光源、聚光镜、目标靶材、真空腔、冷却环、真空泵和气流阀等组成,如
PLD的整个过程包含着复杂的物理现象,涉及到高能量脉冲辐射冲击固体靶材时激光与物质之间的物理相互作用,等离子体羽辉的形成、扩散,蒸发物质通过等离子体羽辉到达热基片表面发生的吸附、扩散和凝聚,以及最终的材料生长、微观结构演化[60]。
PLD被广泛用于薄膜材料的制备,如半导体氧化物薄膜[61-64]、陶瓷氧化物薄膜[65-67]、非氧化物薄膜[68-71]和其他涂层[72-74]等的制备,同时也被应用于零维[75-77]、一维[78-80]微纳结构材料的制备。不同材料和结构的制备方法和机理不尽相同。以下将系统讨论制备一维有序纳米结构的几种典型方法和机理。
2.1 模板辅助法
将PLD法和基于模板的纳米制造工艺相结合是常见的一维有序纳米结构的制备路线。该方法首先在基底上制备孔径为纳米级到微米级的多孔模板,脉冲激光剥蚀产生的高能量等离子体羽辉中的活性粒子被输送到模板的孔壁上并快速凝结,形成均匀有序的一维纳米结构。常用的模板材料包括多孔氧化硅和多孔氧化铝[81],其中阳极氧化铝(AAO)是一种非常均匀的自组装纳米结构阵列材料,已被广泛应用于制备低维纳米结构。目前制备的AAO膜孔径分布在20~200 nm之间,膜厚分布在10~100 nm之间,孔隙率高达1011 cm-3。AAO膜的孔径大小一致,可制备孔径相同、单分散的纳米结构阵列,因此,模板法具有良好的可控性。这种AAO模板阵列材料不仅是纳米科学基础研究的热点材料,而且在高存储密度硬盘、场发射器件、高效蓄电池、纳米传感器、光子晶体等领域也具有广阔的应用前景。
科研工作者已利用模板辅助PLD法制备了一系列一维有序纳米结构材料。2008年,Lee等[82]用超薄AAO掩模辅助PLD技术,在Pt/MgO(100)和Nb∶SrTiO3(100)单晶基底上沉积了大面积外延铁电Pb(Zr0.20Ti0.80)O3(PZT)纳米阵列。2009年,Li等[83]将聚苯乙烯(PS)单层胶体晶体作为模板,采用Nd∶YAG激光源在Si基底上直接生长了垂直有序排列的Co3O4纳米柱阵列,该纳米柱阵列具有可精确控制的表面粗糙度和形貌特征。2009年,Gao等[53]以AAO为模板结合PLD技术,合成了磁性CoFe2O4(CFO)有序纳米点阵列,该阵列表现出了微弱的磁化滞后回路和独特的温度依赖磁性行为。2017年,Tian等[84]以AAO为模板,将PLD法与离子束刻蚀相结合,制备了多铁性BiFeO3(BFO)有序纳米环阵列(纳米环的内径为12 nm,壁厚为30 nm,高度约为10 nm),制备过程如
图 2. AAO模板辅助PLD法制备纳米环阵列示意图[84]
Fig. 2. Schematic of the template-assisted PLD for growing nano-ring arrays[84]
模板辅助法可以比较容易地控制纳米结构的长度、直径、分布,但制备后需要将纳米结构从模板中分离出来,分离步骤复杂且过程冗长,容易在分离过程中引入杂质,限制了此方法在实际器件制备中的应用。
2.2 催化剂辅助法
PLD技术还可以在金属催化剂的辅助下,于高温环境中通过气液固相(VLS)反应制备氧化物一维有序纳米结构[85]。气液固相生长模型是制备一维纳米结构最为成熟的理论之一。一维纳米结构的生长过程可通过Wagner公式表述为
式中:Rmin、V1、σlv、S、R、T分别为纳米晶的最小半径、金属催化剂液滴的摩尔体积、气液表面能、气相过饱和度、气体常数、反应温度[86]。如
气液固相反应已被广泛应用于制造基于纳米线结构的半导体原型器件,如逻辑电路、LED和气体传感器等[91-93]。
目前,通过催化剂辅助PLD法制备的一维纳米结构材料包括Sn
催化剂辅助PLD技术发展得较早,但金属催化剂最终会作为杂质存在于纳米结构中,容易形成缺陷,且其去除过程比较复杂,因此限制了其在纳米器件制备方面的应用。近年来,开展无催化剂辅助PLD技术制备氧化物一维纳米结构的研究引起了人们的极大兴趣。
2.3 自组装法(无模板/无催化剂)
