Name: plasma-assisted molecular beam epitaxy growth of mg3n2 and zn3n2 thin films
Uploaded: 2019-05-11T13:00:00
Description: Watch this Scientific Journal Video about Plasma-Assisted Molecular Beam Epitaxy Growth of Mg3N2 and Zn3N2 Thin Films at JoVE.com

这项工作得到了加拿大自然科学和工程研究理事会的支持。

1. MgO基板制备
注:用于X3N 2(X = Zn和Mg)薄膜生长的商用单面上抛光(100)定向单晶MgO方形基板(1厘米x1厘米)。
<ol><li>高温退火<ol>
<li>将 MgO 放在干净的蓝宝石晶圆样品载体上,抛光面朝上,在 1,000 °C 下,退火 9 小时。在 10 分钟内将温度升高到 1000 °C。 注:高温退火可去除表面的碳,并重建MgO单晶基板的表面晶体结构。</li>
		<li>将 MgO 基板冷却至室温 (RT)。</li>
	...

<ol>
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在选择基材和建立优化薄膜结构和电子特性的生长条件时,需要考虑各种因素。MgO基板在高温下(1000°C)加热,去除表面的碳污染,改善基材表面的结晶顺序。丙酮的超声波清洗是清洁MgO基板的好方法。
当薄膜在高温退火MgO基板上生长时,Zn3N2薄膜的(400)X射线衍射峰值比在未发火基板上生长时更窄。MgO (0.421 nm) 的晶格常数明显小于 Zn3N2 (0.976 nm) 或 Mg<su...

II3-V2材料是一类半导体,与III-V和II-VI半导体1相比,受到半导体研究界的关注相对较少。Mg 和 Zn nititd、Mg3N2和 Zn3N2对消费者应用很有吸引力,因为它们由丰富且无毒的元素组成,与大多数 III-V 和 II-VI 不同,它们价格低廉且易于回收化合物半导体。它们显示了一种与CaF2结构相似的抗双比石晶体结构,其中一个穿插的fccF-sublattices是半占用的2,3,4,5。它们都是直接带隙材料6,使它们适用于光学应用7,8,9。Mg3N2的波段间隙在可见光谱 (2.5 eV)10中,Zn3N2的频段间隙在近红外 (1.25 eV)11中。要探索这些材料的物理特性及其在电子和光学器件应用方面的潜力,获得高质量的单晶膜至关重要。迄今为止,对这些材料的大部分工作都是在反应溅射12、13、14、15、16的粉末或多晶薄膜上进行的。 17.
分子束外延 (MBE) 是一种开发成熟且用途广泛的方法,用于种植单晶化合物半导体薄膜18,具有利用清洁环境和高纯度元素源生产高质量材料的潜力。同时,MBE 快速快门操作可在原子层比例下对胶片进行更改,并允许精确厚度控制。本文以高纯度锌和Mg作为蒸汽源,N2气体作为氮源,报道了等离子体辅助MBE在MgO基板上Mg3 N2和Zn3N2外延膜的生长情况。

<table border="0" cellpadding="0" cellspacing="0" style="width:743px;" width="742">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">(100) MgO</td>
			<td style="width:123px;">University Wafer</td>
			<td style="width:123px;">214018</td>
			<td style="width:276px;">one side epi-polished</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Acetone</td>
			<td style="width:123px;">Fisher Chemical&#160;</td>
			<td style="width:123px;">170239</td>
			<td style="width:276px;">99.8%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Argon laser</td>
			<td style="width:123px;">Lexel Laser</td>
			<td style="width:123px;">00-137-124</td>
			<td>488 nm visible wavelength, 350 mW output power</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:222px;">Chopper&#160;</td>
			<td style="width:123px;">Stanford Research system&#160;</td>
			<td style="width:123px;">SR540</td>
			<td style="width:276px;">&#160;Max. Frequency: 3.7 kHz&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:222px;">Lock-in amplifier&#160;</td>
			<td style="width:123px;">Stanford Research system&#160;</td>
			<td style="width:123px;">37909</td>
			<td style="width:276px;">DSP SR810, Max. Frequency: 100 kHz&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Magnesium&#160;</td>
			<td style="width:123px;">UMC</td>
			<td style="width:123px;">MG6P5</td>
			<td style="width:276px;">99.9999%</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:222px;">MBE system</td>
			<td style="width:123px;">VG Semicon</td>
			<td style="width:123px;">V80H0016-2 SHT 1</td>
			<td style="width:276px;">V80H-10</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Methanol&#160;</td>
			<td style="width:123px;">Alfa Aesar</td>
			<td style="width:123px;">L30U027</td>
			<td style="width:276px;">Semi-grade 99.9%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Nitrogen</td>
			<td style="width:123px;">Praxair</td>
			<td style="width:123px;">402219501</td>
			<td style="width:276px;">99.998%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Oxygen&#160;</td>
			<td style="width:123px;">Linde Gas</td>
			<td style="width:123px;">200-14-00067</td>
			<td style="width:276px;">&#62; 99.9999%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Plasma source</td>
			<td style="width:123px;">SVT Associates</td>
			<td style="width:123px;">SVTA-RF-4.5PBN</td>
			<td>PBN, 0.11&#34; Aperture, Specify Length: 12&#34; &#8211; 20&#34;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:222px;">Si photodiode&#160;</td>
			<td style="width:123px;">Newport</td>
			<td style="width:123px;">2718</td>
			<td style="width:276px;">818-UV Enhanced, 200 - 1100 nm</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:222px;">Zinc&#160;</td>
			<td style="width:123px;">Alfa Aesar</td>
			<td style="width:123px;">7440-66-6</td>
			<td style="width:276px;">99.9999%</td>
		</tr>
	</tbody>
</table>

