CN104388898A - 一种MgZnOS四元ZnO合金半导体材料及其制备方法 - Google Patents
一种MgZnOS四元ZnO合金半导体材料及其制备方法 Download PDFInfo
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Abstract
本发明公开一种MgZnOS四元ZnO合金半导体材料及其制备方法，通过Mg与S同时掺杂ZnO，调节MgZnOS中Mg与Zn、O与S的比例形成全新的MgZnOS四元ZnO合金半导体材料，使得该类宽禁带半导体的带隙在更宽范围内(2.94eV～3.95eV)可调，可用于紫外发光器件或光探测器件。本发明MgZnOS单晶材料为世界上首次成功合成，制备MgZnOS四元ZnO合金半导体材料对于开发波长可调的紫外光电器件具有非常重要的意义。此MgZnOS四元ZnO合金半导体材料可采用常规脉冲激光烧蚀沉积、磁控溅射、电子束蒸发等多种方法进行生长，设备和操作工艺简单，易于控制。
Description
技术领域
本发明属于光电半导体材料制备领域，特别涉及一种MgZnOS四元ZnO合金半导体材料及其制备方法。
背景技术
第三代宽禁带半导体ZnO具有约3.3eV的禁带宽度、60meV的激子束缚能，在紫外光发光及光电探测等方面都有非常广泛的用途。为实现器件应用，还需要对ZnO进行掺杂，以调节其能带。如用Mg部分取代Zn得到MgZnO可获得更宽的禁带。MgZnO是由ZnO与MgO按一定组分固溶而成，当Mg含量较低时为六方结构，当Mg含量较高时为立方结构。通过改变Mg的含量可实现MgZnO带隙单调连续可调，带隙范围在3.26eV～3.87eV；MgZnO可作为ZnO基量子阱器件的势垒层材料或紫外光探测器的有源层。除了可以用阳离子替换Zn2+，还能用阴离子替换O2-。如以S部分取代ZnO中的O，得到ZnOS，也可实现对ZnO能带的调节。与Mg掺杂不同，少量S掺杂取代O会抬高ZnO的价带，形成类ZnS的价带顶，减小带隙。在S含量50％左右时，ZnOS的带隙最低约2.6eV。当S的含量进一步增加，ZnOS的带隙也会随之增加，带隙范围在2.6eV～3.71eV。通过将Mg、S共同掺杂ZnO得到MgZnOS四元半导体合金，不仅能够通过调节Mg、S的含量来实现对ZnO带隙在2.94eV～3.95eV范围自由可调，从而调控光电器件的工作波长，还能调节ZnO的价带和导带结构，改善其电子和空穴特性。相比MgZnO和ZnOS等三元半导体，MgZnOS四元合金半导体能带结构具有更高的可调自由度，从而使得其带隙可调范围变宽。制备MgZnOS四元合金半导体对于开发波长可调的紫外光波段光电器件具有非常重要的意义。目前关于MgZnO和ZnOS半导体材料有些报道，但是尚未见到制备MgZnOS四元合金半导体材料的报道。
发明内容
为实现对ZnO能带的多自由度调节，我们发明了一种MgZnOS四元ZnO合金半导体材料的制备方法，所述MgZnOS四元ZnO合金半导体材料的制备方法包括以下步骤：
步骤1，制备生长MgZnOS四元ZnO合金半导体薄膜所需的陶瓷靶材。
按比例称取ZnS和MgO粉末，所述ZnS粉末和MgO粉末的摩尔比例为99:1～75:25；
在称取的上述粉末中加入粉末总质量60％的去离子水进行球磨；
将球磨后的混合粉末进行真空干燥处理，真空度为0.1Pa，温度为110℃，干燥6～8小时；
在干燥后的ZnS与MgO混合粉末中加入粉末总质量2～6％的去离子水，研磨搅拌使两种粉末均匀混合粘结在一起；
将混匀物置于模具中，压制成陶瓷坯片，陶瓷坯片的厚度为2～3mm，直径可调；
将陶瓷坯片放入真空管式炉，并在陶瓷坯片周围放置硫粉，在氮气保护下，在700℃～1250℃高温烧结4～6小时后得到所需陶瓷材料。
步骤2，利用陶瓷靶材、蓝宝石和有机溶剂，采用脉冲激光烧蚀沉积方法制备MgZnOS薄膜。
采用步骤1制备的陶瓷材料作为激光烧蚀靶材，采用蓝宝石作为薄膜生长的衬底；
将衬底经过丙酮、无水乙醇和去离子水中的一种或几种试剂分别超声波清洗15分钟；
将步骤1制备的靶材和上述清洗得到的衬底分别放在靶台和样品台上装入真空室，并开启真空泵抽真空，真空度为10-4Pa以下，调节衬底的生长温度为25～750℃，开启样品台和靶台自转；
