WO2022148223A1 - 一种利用rheed原位实时定量探测薄膜粗糙度的方法 - Google Patents

一种利用rheed原位实时定量探测薄膜粗糙度的方法 Download PDF

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WO2022148223A1
WO2022148223A1 PCT/CN2021/138645 CN2021138645W WO2022148223A1 WO 2022148223 A1 WO2022148223 A1 WO 2022148223A1 CN 2021138645 W CN2021138645 W CN 2021138645W WO 2022148223 A1 WO2022148223 A1 WO 2022148223A1
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film
roughness
rheed
diffraction pattern
situ
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翟晓芳
梁根豪
成龙
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上海科技大学
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/30—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces
    • G01B11/306—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces for measuring evenness
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/10—Measuring as part of the manufacturing process
    • H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions

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  • the invention relates to the field of condensed matter structure detection, in particular to a method for in-situ real-time detection of the surface roughness of a thin film.
  • Thin film surface roughness has always been a very fundamental and important piece of information in the study of surface and interface physics in condensed matter physics.
  • a buffer layer is grown on the surface of a single crystal SrTiO 3 (001) substrate, and whether the buffer layer is flat or not is directly related to the quality of the subsequent thin films; the interface, such as the two-dimensional electron gas at the LaAlO 3 /SrTiO 3 interface, is very important for the growth of the two materials.
  • the interface flatness is required to be very high, so the roughness of the film surface is directly related to the quality of the epitaxial film.
  • the flatness of the interface has a crucial impact on the performance of the device, such as magnetic tunnel junctions, ferroelectric tunnel junctions, and quantum cascade lasers.
  • sample preparation is generally done in vacuum.
  • reflection high-energy electron diffractometer (hereinafter referred to as RHEED) is a widely used in-situ characterization method. But at present, most of them are only used to qualitatively observe the growth situation, such as the growth mode, the number of growth layers and so on.
  • the detection methods of film surface roughness such as atomic force microscope, ellipsometer and other instruments, need to take the sample out of the vacuum equipment and then test it, and the main method of measuring the interface, such as transmission electron microscope, also needs to remove the sample from the vacuum equipment. Even further processing of the sample is required.
  • many thin films are not stable in the air.
  • the purpose of the present invention is to provide a method for in-situ and real-time detection of surface and interface roughness based on RHEED.
  • the technical solution of the present invention is to provide a method for quantitatively detecting film roughness in situ by using RHEED, which is characterized in that it is used to obtain the surface roughness of the epitaxial film in situ and quantitatively, including The following steps:
  • the surface roughness of the film is obtained by the functional relationship between the shape parameter A of the diffraction pattern and the surface roughness.
  • the epitaxial film is irradiated with a RHEED electron beam during the process of epitaxial growth of the film on the single crystal substrate or after the epitaxial growth of the film on the single crystal substrate.
  • the RHEED when using the RHEED electron beam to irradiate the epitaxial film, the RHEED adopts a relatively small angle of incidence, which is suitable between 0.1 degrees and 10 degrees, so that the RHEED can better detect the surface of the film and obtain more obvious diffraction pattern.
  • the voltage of the RHEED is set to be between 5 and 50 kV, so that the RHEED can obtain a better diffraction pattern.
  • the current size of the RHEED filament is controlled to control the diffraction pattern to be larger than the resolution (minimum pixel point) of the CCD image sensor, so as to facilitate the extraction of feature parameters later.
  • the diffraction pattern should include all diffraction features such as diffraction spots, lines or Kikuchi lines, which makes the subsequent extraction of feature parameters more accurate.
  • the current of the RHEED filament is controlled to control the brightness of the diffraction pattern within the brightness range that can be collected by the CCD image sensor, so that accurate brightness can be obtained later.
  • the brightness distribution of the diffraction pattern is to convert the pattern obtained by the CCD image sensor into a grayscale image to obtain the grayscale distribution of the pixel size in space.
  • the functional relationship between the shape parameter A of the diffraction pattern and the surface roughness is calculated based on the diffraction condition equation.