plasma-assisted molecular beam epitaxy growth of mg3n2 and zn3n2 thin films

本文介绍了通过等离子辅助分子束外延(MBE)生长Mg3N2和Zn3N2薄膜的过程。薄膜生长在100个定向MgO基板上,以N2气体为氮源。介绍了基板制备方法和MBE生长过程。基材和薄膜表面的方向和晶体顺序在生长前和生长过程中通过反射高能电子衍射(RHEED)进行监测。样品表面的镜面反射率在生长过程中使用波长为488nm的Ar-ion激光器进行测量。通过将反射率的时间依赖性与数学模型拟合,确定了薄膜的折射率、光消光系数和生长速率。使用石英晶体监测仪作为熔融细胞温度的函数独立测量金属助焊剂。Mg3N2和 Zn3N2薄膜的生长温度分别为 0.028 nm/s,生长温度为 330°C 和 330°C。

图 5B中所处的黑色对象是一张已生长的 200 nm Zn3N2薄膜的照片。同样,图 5C中 INSET 中的黄色对象是生长的 220 nm Mg3N2薄膜。黄色胶片是透明的,因为它很容易阅读的文本放在电影10后面。
RHEED对基板和薄膜的表面进行了原位监测。...

Watch this Scientific Journal Video about Plasma-Assisted Molecular Beam Epitaxy Growth of Mg3N2 and Zn3N2 Thin Films at JoVE.com

Plasma-Assisted Molecular Beam Epitaxy Growth of Mg3N2 and Zn3N2 Thin Films

本文介绍了以N2气体为氮源和光生长监测的等离子体辅助分子束外延在MgO基板上Mg3 N2和Zn3N2的外延膜的生长情况。

Mg3N2和 Zn3N2薄膜的等离子辅助分子束外延生长

This article describes a procedure for growing Mg3N2 and Zn3N2 films by plasma-assisted molecular beam epitaxy (MBE). The films are grown on 100 oriented ...