通入氧气，调整氧压为0～10Pa，开启激光器，将陶瓷靶材表面原子烧蚀出来沉积在衬底表面形成MgZnOS薄膜，激光能量为250-600mJ/pulse。
同时本发明提供了一种根据所述MgZnOS四元ZnO合金半导体材料的制备方法制得的MgZnOS四元ZnO合金半导体材料，通过将Mg和S共同掺杂到ZnO中得到MgZnOS四元ZnO合金半导体材料。
所述MgZnOS四元ZnO合金半导体材料为薄膜。
通过调节Mg、S的含量来实现对ZnO带隙的调节，从而调控光电器件的工作波长，还能通过调节ZnO的价带和导带结构，改变其电子和空穴特性。
本发明的有益效果为：
1、通过将Mg、S共同掺杂ZnO得到MgZnOS四元ZnO合金半导体材料，不仅能够通过调节Mg、S的含量来实现对ZnO带隙在更宽范围的自由可调，从而调控光电器件的工作波长，同时还能调节ZnO的价带和导带结构，改善其电子和空穴特性。制备的MgZnOS四元ZnO合金半导体材料对于开发波长可调的光电器件具有非常重要的意义。
2、本发明的MgZnOS四元ZnO合金半导体材料可采用常规脉冲激光烧蚀沉积、磁控溅射、电子束蒸发等多种方法进行生长，设备和操作工艺简单，易于控制。
附图说明
图1为本发明方法(实施例1)所制备的MgZnOS薄膜的X射线光电子能谱(XPS)测试图谱；
图2为本发明方法(实施例2)所制备的MgZnOS薄膜的吸收系数平方(α2)与入射光子能量(hν)关系图谱；
图3为本发明方法(实施例3)所制备的MgZnOS薄膜的X射线衍射(XRD)测试图谱。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，下面结合实施例对本发明作进一步详细说明，但所举实例不作为对本发明的限定。
实施例1
按摩尔比ZnS：MgO＝99:1称取ZnS粉末39.8336克和MgO粉末0.1664克混合后加入去离子水24克球磨4小时，之后在110℃真空干燥8小时。干燥后的粉料加入2克去离子水充分研磨搅拌后压片成直径27.5mm、厚度2.5mm的圆形坯片。坯片放入坩埚并放置在真空管式炉中，并在其周围放上成分相同的粉料5.0000克、高纯硫粉0.5000克。将真空管式炉抽真空至0.1Pa后通入高纯氮气。在保护气氛下将管式炉升温至1100℃并保温5小时，随后自然冷却至室温，得到所需陶瓷靶材。以此陶瓷材料作为激光烧蚀靶材，与经过丙酮、无水乙醇和去离子水等分别超声波清洗15分钟的衬底一起装入真空室，并抽真空至10-4Pa。开启衬底加热并调节衬底温度为750℃。不通氧气，使得制备室在整个薄膜沉积过程中维持在高真空状态。开启衬底和靶台自转。设定激光器输出能量为350mJ/pulse，脉冲重复频率为10Hz。开启激光沉积40分钟后关闭氧气与衬底加热。样品在真空中自然冷却至室温后取出真空室。
对该实例制备出的MgZnOS四元ZnO合金半导体材料进行光电子能谱测试，测试结果如图1所示。证实了在以c面蓝宝石为衬底生长的薄膜中确实有Zn、Mg、O、S四种元素存在。
实施例2
按摩尔比ZnS：MgO＝94:6称取ZnS粉末38.9714克和MgO粉末1.0286克混合后，加入去离子水24克球磨4小时，之后在110℃真空干燥7小时。干燥后的粉料加入2克去离子水充分研磨搅拌后压片成直径27.5mm、厚度2mm的圆形坯片。坯片放入坩埚并放置在真空管式炉中，并在其周围放上成分相同的粉料5.000克、高纯硫粉1.1000克。将真空管式炉抽真空至0.1Pa后通入高纯氮气。在保护气氛下将管式炉升温至1250℃并保温4小时，随后自然冷却至室温，得到所需陶瓷靶材。以此陶瓷材料作为激光烧蚀靶材，与经过丙酮、无水乙醇和去离子水等分别超声清洗15分钟的衬底一起装入真空室，并抽真空至10-4Pa。开启衬底加热并调节衬底温度到设定值(25℃,300℃，700℃，750℃)。通入氧气，使得气压在整个薄膜沉积过程中维持在2Pa。开启衬底和靶台自转。设定激光器输出能量为250mJ/pulse，脉冲重复频率为5Hz。开启激光沉积40分钟后关闭与衬底加热。样品在真空中自然冷却至室温后取出真空室。