模板或催化剂辅助PLD技术是制备一维有序纳米结构的常规方法,但存在制备过程繁冗复杂、结晶质量不高等缺点。PLD技术是一种热动力学平衡态高度可控的沉积技术,它可基于多维激光参数和制备参数对材料的生长过程进行精确控制,使得通过调制晶体生长模式实现功能氧化物一维有序纳米材料的自组装成为可能。然而,由于对氧化物纳米结构的晶体生长过程和机理缺乏深刻认识,人们在利用晶体生长的微观结构成形控制自组装技术制备取向良好的垂直有序纳米结构方面仍面临巨大挑战。下面将系统介绍几种常见的PLD自组装氧化物一维有序纳米结构的制备方法。
2.3.1 纳米粒子辅助法
作为一种制备高质量薄膜材料的沉积技术,PLD技术通常是在相对较低的氧气压强(<1 Pa)下进行的。而改进的纳米粒子辅助脉冲激光沉积技术(NAPLD)采用的是相对较高的气氛压强(几十到几百帕),可促使等离子体羽辉中形成较大的气相原子团簇。这些原子团簇在基底上形成了均匀分布的液滴状晶种层,该晶种层作为晶核点可以引导有序纳米结构成形,在没有模板或催化剂的情况下,遵循气固(VS)生长机制实现一维有序纳米结构的制备[107-111]。
2003年,Yan等[92]提出了形核引发的电场辅助生长模型,然后在外延生长的GaN层和蓝宝石基底上制备了高取向的Ga掺杂ZnO纳米柱阵列,其中Ga的掺杂水平在ZnO纳米柱的形成中起关键作用,而氧分压和基底温度也会影响纳米柱的形貌。2006年,Sun等[112]发现:在Si基底上直接生长的ZnO柱呈针状,其直径与长度分别在20~60 nm和200~800 nm范围内,并且大多数情况下其尖端覆盖着ZnO颗粒;若在基底上预沉积一层ZnO薄膜,则可得到较长(1~1.2 mm)、更薄(6~20 nm)的致密纳米柱阵列,而且无明显的颗粒覆盖。2006年,Liu等[113]在60~250 Pa 相对较高的背景压强和550~700 ℃的基底温度下,合成了直径不同的ZnO纳米柱。2009年,Fuge等[114]使用两阶段扩散脉冲激光沉积(DPLD)技术(先采用脉冲激光烧蚀ZnO靶材形成约50 nm厚的种子层,然后将样品转向远离烧蚀羽流的传播方向)生成了密集的超薄纳米柱阵列,这些纳米柱的直径约为10 nm,其纵横比比同条件下传统PLD技术生长的纳米柱高20倍。如
图 4. NAPLD法制备垂直排列的ZnO纳米柱示意图[111]
Fig. 4. Schematic of the growth of vertically aligned ZnO nanorods using NAPLD process[111]
NAPLD制备的纳米结构的尺寸仅取决于生长条件以及初期成核密度和成核尺寸,这种方法制备的纳米结构的位置、密度、尺寸、结晶度和缺陷受生长温度、环境气氛、退火温度、脉冲激光频率的影响很大。此外,NAPLD生长的纳米结构是在高气氛压强下沉积的,难以避免产生生长缺陷,这些缺陷会影响纳米结构的结晶质量以及电学和光学特性。
2.3.2 表面扩散限制法
PLD过程包含多种表面原子的运动过程,如扩散、成核、附着/分离和层间运输等。表面扩散系数的增加会促使等离子体羽辉形核后聚集,这意味着材料在较大厚度时能达到连续,从而形成致密的薄膜。然而,在形核聚集过程中存在许多生长不稳定因素,如扩散受限导致的聚合、团聚、错位等。这种不稳定的生长过程与理想的逐层致密生长所需的表面平滑过程相竞争,导致了生长缺陷的产生和生长表面的粗糙化。在常规氧化物薄膜的外延过程中,为了获得原子级表面平整均匀的薄膜材料,科研人员尝试通过调整实验参数来提高表面扩散系数,促进形核聚集的快速完成。
然而,本研究团队[117]发现,通过调整关键制备参数适当降低表面扩散系数,可在一定程度上抑制等离子体羽辉在衬底表面的形核聚集,提高生长表面粗糙度,改变致密生长机制,制备出疏松的一维有序纳米结构。如
图 5. 表面扩散限制法制备一维垂直有序纳米结构的生长机理示意图[117]
Fig. 5. Schematics of the growth mechanism of one-dimensional well-ordered nanostructures by limiting surface diffusion[117]