在这段视频中，我们展示如何通过等离子体辅助分子束外延（或短期 MBE）来种植亚硝酸镁和亚硝酸锌的外延膜。亚硝酸镁和亚硝酸锌是II-V复合半导体材料。这是一个相对未开发的半导体类。它们具有抗双比石晶体结构，在传统的立方体单元细胞中有80个原子。薄膜生长在VG V80 MBE系统中。左侧的水平室是制备室，右侧的圆形室是发生薄膜生长的生长室。样品入口锁，位于制备室的左侧。我们找到的用于生长亚硝酸镁和亚硝酸锌的最佳基质是100为导向的单晶氧化镁。一厘米方形基板首先放置在蓝宝石晶圆样品载体上，抛光侧向上，在1000摄氏度下退火9小时。 高温退火从表面去除碳，重建氧化镁单晶基板的表面晶体结构。退火后，样品在去维水中冲洗，在丙酮中煮30分钟，以去除处理过程中的任何有机碳污染，然后再次用甲醇冲洗并用氮气吹干。MBE 增长的第一步是打开融合细胞的冷却水以及生长室中的低温罩。然后打开生长监测激光器、RHEED电源、RF等离子发生器电源和石英晶体微平衡系统。氧化镁基板安装在三英寸直径的硅质样品架上，带钨弹簧夹。将样品装入 MBE 的第一步是关闭涡轮泵并排放快速入口锁。样品架盒从快速进入锁中取出，新样品加载到盒式磁带中，盒式磁带放回快速进入锁中。涡轮泵用于疏散快速进入锁。因此，我们通常将基板在100摄氏度的快速进入锁中去气30分钟。然后，将其转移到制备室，在400摄氏度下去气5小时。脱气样品架通过推车机构转移到生长室中，并装入样品操纵器。样品在750摄氏度的机械器中气体化30分钟。确保低温罩中的冷却水已打开，以避免过热。在亚硝酸镁生长的情况下，基底的温度将降低至330度。生长室压力现在应低于10至负8托尔。反射高能电子衍射枪（即短期 RHEED）上的电压缓慢增加到 15 千伏，灯丝加热器电流设置为 1 微安。基板支架被旋转，直到电子衍射模式显示与基板的原理晶体图形轴对齐，并且可以看到清晰的单晶电子衍射模式。标准组三型扩散细胞或低温扩散细胞用于镁和锌。熔炉分别装有15克和25克高纯度镁和锌。锌和镁源融合细胞在250度下被气体化一小时，其百叶窗关闭。通常，在将基板装入操纵器之前，可以完成此操作。装入基板后，将锌聚变电池加热至350摄氏度，将镁电池加热至390摄氏度。可伸缩石英晶体监视器位于腔内基板的前面。确保基板完全被探测器覆盖，以便基材上不会沉积任何金属。将金属的密度输入石英晶体监测控制器，使控制器可以读取石英晶体传感器上沉积金属的厚度。为了校准助焊剂，我们打开其中一个金属源上的快门，让其中一个输液单元中的金属通量沉积在传感器上。当金属在传感器上积聚时，控制器测量的厚度将随着时间而线性增加。通过将一条直线与厚度作为时间函数，我们可以获得金属通量的精确测量。一旦磁通量测量完成，关闭输液单元上的百叶窗，然后从样品架前部收回石英晶体监测器。此图显示了使用石英晶体监视器测量金属源的通量的温度依赖性。直线固定在阿雷纽斯关系上。在源温度每升高 12 度时，通量大约增加一倍。关闭 RHEED 喷枪上的灯丝电流和高压，以防止在生长室中存在高氮气压力的情况下损坏灯丝。下一步是启动氮气等离子体源。在高压气瓶上打开一个气体阀，然后慢慢打开泄漏阀，直到生长室中的氮气压力达到三到四倍，10到负五托尔。然后将 13.56 MHz RF 电源的功率设置为 300 瓦。等离子体以等离子源上的点火器启动。当等离子体启动时，从等离子源背面的视图端口可以看到明亮的紫色光。调整射频匹配盒上的控制，尽可能减小反射功率。反射功率小于 15 瓦是好的。将从生长室基板反射的切碎的 488 纳米波长 argon 激光聚焦到硅胶光电二极管上，以便锁定放大器可以检测到电信号。通过调整基板的角度，通过旋转基板支架围绕两个轴，并调整硅胶探测器的位置和对焦镜头，收集反射光，如图所示，实现。激光线滤波器用于阻挡除来自 argon 激光的 488 纳米光之外的所有光线。光电二极管输出用锁定放大器测量，该单与基板表面的反射率成正比。打开其中一个金属源的快门。使用计算机控制的数据记录器记录时间相关反射率。外延膜的生长会产生与薄膜前表面和后表面之间的薄膜光学干扰相关的振荡反射信号。当亚硝酸镁薄膜首次从 MBE 中取出来时，它们是黄色的，但会很快褪色成白色。为了保护薄膜免受氧化和空气的腐蚀，建议在将薄膜从生长室中带出之前，先将氧化镁的封装层沉积在顶部，以保护薄膜在暴露于空气中时免受氧化。这对亚硝酸镁尤其重要，对亚硝酸锌来说也不太重要。为了沉积氧化镁封装层，关闭氮气并切换到氧气，将氧气压力增加至10至负5托尔。在封盖层的增长过程中，我们将射频功率降低至 250 瓦。等离子体的射频功率比氮气低。氧气等离子体运行后，打开镁源上的快门，监控时间取决于反射率 10 分钟。这将产生一个约10纳米厚的氧化镁薄膜。可以在此方程中对样品的光学反射率进行建模。n2是488纳米氧化镁基板的折射率，等于1.75。无用是事件测量的角度与基板法线。在成长过程中，t 是时间。薄膜的光学常数，n1和k1，以及通过将反射率与方程拟合为时间函数，获得增长率。黄色方块是亚硝酸镁薄膜的一个例子，黑色方块是亚硝酸锌膜。亚硝酸镁是黄色的，因为它有一个带隙在可见，而锌亚硝酸盐是黑色，因为它的带隙是红外线。左侧的图片是裸氧化镁基板的 RHEED 电子衍射模式，电子束与 110 方向平行。中间图片是亚硝酸锌膜的衍射图案，右边的图片来自亚硝酸镁膜。这些结果表明，沉积膜的晶体结构是面向基材平面的，正如我们对外延膜所期望的那样。这显示了在样品操纵器中旋转裸氧化镁基板时电子衍射模式发生的情况。此图显示了亚硝酸锌和亚硝酸镁薄膜生长过程中光反射率作为时间函数。通过将反射率作为时间函数拟合到光学模型中，可以提取胶片的折射率、n、消光系数、k和生长速率 g 的指数。由于表面粗糙度散射，在亚硝酸镁薄膜的情况下，反射率会随着时间而下降，我们用阻尼指数对它进行数学建模。在这段视频中，我们展示了如何通过等离子辅助分子束外延来种植外延镁和亚硝酸锌薄膜。我们的一个结果是，在样品生长时测量样品的光学反射率是确定薄膜的生长速率和光学常数的一个好方法。不幸的是，我们的材料没有显示光致发光，无论是室温或低温，所以有必要进一步改善薄膜质量。在我们的实验室中对粉末样品进行的实验为如何这样做提供了线索。在高温下，由锌与氨反应产生的亚硝酸锌粉确实表现出强烈的光致发光性。这表明，使用氨代替氮气作为氮气源可能是制造具有改进电子性能的材料的一种方式。

