CN109440075B - 一种提高离子注入GaN基稀磁半导体材料室温铁磁性的热退火方法 - Google Patents
一种提高离子注入GaN基稀磁半导体材料室温铁磁性的热退火方法 Download PDFInfo
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Abstract
本发明为一种提高离子注入GaN基稀磁半导体材料室温铁磁性的热退火方法。该方法首先将非磁性离子注入到GaN基底中，对该样品进行快速热退火处理，然后将磁性金属注入到经过退火处理的离子注入GaN基底中，对双离子注入的GaN样品进行第二次快速热退火处理，两次热退火处理都通入了相同的保护气体，升温速率和保温时间根据离子注入的离子种类进行设定。该方法有利于最大程度的激活注入离子活性，消除GaN基稀磁半导体材料中的离子注入损伤，增加自旋电子与载流子之间的交互作用，从而提高了GaN基稀磁半导体材料的室温铁磁性。
Description
技术领域
本发明涉及一种利用两步热退火工艺恢复GaN基稀磁半导体离子注入损伤及提高稀磁半导体室温铁磁性的方法。
背景技术
当代和未来都是信息主宰的社会，而支持信息技术存在和发展的两大决定性因素分别是信息的存储和信息的处理。信息的存储是利用了磁性材料中电子的自旋属性，而信息的存储则依靠半导体芯片中电子的电荷属性得以实现。稀磁半导体是将磁性过渡族金属离子或稀土离子部分代替半导体中的非磁性阳离子之后而形成的半导体材料，其具有电子和电荷的双重属性，是制备高效、低功耗的自旋电子器件的重要材料之一。
要制备具有实用化的电子自旋器件，稀磁材料的居里温度高于室温是一个必要条件，最近的理论和实验研究表面过渡族金属和稀土元素掺杂的GaN基材料最有希望获得室温以上的铁磁性。另外，低掺杂浓度高铁磁性是稀磁半导体材料应用的另一必要条件。离子注入过程是一个将不同磁性离子引入GaN基材料中的简便方法，不受生长条件的限制，且离子注入可以有效的引入杂质和缺陷，已有研究表明杂质和缺陷的存在可以有效的提高GaN基稀磁半导体的铁磁性。但是直接将磁性离子注入到GaN基材料中，并不能够获得较高的室温铁磁性，离子注入引入的大量的注入损伤，降低了自旋电子与载流子之间的相互作用。目前，离子注入后的GaN基稀磁半导体材料都要经过热退火处理，一般采用的退火方法是一步快速热退火，即直接将温度升高到设定温度，保温一段时间，然后进行降温处理。目前的研究表明采用磁性金属和非磁性离子共同注入可以有效提高GaN基稀磁半导体材料的室温铁磁性，但是磁性金属和非磁性离子在GaN晶格中的扩散温度不同，因此一步热退火处理技术并不能够完全激活注入离子，直接限制了GaN基稀磁半导体材料室温铁磁性的进一步提高。
发明内容
本发明的目的为针对如何进一步提高离子注入GaN基稀磁半导体材料的室温铁磁性的问题，提供一种用于磁性金属和非磁性离子共同注入GaN基稀磁半导体材料的热退火处理方法。该方法为磁性金属和非磁性离子共同注入的GaN基稀磁半导体材料的制备采用两次离子注入的方法，根据磁性金属和非磁性原子的注入能量和剂量均不同，首先将非磁性离子注入到GaN基底中，对该样品进行快速热退火处理，然后将磁性金属注入到经过退火处理的离子注入GaN基底中，对双离子注入的GaN样品进行第二次快速热退火处理，两次热退火处理都通入了相同的保护气体，升温速率和保温时间根据离子注入的离子种类进行设定。该方法有利于最大程度的激活注入离子活性，消除GaN基稀磁半导体材料中的离子注入损伤，增加自旋电子与载流子之间的交互作用，从而提高了GaN基稀磁半导体材料的室温铁磁性。
本发明的技术方案为：
一种提高离子注入GaN基稀磁半导体材料室温铁磁性的热退火方法，包括如下步骤：