沉积速率是决定表面形态和结晶质量的重要参数。以二维晶格模型为例,相邻两个原子到达基底的平均时间间隔可以表示为[118]
式中:v为沉积速率;a为最近相邻原子的距离;n为铺满单层的原子数。沉积速率越高,两个连续沉积的原子到达基底的时间间隔越短,新进入的原子快速覆盖已吸附原子,极大地缩短了吸附原子在基底表面的扩散时间,从而减小了吸附原子的表面扩散系数。
本研究团队采用PLD技术制备了具有不同的电、磁、光等物理特性的具有原子级清晰界面的高质量氧化物一维有序单晶纳米结构材料,如TiO2、CeO2、Y2O3、CoFe2O4等[117,119-120],并制备了CeO2/Y2
2.3.3 晶化自主分离法
诸多研究发现,在合适的氧化物组合下,采用PLD技术共沉积方法能使其中一种氧化物相自发地形成纳米柱镶嵌于另一种氧化物基体中,从而形成一种特殊的多维纳米复合结构[122-124]。在这种嵌入式多维纳米复合结构中,氧化物相之间的界面会产生高密度、强关联的电子电荷、自旋、轨道、晶格耦合,促进了各种新奇物理效应的产生,使新型器件的设计成为可能。
最典型的纳米复合材料是单晶尖晶石纳米柱异质外延嵌入钙钛矿基体形成的复合磁电纳米结构薄膜[125],其中基质是压电性BiFeO3,纳米柱是压磁性CoFe2O4。这两种氧化物相的表面能不同,因此其在基底表面的润湿性不同,最终使得这两种氧化物相在晶化过程中自主分离组装成了复合纳米结构材料。
根据Winterbottom模型,晶核的形状由基底表面能γ1、晶相表面能γ2、基底与晶相界面的表面能γ12决定,晶相在基底上的润湿能力由Δγ=γ12-γ1决定。若Δγ≤-γ2,则该晶相能完全润湿基底,其生长过程遵循不存在结晶势垒的逐层生长模式;若γ2≥Δγ≥-γ2,则该晶相能部分润湿基底,但需要克服一定的结晶势垒成核,从而遵循岛状生长模式(Volmer-Weber模式)。
以下以钙钛矿-尖晶石系统[126]为例进行阐述。如
图 6. 在{001}和{111}表面晶化自主分离得到钙钛矿-尖晶石复合纳米结构薄膜示意图[126]
Fig. 6. Schematics of the perovskite-spinel composite nanostructured film by crystallization autonomous separation on {001} and {111} surfaces[126]
另一种采用PLD制备的纳米复合结构材料是引入纳米柱作为人工钉扎中心的超导氧化物材料,它可以改善磁场作用下超导体的临界电流密度。2008年,Teranishi等[127]采用PLD技术通过激光剥蚀混合了BaMO3 (BMO, M=Zr,Sn)的ErBa2Cu3O7(EBCO)陶瓷靶材,在SrTiO3 (STO)(100)基底上制备了BMO纳米柱复合EBCO薄膜,BMO纳米柱的直径为10~20 nm;他们对EBCO薄膜进行研究后发现,在平行于c轴的磁场作用下,BMO纳米柱复合EBCO薄膜的临界电流密度得到了增强。2007年,Ichinose等[128]通过改变靶材中的BaZrO3含量以及交替烧蚀包含BaZrO3的YBa2Cu3O7混合靶材和纯YBa2Cu3O7靶材,对BaZrO3纳米柱的长度和密度进行了调控。
3 PLD制备一维有序纳米结构氧化物的类别
功能氧化物一维有序纳米结构在新型纳米器件设计和传统器件升级(如场发射显示器、高密度存储元件、纳米谐振器、紫外线传感器、气体传感器等)方面具有广阔的应用前景。在该节,本文将介绍近年来PLD在典型氧化物纳米结构制备方面的研究进展。
3.1 二元氧化物
3.1.1 ZnO
ZnO是PLD制备的重要氧化物材料之一。已报道的一维ZnO纳米结构主要包括线状、针状、柱状、纤维状、管状、指甲状及带状[129-135]。一维ZnO纳米结构具有直接带隙、高激子结合能(60 meV)、高迁移率、高比表面积和长径比、高强度、高导热性和良好的热稳定等,已被广泛应用于太阳能电池、气体传感器、激光器、紫外光探测器、发光二极管、压电转换器件和阻变存储器等[5,136-142]。一维ZnO纳米结构的PLD制备可分为催化剂辅助法和纳米粒子自组装两类。