对于该实例制备的MgZnOS薄膜进行吸收系数平方(α2)与入射光子能量(hν)关系进行测试和图谱分析。从图2中可知，以c面蓝宝石为衬底生长的MgZnOS四元合金半导体材料的带隙值通过调节Mg、S的含量可以在2.94eV～3.95eV范围之间可调。
实施例3
按摩尔比ZnS：MgO＝75:25称取ZnS粉末35.1545克和MgO粉末4.8455克，混合后加入去离子水24克球磨4小时，之后在110℃真空干燥8小时。干燥后的粉料加入2克去离子水充分研磨搅拌后压片成直径27.5mm、厚度3mm的圆形坯片。坯片放入坩埚并放置在真空管式炉中，并在其周围放上成分相同的粉料5.0000克、高纯硫粉2.0000克。将真空管式炉抽真空至0.1Pa后通入高纯氮气。在保护气氛下将管式炉升温至750℃并保温6小时，随后自然冷却至室温，得到所需陶瓷靶材。以此陶瓷材料作为激光烧蚀靶材，与经过丙酮、无水乙醇和去离子水等分别超声波清洗15分钟的衬底一起装入真空室，并抽真空至10-4Pa。开启衬底加热并调节衬底温度为700℃。通入氧气，使得气压在整个薄膜沉积过程中维持在10Pa。开启衬底和靶台自转。设定激光器输出能量为600mJ/pulse，脉冲重复频率为3Hz。开启激光沉积40分钟后关闭氧气与沉底加热。样品在真空中自然冷却至室温后取出真空室。
对该实例制备出的MgZnOS四元ZnO合金半导体材料进行X射线衍射测试，测试结果如图3所示。衍射峰分布证实在以c面蓝宝石为衬底生长的薄膜是单相物质MgZnOS。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种MgZnOS四元ZnO合金半导体材料的制备方法，其特征在于，所述MgZnOS四元ZnO合金半导体材料的制备方法包括如下步骤：
步骤1，制备生长MgZnOS四元ZnO合金半导体薄膜材料所需的陶瓷靶材，
1.1、按比例称取ZnS和MgO粉末，所述ZnS粉末和MgO粉末的摩尔比例为99:1～75:25；
1.2、在称取的上述粉末中加入粉末总质量60％的去离子水进行球磨；
1.3、将球磨后的混合粉末进行真空干燥处理，真空度为0.1Pa，温度为110℃，干燥6～8小时；
1.4、在干燥后的ZnS与MgO混合粉末中加入粉末总质量2～6％的去离子水，研磨搅拌使两种粉末均匀混合粘结在一起；
1.5、将混匀物置于模具中，压制成陶瓷坯片，陶瓷坯片的厚度为2～3mm；
1.6、将陶瓷坯片放入真空管式炉，并在陶瓷坯片周围放置硫粉，在氮气保护下，在700℃～1250℃高温烧结4～6小时后得到所需陶瓷材料；
步骤2，利用陶瓷靶材、蓝宝石和有机溶剂，采用脉冲激光烧蚀沉积方法制备MgZnOS薄膜，
2.1、采用步骤1制备的陶瓷材料作为激光烧蚀靶材，采用蓝宝石作为薄膜生长的衬底；
2.2、将衬底经过丙酮、无水乙醇和去离子水中的一种或几种试剂超声波清洗15min；
2.3、将步骤1制备的靶材和步骤2.2清洗得到的衬底分别放在靶台和样品台上装入真空室，并开启真空泵抽真空，真空度为10-4Pa以下，调节衬底的生长温度为0～750℃，开启样品台和靶台自转；
2.4、通入氧气，调整氧压为0～10Pa，开启激光器，将陶瓷靶材表面原子激光烧蚀出来沉积在衬底表面形成MgZnOS薄膜，激光能量为250-600mJ/pulse。
2.根据权利要求1所述制备方法制得的MgZnOS四元ZnO合金半导体材料，其特征在于，通过将Mg和S共同掺杂到ZnO中得到MgZnOS四元ZnO合金半导体材料。
3.根据权利要求2所述的MgZnOS四元ZnO合金半导体材料，其特征在于，所述MgZnOS四元ZnO合金半导体材料为薄膜。
4.根据权利要求2所述的MgZnOS四元ZnO合金半导体材料，其特征在于，通过调节Mg、S的含量来实现对ZnO带隙的调节，从而调控光电器件的工作波长，还能通过调节ZnO的价带和导带结构，改变其电子和空穴特性。
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| CN109880617A (zh) * | 2019-03-18 | 2019-06-14 | 深圳大学 | 光色和光强可调的双相应力发光材料 |
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