第一步，采用金属有机物气相外延方法(MOCVD)在蓝宝石衬底上生长GaN薄膜材料；GaN薄膜材料的厚度为2-4μm；
第二步，对生长的GaN薄膜进行第一次离子注入：
对GaN基底进行非磁性离子注入，非注入能量在50KeV-100KeV,注入剂量为1x1014/cm-2～1x1015/cm-2；然后进行第一次退火，退火温度设为500℃～700℃，退火保温时间设为30分钟～60分钟，得到非磁性离子掺杂的GaN薄膜材料；
第三步，对上一步得到的薄膜材料进行第二次磁性金属离子注入，磁性金属离子为稀土金属离子，磁性金属离子的注入能量为200KeV-400KeV，注入剂量为1x1015/cm-2～1x1017/cm-2；磁性离子注入后，对样品进行第二次快速热退火，热退火温度为700℃～1000℃，退火温度为30秒～5分钟；
最后，得到非磁性离子和磁性离子共同掺杂的GaN基稀磁半导体材料。
所述的非金属离子具体为C或O；
所述的稀土金属离子具体为Gd,Dy,Sm或Er。
所述的第一退火或第二次退火时，温度从室温升到设定温度，升温速率为75℃/秒-150℃/秒；保温结束后温度从设定温度降温到室温，降温速率为200℃/分钟。
本发明的实质性特点为：
本发明经过大量的研究和实验，开创性的将当前技术中使用的一次退火改为了两次退火；首先对GaN基底进行非磁性离子注入，非磁性离子一般为C和O等，由于C和O的质量较轻，为了使两种离子在GaN基底中的分布重合，在第一次注入中非磁性离子注入较低的能量，注入能量在50KeV-100KeV；然后，对第一次非磁性离子注入并退火后的样品进行第二次磁性金属离子注入，由于磁性金属离子为稀土金属离子，稀土金属质量较重，磁性金属离子的注入能量为200KeV-400KeV。而在退火时，第一次非磁性离子注入后，由于非磁性离子的原子半径较小，离子注入进入GaN基底后可以处于GaN晶格的间隙位置或取代GaN晶格的N原子，根据注入离子在GaN基底中的扩散温度，退火温度设为500℃～700℃；第二次磁性离子注入后，对样品进行第二次快速热退火处理，磁性金属离子为稀土金属离子，稀土金属离子半径较大，离子注入后在GaN晶格中一般取代Ga的位置，需要经过热退火激活，热退火温度为700℃～1000℃。
本发明的有益效果为
本发明可以最大程度的激活非磁性离子和稀土离子，使其占据GaN晶格的位置，修复离子注入在GaN晶格中引入的注入损伤。热退火过程中非磁性离子一般取代GaN晶格中N的位置，而稀土离子取代GaN晶格中Ga的位置，因此非磁性离子与磁性稀土离子的交互作用增强，提高了双离子共注GaN基稀磁半导体的室温铁磁性，增长率可达30％。
附图说明
图1是本发明提供的采用磁性金属和非磁性金属共同离子注入GaN基稀磁半导体材料的热退火方法流程图；
图2是依照本发明实施例制备的GaN:Dy+C稀磁半导体材料在室温下的M-H曲线图。
具体实施方案
下面具体以非磁性C离子和稀土Dy离子共同注入GaN基稀磁半导体材料的热退火为例来详细说明其处理过程。
实施例1
第一步，准备用于离子注入的GaN薄膜材料。GaN基底材料是在蓝宝石衬底(0001)面上采用金属有机物外延生长技术(MOCVD)外延生长的GaN薄膜，GaN薄膜的厚度为3μm，GaN薄膜材料为非故意掺杂的n型GaN。
第二步，对GaN薄膜材料进行第一次离子注入。离子注入前先对GaN薄膜材料用丙酮和酒精反复清洗，以防在离子注入过程中GaN表面的杂质进入GaN晶格。采用离子注入机(中国电子科技集团公司第四十八研究所研制的LC-4型离子注入机)对GaN薄膜进行离子注入，离子注入过程在室温下进行，注入的离子为非金属C离子，离子注入角度与GaN表面呈7°角，以防在晶格中形成沟道效应，C离子的注入能量为150KeV，注入剂量为1x1014/cm2。