Research

JoVE Journal

Engineering

Plasma-Assisted Molecular Beam Epitaxy Growth of Mg3N2 and Zn3N2 Thin Films

Molecular Beam Mass Spectrometry With Tunable Vacuum Ultraviolet (VUV) Synchrotron Radiation

Molecular Beam Mass Spectrometry With Tunable Vacuum Ultraviolet VUV Synchrotron Radiation

可调式真空紫外（VUV）同步辐射分子束质谱分析

Tunable soft ionization coupled to mass spectroscopy is a powerful method to investigate isolated molecules, complexes and clusters and their spectroscopy ...

科研

工程学

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

环境钚的薄膜弥散形态和生物利用度测量

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

Plasma-assisted Molecular Beam Epitaxy of N-polar InAlN-barrier High-electron-mobility Transistors

N极性InAlN阻高电子迁移率晶体管的等离子体辅助分子束外延

Plasma-assisted molecular beam epitaxy is well suited for the epitaxial growth of III-nitride thin films and heterostructures with smooth, abrupt ...

In Situ Monitoring of the Accelerated Performance Degradation of Solar Cells and Modules: A Case Study for Cu(In,Ga)Se2 Solar Cells

In Situ Monitoring of the Accelerated Performance Degradation of Solar Cells and Modules: A Case Study for CuIn,GaSe2 Solar Cells

就地太阳能电池和模块加速性能退化的监测: 铜 (in, Ga) Se2太阳能电池的实例研究

The levelized cost of electricity (LCOE) of photovoltaic (PV) systems is determined by, among other factors, the PV module reliability. Better prediction ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

基于 LiPON 的固态锂离子 Nanobatteries 的聚焦离子束制备方法在原位测试中的研究

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

用斜角沉积法制备高吸收介质的超薄彩色薄膜

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present ...

Film Control to Study Contributions of Waves to Droplet Impact Dynamics on Thin Flowing Liquid Films

薄膜控制研究波浪对液滴冲击动力学的影响薄流动液体薄膜

Droplet impact is a very common phenomenon in nature and attracts attention due to its aesthetic fascination and wide-ranging applications. Previous ...

Fabrication of Schottky Diodes on Zn-polar BeMgZnO/ZnO Heterostructure Grown by Plasma-assisted Molecular Beam Epitaxy

等离子体辅助分子束外延法制备的锌极性 BeMgZnO/氧化锌异质结构肖特基二极管的制备

Heterostructure field effect transistors (HFETs) utilizing a two dimensional electron gas (2DEG) channel have a great potential for high speed device ...

Demonstration of Equal-Intensity Beam Generation by Dielectric Metasurfaces

电介质元表面的等强度光束生成演示

The fabrication and characterization protocol for a metasurface beam splitter, enabling equal-intensity beam generation, is demonstrated. Hydrogenated ...

Procedure for the Transfer of Polymer Films Onto Porous Substrates with Minimized Defects

聚合物薄膜在多孔基板上的转移程序,具有最小化的缺陷

The fabrication of devices containing thin film composite membranes necessitates the transfer of these films onto the surfaces of arbitrary support ...