2005年,Zhang等[143]以飞秒激光作为光源,Au作为催化剂,合成了一维有序ZnO纳米线结构。2010年,Yang等[144]采用PLD技术在高温高压下于Si基底上先沉积一层约10 nm的Au层,然后烧蚀ZnO∶Eu2O3复合靶材,制备了掺Eu的ZnO纳米线;他们对该纳米线进行研究后发现,该纳米线顶端覆盖着Au-Zn合金颗粒,证实了这种催化剂辅助法制备的一维ZnO纳米线结构遵循气液固相生长机制。2011年,Palani等[145]以Sb作为催化剂在Si基底上制备了ZnO纳米结构,但由于Sb的温度敏感性,制备的ZnO纳米具有纳米线和纳米片两种结构,前者在光致发光光谱中表现出了强烈的绿光发射特性。
2009年,Premkumar等[146]分别采用Nd∶YAG (1064 nm, 532 nm) 激光和KrF (248 nm) 激光烧蚀ZnO靶材,在Al2O3和GaN基底上沉积了ZnO薄膜,结果发现:只有当激光波长为532 nm时,才能够在GaN和Al2O3基底上制备一维ZnO纳米柱结构,所制备的ZnO纳米柱源于生长初始阶段在基底表面形成的ZnO亚微米晶核层。Premkumar等采用的方法是一种纳米颗粒自组装PLD生长方法。2011年,Liu等[147]探究了三种不同能量密度(4.0, 1.8, 1.2 J/cm2)下自组装生长的ZnO纳米柱的形态以及光致发光和氧气传感特性,结果发现,能量密度减小时相应的纳米柱长度、直径、密度都减小,且垂直度变好,如
图 7. 三种不同激光能量密度下生长的ZnO纳米柱的俯视图和横截面SEM图像[147]。(a~b) 4.0 J/cm2;(c~d) 1.8 J/cm2;(e~f) 1.2 J/cm2
Fig. 7. Top view and cross-sectional view SEM images of ZnO nanorods grown under three different laser influences[147]. (a-b) 4.0 J/cm2; (c-d) 1.8 J/cm2; (e-f) 1.2 J/cm2
除此外,PLD生长的一维ZnO纳米结构的形貌与光学性能可以通过调节生长参数(如基底温度、氧分压和生长时间等[57,110,148])来控制。在制备ZnO一维有序纳米结构的PLD方法中,纳米粒子辅助自组装法无催化剂或模板,制备过程简单,在制备ZnO纳米结构上具有更大的潜力。
3.1.2 TiO2
一维TiO2纳米结构具有出色的电子电荷传输特性、离子交换/嵌入活性、吸附/光催化特性和高的表面体积比,在光催化(包括污染物降解、CO2转化为能量燃料、水分解等)、电池(含染料敏化型、量子点敏化型和钙钛矿型太阳能电池以及锂电子电池等)、超级电容等领域应用广泛[149-156]。
本研究团队[119]采用PLD技术,通过表面扩散限制法,自组装制备了具有高比例{001}表面刻面的一维锐钛矿型TiO2“纳米刷”结构,如
图 8. 具有{001}高活性表面刻面的单晶TiO2纳米刷[119]。(a) TEM截面微观形貌图;(b) TiO2纳米刷、纳米颗粒和纳米薄膜的光电转化I/V曲线
Fig. 8. Single-crystallineTiO2 nanobrushes with high energy {001} facets [119]. (a) Cross-sectional SEM images showing the nanobrush microstructure; (b) photovoltaic I/V curves of TiO2 nanobrushes, nanoparticles, and thin film
2009年,Li等[157]以单层聚苯乙烯胶体为模板,采用PLD技术,制备了周期排列的TiO2六角形纳米柱,如
