CN110195217B - 一种制备β-Ga2O3薄膜方法 - Google Patents
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Abstract
一种制备β‑Ga2O3薄膜方法属于微电子技术领域,解决制备β‑Ga2O3薄膜存在混相和晶体质量差的问题。该方法先利用等离子体增强原子层沉积在蓝宝石衬底上生长Ga2O3薄膜,然后再进行高温退火重结晶,将亚稳态的Ga2O3转化为稳态的,最后采用金属有机物化学气相沉积技术生长β‑Ga2O3薄膜。本发明制备单相β‑Ga2O3方法可为后面再制备较厚的β‑Ga2O3材料和器件奠定基础。
Description
技术领域
本发明属于微电子技术领域,涉及半导体材料科学技术领域,具体涉及一种制备β-Ga2O3薄膜方法。
背景技术
在继宽禁带半导体材料SiC/GaN之后,超宽带隙(UWB)半导体是一种新兴的半导体,与传统小带隙Si基芯片相比,它的工作温度和功率都要高得多。因此,超宽带隙(UWB)半导体它在节能减排、信息技术以及国防装备等领域有重要的应用前景。超宽禁带半导体氧化镓(Ga2O3)材料具有有α,β,γ,δ,ε五种同分异构体晶体结构,其中β-Ga2O3结构最为稳定并能和其他四种氧化镓之间互相转化。β-Ga2O3在日盲紫外和可见光区域具有优良的透光率(>80%),已经很好的适合了日盲紫外探测区域的需要,不需要通过掺杂等手段来调节其禁带宽度。β-Ga2O3击穿场强高,在功率耐压器件中也有广阔的应用前景。然而制备β-Ga2O3单晶材料十分困难,且价格昂贵。目前报道的用于制备β-Ga2O3的方法包括射频磁控溅射、分子束外延、金属有机物化学气相淀积(MOCVD)、脉冲激光沉积和原子层沉积(ALD)等等。其中原子层沉积法是脉冲交替,逐层成膜,周期循环沉积的,在每个周期中,设备可控制沉积在衬底材料分子的量,且沉积过程受温度影响效果较弱,沉积的薄膜具有良好的共形性和均匀性。但是用该法沉积的Ga2O3薄膜处于亚稳态,易转化为多晶形式Ga2O3,无法得到期望的β-Ga2O3单晶,进而影响包括日盲紫外探测器在内的基于β-Ga2O3的光电器件的性能。因此,需要找到一种便于制备高晶体质量、高光电性能的β-Ga2O3薄膜的方法。
发明内容
针对沉积过程中存在的上述问题,本发明提出了一种β-Ga2O3薄膜的制备方法,通过此法获得的制得的β-Ga2O3薄膜具有较高的晶体质量和光学特性。
本发明提出的技术方案如下:
一种制备β-Ga2O3方法,包括如下步骤:
选择蓝宝石衬底;
利用等离子体增强原子层沉积法在蓝宝石生长Ga2O3薄膜,
将沉积后的Ga2O3薄膜在LPCVD管式炉中退火,
再采用MOCVD技术生长Ga2O3。
一种制备β-Ga2O3方法,其特征在于包括如下步骤:
(1)选c面蓝宝石衬底,等离子体增强原子层沉积Ga2O3薄膜时,设置射频等离子体功率为1800-2000W,沉积温度为240-270℃,以氮气为载气;
(2)等离子体增强原子层沉积依次为:①通入TMGa源0.1-0.2s,TMGa 流量为190-220sccm;②通入氮气5-10s;③通入氧气15-25s,氧气的流量为 190-220sccm;④通入氮气5-10s;⑤将①步到④步依顺序循环重复400-440 次;
(3)向LPCVD管式炉中通入氮气,将沉积的Ga2O3薄膜放入炉中,退火时炉中温度为850-1050℃;退火时间为0.5-2小时。
(4)将退火后的薄膜进行金属有机物化学气相沉积(MOCVD)生长β-Ga2O3,生长温度550-650℃。
所述的β-Ga2O3制备方法,其机理和特点在于:
本发明中,首先采用等离子体增强原子层在蓝宝石衬底上沉积Ga2O3材料,辅助了ALD能量增强,使用的反应剂活性提高。等离子体用于激活脉冲中的氧气,可加快沉积速率并降低反应需要的温度。在沉积过程中通入纯净氮气,将前一步反应残留的反应物及生产的其他物质吹扫并排出反应室,保证下一步反应时薄膜具有清洁表面,避免沉积的薄膜中存在杂质,进而保证薄膜具有较高的晶体质量。其次,沉积后Ga2O3容易以多晶形式的存在,高温热退火处理制备出β-Ga2O3关键是对积聚或重熔的粒子实现重结晶的过程,该步骤可将沉积的亚稳态Ga2O3薄膜转化为需要的β-Ga2O3。退火过程采用氮气气氛下,相比于其他常见气体(如氧气),在这个过程中氮气可以起到载气的作用,提高了原子表面迁移率,并且在高温的条件下使Ga和O原子能够获得足够的能量迁移到合适的位置,尤其是对在晶界存在许多与O和Ga缺陷有关的悬挂键,这些缺陷倾向于在合并过程中形成较大的晶粒。而且在原子层沉积过程中所采用的Ga/O剂量的条件下,氮气的稳定性也保障了在高温退火条件下不会与沉积的Ga2O3薄膜发生反应生成杂质,进而避免晶体质量的降低,从而使Ga2O3具有较高的光学性能。最后,再采用MOCVD生长β-Ga2O3,是以热处理后的Ga2O3为基底,且已经将亚稳态的Ga2O3转化稳态的,在此基础上,再次生长利于获得高质量的β相Ga2O3。
附图说明
图1为β-Ga2O3工艺制备流程;
图2为沉积后Ga2O3薄膜XPS能谱图;
图3为沉积后Ga2O3薄膜表面AFM图;
图4为1000℃退火处理0.5小时后Ga2O3薄膜表面AFM图;
图5为MOCVD生长的Ga2O3薄膜XRD的θ-2θ扫描曲线;
图6为MOCVD沉积后的Ga2O3薄膜透射谱。
具体实施方式
下面结合附图对本发明的技术方案作更清晰完整的描述,凡是对本发明技术方案进行修改或等同替换,而不脱离本发明技术方案的范围,均应涵盖在本发明的保护范围内。
具体实施步骤包括:
(1)选(0001)面蓝宝石衬底;利用等离子体增强原子层沉积法在蓝宝石生长Ga2O3薄膜,射频等离子体功率为2000W,加热衬底保持到250℃恒定,以氮气为载气;
(2)等离子体增强原子层沉积依次为:①然后通入TMGa源0.1s,TMGa 流量为200sccm;②然后通入氮气5s;③然后通入氧气20s,氧气的流量为200sccm;④然后通入氮气5s;⑤然后将①步到④步周期循环420个周期后进入下一步;
(3)向管式炉中通入氮气,将沉积的Ga2O3薄膜放入LPCVD管式炉中,将管式炉中温度加热至1000℃,热退火0.5小时;
(4)以退火后的薄膜为基底,再进行(MOCVD)生长β-Ga2O3,生长温度550℃,生长时间40min;一般时间范围为35-60min。
图2表明:PEALD沉积的薄膜表面及近表面区域有Ga元素和O元素的存在,且无其他杂质原子的混入。
从图3可以看出:在PEALD沉积后的Ga2O3表面存在一些大晶粒,即图中的白色斑点。
与图3相比,从图4中可发现:由于重结晶过程导致高温退火0.5小时后Ga2O3表面较大晶粒数量减少,晶粒尺寸减小而密集。
由图5可看出:MOCVD沉积后Ga2O3薄膜XRD扫描曲线,显示了在 19.0°,38.9°和59.2°出现较高强度β相Ga2O3(-201)晶系的特征峰,因此表面获得了β-Ga2O3。
图6显示了用本制备方法制得的β-Ga2O3薄膜在紫外及可见光范围内的透射光谱,可以看到:对于350nm到更长波长的入射光,透射率超过80%;而对于波长在300nm以下的光,透射率迅速下降,表明薄膜具有良好的光谱选择性,可用于制备高性能的日盲紫外探测器件。
Claims (1)
1.一种制备β-Ga2O3薄膜的 方法,其特征在于,包括以下步骤:
(1)选c面蓝宝石衬底,等离子体增强原子层沉积Ga2O3薄膜时,设置射频等离子体功率为1800-2000W,沉积温度为240-270℃,以氮气为载气;
(2)等离子体增强原子层沉积时,①先通入TMGa源0.1-0.2s,TMGa流量为190-220sccm;②通入氮气5-10s;③通入氧气15-25s,氧气的流量为190-220sccm;④通入氮气5-10s;⑤将①步到④步依顺序循环重复400-440次;
(3)向LPCVD管式炉中通入氮气,将沉积的Ga2O3薄膜放入炉中,退火时炉中温度为850-1050℃;退火时间为0.5-2小时;
(4)将退火后的薄膜再放到MOCVD系统生长β-Ga2O3,生长温度550-650℃。
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