CN110195217A - 一种制备β-Ga2O3薄膜方法 - Google Patents

一种制备β-Ga2O3薄膜方法 Download PDF

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CN110195217A
CN110195217A CN201910559237.6A CN201910559237A CN110195217A CN 110195217 A CN110195217 A CN 110195217A CN 201910559237 A CN201910559237 A CN 201910559237A CN 110195217 A CN110195217 A CN 110195217A
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邢艳辉
张尧
韩军
曹旭
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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

一种制备β-Ga2O3薄膜方法
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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CN110854233A (zh) * 2019-11-17 2020-02-28 金华紫芯科技有限公司 一种Ga2O3薄膜基日盲紫外探测器、制备方法及应用
CN110911270A (zh) * 2019-12-11 2020-03-24 吉林大学 一种高质量氧化镓薄膜及其同质外延生长方法
CN110993504A (zh) * 2019-10-14 2020-04-10 西安电子科技大学 基于SiC衬底的Ga2O3薄膜的制备方法及基于SiC衬底的Ga2O3薄膜
CN111524995A (zh) * 2020-04-21 2020-08-11 昌吉学院 β-Ga2O3/GaN异质结日盲/可见盲双色紫外探测器及其制备方法
CN112647130A (zh) * 2020-11-20 2021-04-13 山东大学 一种低压化学气相沉积生长氧化镓薄膜的方法
CN112877674A (zh) * 2021-01-11 2021-06-01 复旦大学 一种含量可精确调控的Sn掺杂氧化镓膜材料的生长方法
CN113066902A (zh) * 2021-03-25 2021-07-02 北京邮电大学 一种通过氧空位浓度调控ε相氧化镓光电响应性能的方法
CN113517172A (zh) * 2021-06-07 2021-10-19 西安电子科技大学 一种β-Ga2O3薄膜及其制备方法
CN113643960A (zh) * 2021-06-07 2021-11-12 西安电子科技大学 一种基于脉冲法的β-Ga2O3薄膜及其制备方法

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CN110911270A (zh) * 2019-12-11 2020-03-24 吉林大学 一种高质量氧化镓薄膜及其同质外延生长方法
CN110911270B (zh) * 2019-12-11 2022-03-25 吉林大学 一种高质量氧化镓薄膜及其同质外延生长方法
CN111524995B (zh) * 2020-04-21 2022-02-15 昌吉学院 β-Ga2O3/GaN异质结日盲/可见盲双色紫外探测器及其制备方法
CN111524995A (zh) * 2020-04-21 2020-08-11 昌吉学院 β-Ga2O3/GaN异质结日盲/可见盲双色紫外探测器及其制备方法
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CN113643960A (zh) * 2021-06-07 2021-11-12 西安电子科技大学 一种基于脉冲法的β-Ga2O3薄膜及其制备方法
CN113517172A (zh) * 2021-06-07 2021-10-19 西安电子科技大学 一种β-Ga2O3薄膜及其制备方法
CN113517172B (zh) * 2021-06-07 2023-02-10 西安电子科技大学 一种β-Ga2O3薄膜及其制备方法
CN113643960B (zh) * 2021-06-07 2024-03-19 西安电子科技大学 一种基于脉冲法的β-Ga2O3薄膜及其制备方法

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