图 9. 六角形TiO2纳米柱阵列[157]。(a) SEM表面形貌图; (b) SEM截面形貌图;(c)场发射I-V曲线;(d)场发射增强因子与阵列周期的关系
Fig. 9. Hexagonal nonclose-packed TiO2 nanorod arrays[157]. (a) SEM image of the surface morphology; (b) SEM image of the cross-sectional morphology; (c) field emission I-V curve; (d) the relationship between field-enhancement factor and array period
3.1.3 WO3
氧化钨(WO3)是一种带隙为2.6~3.0 eV的n型半导体金属氧化物,具有独特的电致变色[159]、光致变色[160]、热致变色[161]和气致变色[162]等特性,被广泛应用在智能窗户、传感器、催化剂、电池、超级电容上[163-167]。
2011年,Ponzoni等[169]采用PLD技术制备了由纳米颗粒和纳米柱组成的具有不同形貌特征的WO3纳米结构材料;对其进行研究后发现,以纳米柱为主的纳米结构对氨气表现出更高的敏感度,以纳米颗粒为主的纳米结构的气体敏感性更高,这些差异有助于获得选择性气体检测器件。2012年,Ahmad等[170]使用193 nm ArF激光器,采用PLD技术,在电导传感器上成功制备了用于H2和乙醇传感器的WO3纳米柱结构。2014年,Huang等[168]在低氧背景压强下,使用193 nm KrF准分子激光器,在W、Ta和Cu基底上制备了WO3纳米柱结构。
图 10. 采用PLD技术在不同的W基体温度下制备的WO3纳米柱[168]
Fig. 10. WO3 nanorods prepared by PLD with varied W substrate temperature[168]
3.2 多元氧化物
多元氧化物材料通常具有各种突出的特性,例如铁电、压电和超导特性[171-173],常被应用于功能电子器件上,如非易失性存储器、微型电动机和传感器等[174-176]。虽然以钙钛矿ABO3和AB2O4结构为主的多元氧化物具有丰富的物相,但钙钛矿的相稳定性较差,大大限制了其一维纳米结构的制备。因此,与二元氧化物相比,关于多元氧化物一维纳米结构的研究较少。但近年来,随着PLD技术的发展以及对PLD生长技术的深入了解,多元氧化物一维有序纳米结构的报道逐渐增多。
3.2.1 CoFe2O4
2004年,Zheng等[124]采用PLD技术,在STO基底上制备了纳米结构的BaTiO3-CFO纳米复合铁电磁体,BaTiO3基体内镶嵌的CFO纳米柱的尺寸均匀,平均间距在20~30 nm之间。2005年,Li等[177]采用PLD技术,分别在具有{001}和{110}取向的STO单晶基底上自组装生长了PbTiO3-CFO复合纳米结构薄膜;结果发现,两种基底上都生长了包含有垂直柱状或片柱状CFO的复合纳米结构,但在{001}取向基底上生长的结构平行于{110}面,而在{110}取向基体上生长的纳米结构平行于{111}面。2020年,Tang等[178]采用PLD技术在Pb(Mg1/3Nb2/3)0.70Ti0.30O3(PMN-30PT)单晶基底上外延制备了CFO和SrRuO3纳米柱异质结构。这种自组装的纳米柱异质结构作为电极具有增强的介电常数和压电常数。
通过精确控制热力学表面平衡和动力学扩散限制聚集之间的微妙平衡过程,本研究团队[120]采用PLD技术制备了如
图 11. 表面扩散法制备的CoFe2O4纳米刷的结构表征[120]。(a) 纳米刷的STEM截面形貌图;(b)纳米刷侧壁的原子尺度高分辨率STEM图;(c)纳米刷衬底过渡区域STEM截面形貌图;(d)纳米刷衬底界面的原子尺度高分辨率STEM图;(e)纳米刷衬底界面的傅里叶转换图