第三步，对非金属C离子注入的GaN薄膜材料进行第一次快速热退火处理。热退火处理在快速热退火炉中进行，退火过程中采用氮气作为保护气体，退火过程中将离子注入的GaN样品表面用未注入的GaN样品覆盖，退火温度为600℃，升温速率为100℃/秒，在600℃时保温30min，再自然冷却到室温。
第四步，对非金属C离子注入的样品进行第二次离子注入。注入的离子为稀土Dy离子，离子注入角度与GaN表面呈7°角，以防在GaN晶格中形成沟道效应，离子注入能量为300KeV，注入剂量为7x1014/cm3
第五步，对稀土Dy离子和非金属C离子注入的GaN样品进行第二次快速热退火处理。热退火处理在相同的快速热退火炉中进行，退火过程中采用氮气作为保护气体，退火过程中将离子注入的GaN样品表面用未注入的GaN样品覆盖，退火温度为800℃，升温速率为150℃/秒，在800℃时保温3min，再自然冷却到室温。(说明：第二次热退火处理过程温度较高，为了有效抑制GaN晶格中N原子的挥发，热退火保温时间设置为不大于5min。)
第六步，对两次热退火后的离子共注GaN样品进行室温铁磁性测量。测试设备采用综合物性测试系统(PPMS)，磁性测量结果与一次热退火的C和Dy共注GaN样品的磁性进行比较，图2显示了两种方法制备样品的磁化强度随磁场强度的变化曲线，发现两种方法制备的样品都具有室温铁磁性，但是两次热退火后的C和Dy离子共注GaN样品比仅一次热退火的GaN基稀磁样品的饱和磁化强度增加了约5emu,增加幅度约为一次热退火样品饱和磁化强度的30％。
实施例2
其它步骤同实施例1，不同之处为注入的磁性金属离子由稀土离子Dy改为稀土离子Gd。得到的样品的饱和磁化强度的增加百分比与实施例1近似。
以上实施例是对本发明的举例，依照本发明的原理，对于其它磁性金属离子和非磁性离子共同注入的GaN基稀磁半导体材料都可以采用该退火过程处理，不同材料对应的退火过程略有不同，表现出高室温铁磁性的退火温度也不同，但都包括在该发明之内。
本发明未尽事宜为公知技术。
Claims (1)
1.一种提高离子注入GaN基稀磁半导体材料室温铁磁性的热退火方法，其特征为该方法包括如下步骤：
第一步，采用金属有机物气相外延方法（MOCVD）在蓝宝石衬底上生长GaN薄膜材料；GaN薄膜材料的厚度为2-4μm；
第二步，对生长的GaN薄膜进行第一次离子注入：
对GaN基底进行非磁性离子注入，非磁性离子注入能量在50KeV-100KeV,注入剂量为1ｘ1014/cm2 ~1ｘ1015/cm2 ；然后进行第一次退火，退火温度设为500oC~700℃，退火保温时间设为30分钟~60分钟，得到非磁性离子掺杂的GaN薄膜材料；注入设备为LC-4型离子注入机；
第三步，对上一步得到的薄膜材料进行第二次磁性金属离子注入，磁性金属离子为稀土金属离子，磁性金属离子的注入能量为200KeV-400KeV，注入剂量为1ｘ1015/cm2 ~1ｘ1017/cm2 ；磁性离子注入后，对样品进行第二次快速热退火，热退火温度为700oC~1000℃，退火时间为30秒~3分钟；所述的退火在快速热退火炉进行；
最后，得到非磁性离子和磁性离子共同掺杂的GaN基稀磁半导体材料；
所述的非磁性离子具体为C；
所述的稀土金属离子具体为Gd,Dy,Sm或Er；
所述的第一次退火或第二次退火时，温度从室温升到设定温度，升温速率为75℃/秒-150℃/秒；保温结束后温度从设定温度降温到室温，降温速率为200℃/分钟。
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