Fig. 11. Microstructures of CoFe2O4 fabricated by surface diffusion method[120]. (a) STEM image showing the cross-sectional structure of nanobrushes; (b) atomic-resolution STEM image of the sidewall of a nanobrush; (c) STEM cross-section image showing the nanobrush/substrate interface; (d) atomic-resolution STEM image showing the nanobrush/substrate interface; (e) Fourier transform of nanobrush/substrate interface
3.2.2 Pb(Zr1-xTix)O3
在多元金属氧化物中,具有钙钛矿结构的PZT由于具有极高的介电常数、大的磁滞和出色的压电系数而成为最有代表性的压电陶瓷材料之一,被广泛应用于基础研究和实际器件中。2012年,Chen等[179]采用PLD技术在STO基底上外延生长了具有锥度形态的单晶PZT纳米线阵列,并在不同温度和压力下,系统研究了PZT膜或纳米线的生长窗口(见
图 12. PZT纳米线阵列[179]。(a)~(g)不同生长温度下制备的PZT纳米线的SEM界面形貌图;(h) PZT纳米线长度和过渡区PZT薄膜区厚度随生长温度的变化曲线;(i) PZT纳米线在不同温度和压力下的生长窗口
Fig. 12. SEM images of vertically aligned taper PZT nanowires arrays[179]. (a)--(g) SEM interface images of PZT nanowires prepared at varied growth temperatures; (h) the lengths of PZT nanowires and the thicknesses of PZT film in transition region as the function of growth temperature; (i) growth window of the PZT nanowires at different temperatures and pressures
3.2.3 YBa2Cu3O7
YBa2Cu3O7(YBCO)的一维纳米结构可以通过溶胶-凝胶[181-183]、静电纺丝[184]、生物聚合[185]、溶液化学[182]、超声辐照[186]等方法制备。2000年,Zhang等[187]采用PLD技术,在YBCO纳米颗粒上制备了直径在18~96 nm、长度在几微米范围内的一维YBCO晶体纳米柱。如
图 13. 不同温度下采用PLD法生长的YBCO纳米柱[187]。(a) 630 ℃;(b) 680 ℃
Fig. 13. YBCO nanorods grown by PLD at different temperatures[187]. (a) 630 ℃; (b) 680 ℃
3.3 纳米异质结构
一维纳米异质结构包括一维核壳结构与轴向超晶格结构。与二维纳米结构相比,一维纳米异质结构在发光二极管、激光器、传感器、生物标签、量子器件和热电材料中的应用吸引着越来越多的目光[188-195]。
2002年,Wu等[196]基于气固液相生长机制,采用PLD与CVD复合的方法合成了具有周期性纵向异质结构的Si/SiGe单晶纳米线。首先,在850~950 ℃的反应温度下,使基底表面的Au薄膜与Si基体形成液态合金,并自发地分解成纳米尺度的液滴;随后采用激光烧蚀Ge靶材产生Ge蒸气,Ge蒸气和Si液滴都溶解在合金液滴中,并从固液界面析出SiGe合金,通过交替打开关闭激光器可得到Si/SiGe超晶格纳米线。2005年,Wu等[197]使用Nd∶YAG激光器,将PLD技术与CVD技术相结合,在Si基底上生长了沿{0001}方向取向的ZnS/CdSe核-壳纳米结构。与之相似,2011年,Choi等[198]设计了热辅助PLD系统,采用248 nm准分子激光器在热炉供热氛围中生长出毛刷状一维SnO2-ZnO异质结构,这种结构具有较大的比表面积,特别适宜应用于化学传感器领域。2005年,Hayden等[199]制备了多晶径向异质结构纳米线,该结构由p型Si芯和n型CdS壳组成,可被用来制作纳米发光二极管。2010年,Park等[200]采用静电纺丝和PLD相结合的方法制备了SnO2-ZnO复合纳米纤维,即先用静电纺丝法在Si基底上制备ZnO纳米纤维,然后用PLD法沉积SnO2,最后进行高温退火;对SnO2-ZnO复合纳米纤维结构进行研究后发现,该结构在200 ℃下对NO2气体浓度的响应非常高。
多数一维纳米异质节结构都需要通过复合两种或两种以上方法或步骤进行制备,用PLD一步合成一维纳米异质结构比较困难,但研究人员仍取得了一定突破。2008年,Huo等[201]在蓝宝石基底上用PLD直接生长了ZnO/Zn0.85Mg0.15O一维超晶格纳米针结构,研究后发现,ZnO缓冲层有助于提高超晶格的质量。本研究团队采用PLD技术,通过调控、限制表面扩散过程并利用几何阴影效应,成功地在Si基底上合成了一维CeO2/Y2O3超晶格纳米刷结构[121]。如
图 14. 一维CeO2/Y2O3纳米超晶格结构[121]。(a) STEM截面形貌图;(b)原子探针断层扫描重建一维CeO2/Y2O3纳米超晶格的三维结构
Fig. 14. One-dimensional CeO2/Y2O3 nanobrush superlattice[121]. (a) A STEM image showing its cross-sectional structure; (b) three-dimensional structure of one-dimensional CeO2/Y2O3 nano-superlattice reconstructed by atom probe tomography
4 结束语
PLD是一种被广泛应用的制备氧化物薄膜的方法,也是制备氧化物一维有序纳米结构的重要方法之一。本文综述了PLD制备一维有序纳米结构的方法和机理,并介绍了二元氧化物、多元氧化物及纳米异质结构的研究进展。最后,本文将讨论PLD制备一维有序纳米结构过程中纳米结构成形控制难题的解决思路,以及超快激光在该技术中的应用前景。
1)纳米结构成形控制
一维纳米结构在催化、光电转化、新能源、微电子器件等领域有着广阔的应用前景。但是一维纳米结构的性能和应用不仅取决于其化学组成,还与纳米结构的形貌特征(晶体取向、表面刻面、界面取向、界面成分、尺寸、密度等)密切相关。随着高新技术的发展,器件的高度集成和微小化对纳米结构的尺寸和形貌提出了更为苛刻的要求,需要通过控制纳米结构的尺寸和形貌对其性质进行优化。因此,一维纳米结构制备的一个重要目标就是获得有序、稳定性好、纳米结构形貌可控的纳米结构。根据不同的用途,寻找简单的方法,制备尺寸、形貌可控的一维纳米结构具有非常重要的意义。然而,迄今为止,制备可控晶体形态、取向和表面结构的纳米材料仍然是一个重大挑战。在一维有序纳米结构的PLD制备中,与制备参数相关的晶体成核以及生长过程是控制一维纳米结构尺寸和形貌的关键。因此,纳米结构的成形控制在很大程度上取决于对晶体生长机理和激光剥蚀等离子羽辉演化机理的进一步研究和深入了解。
在PLD纳米结构制备中,决定纳米结构成形的主要因素包括晶种相的选取、晶体生长的热力学和动力学控制、生长环境的调控。纳米结构成形是生长动力学和热力学之间的平衡,晶体生长形貌首先取决于晶体结构的对称性、结构基元间的作用力、晶格缺陷等。在PLD制备中,晶种相的选取可控制成核密度、成核晶向,对纳米结构成形密度、尺寸、取向的影响较大;通过对衬底与材料的晶格匹配性进行筛选,可有效利用晶体生长应力对成核初期的表面起伏进行控制,从而影响纳米结构成形密度、尺寸和晶体取向。对纳米结构成形控制的研究,不能局限于某一方面,既要注意到晶体结构因素,又要考虑到生长环境的影响(氧分压、衬底温度、等离子体相组成和杂质等对纳米结构成形具有较大影响)。其中,激光剥蚀等离子体中活性粒子的动能控制着生长表面的扩散过程,对一维纳米结构单元尺寸、纳米单元间距以及表面刻面调控具有重要影响。
2)超快激光PLD的发展
目前,纳秒脉冲激光器是PLD技术中采用的主流激光器。然而,纳秒PLD存在诸多缺点:首先,纳秒激光脉冲宽度长,激光束与靶材作用时间长,激光能量通过电子晶格耦合过程在靶材中形成热积累,对靶材质量造成不可逆的热损坏。同时,靶材表面的热积累导致激光作用区域内的靶材表面熔融,熔融液滴或靶材碎片会溅射到基板上。靶材的热损坏和液滴溅射都会严重影响所制备材料的质量(包括衬底附着性降低、表面微颗粒形成和化学计量比失配)。其次,纳秒脉冲激光在剥蚀高导热性和透明材料方面存在困难。因此,为了提高对宽禁带、透明、光吸收率低的材料的剥蚀效率,在PLD过程中通常采用波长为193 nm(ArF准分子激光)、248 nm(KrF准分子激光)和266 nm(Nd∶YAG固体激光器的四倍频输出)的紫外激光。
随着超快激光技术的快速发展,近年来,超快脉冲(皮秒或飞秒)激光被广泛应用于PLD技术中,用以克服传统纳秒PLD中存在的问题。已有人采用超短脉冲激光生长了新型材料,例如,具有高比例sp3键[202]和高生长速率且无微米级液滴[203]的类金刚石碳膜。超短脉冲激光的两个显著特征是极高的峰值功率密度(高达1021 W/cm2)和极短的激光脉冲宽度(10-14~10-15 s)。超快激光与纳秒激光的电离机制完全不同。首先,超快激光的高峰值功率密度可引发多光子吸收过程,解决纳秒PLD中材料剥蚀率对光波长的依赖问题,实现同一波长的激光可剥蚀任意材料。以Si为例,超短脉冲激光的波长是800 nm,只稍稍高于Si的带隙宽度(1.12 eV),如果采用激光量子能量稍大于Si带隙宽度的连续激光束聚焦在Si表面,电子就会通过耦合声子的间接激发方式被激发到导带中,激光能量大部分转化为热能,剥蚀效率低;但是,如果采用超短脉冲激光,在其超强的峰值功率密度(大于1013 W/cm2)下,电子被激发到导带中,可以连续吸收第二个光子,从而诱导非线性雪崩电离过程,光吸收率随着激光能量密度增大呈指数增大。非线性吸收特性使得超短脉冲激光的吸收发生在靶材表面浅层区域,剥蚀精度高,可制备的材料种类广。其次,超短激光脉冲具有超窄的脉冲宽度(10-14~10-15 s),脉冲宽度小于电子-声子弛豫时间(几到几十皮秒),所以超短脉冲激光剥蚀对靶材的热影响小,在很大程度上避免了长脉宽、低强度纳秒脉冲激光造成的材料表面熔融和热损坏,大大提高了剥蚀精度。
除此之外,研究人员还发现超快激光PLD具有一个特殊的现象:在较低的激光通量下,超短脉冲激光的等离子体富含电子、高能离子和活性原子。但当激光通量很大时,纳米级粒子团簇会在超快激光剥蚀等离子体羽辉中自动形成,无需施加高压背景气体来诱导成核[204-206]。激光剥蚀等离子体羽辉中自发形成的纳米粒子是一维有序纳米结构成形的有利条件。如果可以在相对低的背景气压下制备功能氧化物一维有序纳米结构,就可以大大提高纳米结构材料的结晶质量。
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Article Outline
范丽莎, 张硕文, 张群莉, 姚建华. 脉冲激光沉积制备一维有序氧化物纳米结构的研究进展[J]. 激光与光电子学进展, 2020, 57(19): 190001. Lisha Fan, Shuowen Zhang, Qunli Zhang, Jianhua Yao. Research Progress on Fabrication of One-Dimensional Well-Ordered Oxide Nanostructures by Pulsed Laser Deposition[J]. Laser & Optoelectronics Progress, 2020, 57(19): 190001.
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