  • the functional relationship between the shape parameter A of the diffraction pattern and the surface roughness is:
  • the shape parameter A is the aspect ratio of the diffraction spot
  • ⁇ is the roughness of the film surface
  • k is the incident wave vector of the reflective high-energy electron diffractometer
  • d 0 and ⁇ 0 are the inverted space pillars on the surface of the single crystal substrate, respectively.
  • width and surface roughness ⁇ is the incident angle of the reflection high-energy electron diffractometer.
  • the roughness ⁇ is defined as the root mean square value of the coordinates of all particles on the surface of the epitaxial film in the direction perpendicular to the substrate, and the expression is:
  • z(k) is the spatial coordinate value of the kth particle on the film surface perpendicular to the surface
  • n is the total number of all particles on the surface of the epitaxial film.
  • the vacuum device system can adopt pulsed laser deposition, molecular beam epitaxy, magnetron sputtering or chemical vapor deposition system, etc. These systems can grow epitaxial thin films maturely and are suitable for installing RHEED.
  • the single crystal substrates use various semiconductors such as silicon and gallium arsenide, metals and their compounds, perovskites and the above-mentioned types of doped single crystals. These single crystal substrates are easy to obtain and suitable for growing epitaxial films.
  • the present invention utilizes RHEED, which can monitor thin film growth in situ and in real time.
  • RHEED Reflected Electrode
  • the method provided by the present invention extracts characteristic parameters from it, and deduces the functional relationship between the characteristic parameters of the diffraction pattern and the surface roughness based on the diffraction equation, thereby realizing the real-time detection of surface and interface roughness in situ. an important function.
  • Figure 1 shows the RHEED images of LaCoO3 thin films and SrTiO3 substrates grown at temperatures of 560°C, 580°C, 600°C, 620°C, and 640°C.
  • Figure 2 shows the characteristic values of the RHEED diffraction patterns of LaCoO 3 films grown at different temperatures
  • Figure 3 shows the roughness of LaCoO 3 thin films measured by atomic force microscopy and obtained based on this method at different growth temperatures
  • Figure 4 shows the real-time oscillation of the film surface roughness and the intensity of the RHEED diffraction spot.
  • LaCoO 3 thin films were grown on SrTiO 3 (001) single crystal substrates by pulsed laser deposition.
  • the growth conditions were pure oxygen, oxygen pressure of 10 Pa, laser energy density of 2 J/cm 2 , laser frequency of 1 Hz, and RHEED voltage set to 30kV, and the incident angle was set to 2°.
  • the substrate was heated to grow LaCoO 3 films with different surfaces at different temperatures.
  • the growth temperatures were 560°C, 580°C, 600°C, 620°C, and 640°C, respectively.
  • the characteristic parameter A of the surface roughness is extracted from the diffraction pattern, and its value is calculated, as shown in Figure 2.
  • LaCoO 3 thin films were grown on SrTiO 3 (001) single crystal substrates by pulsed laser deposition.
  • the growth conditions were substrate temperature of 650°C, oxygen pressure of 20Pa, laser energy density of 1.5J/cm 2 , RHEED voltage of 30kV and incident angle of 1.8°.
  • a RHEED diffraction pattern was obtained every 5 seconds, the brightness distribution of the diffraction pattern was obtained in real time, and the characteristic parameter A of the diffraction pattern was extracted at the same time.
  • InGaN/GaN multiple quantum well films were grown on silicon single crystal substrates by metal-organic chemical vapor deposition (MOCVD), AlN buffer layers were grown at 400-500°C, undoped GaN layers were grown at 500-700°C, and undoped GaN layers were grown at 700°C. InGaN/GaN multiple quantum wells are grown at ⁇ 800°C.
  • the RHEED voltage was 15kV and the incident angle was 0.5°.
  • a RHEED diffraction pattern was obtained every 3 seconds, the brightness distribution of the diffraction pattern was obtained in real time, and the characteristic parameter A of the diffraction pattern was extracted at the same time.
  • the roughness ⁇ value of the film is obtained in real time according to this functional relationship table.
  • Bi 2 Se 3 thin films were grown on sapphire substrates by molecular beam epitaxy.
  • the substrate temperature was 390°C
  • the Bi and Se evaporation temperatures were 600°C and 400°C, respectively
  • the RHEED voltage was 15kV
  • the incident angle was 0.5°.
  • the RHEED diffraction image acquired by the CCD was intercepted.
  • the characteristic parameter A of surface roughness is extracted from the diffraction pattern, and its value is calculated.
  • Titanium thin films were grown on gold substrates by magnetron sputtering under the conditions of gas pressure of 0.5 Pa, RHEED voltage of 20 kV, and incident angle of 3°.
  • the roughness ⁇ value of the film is obtained in real time according to this functional relationship table.

Abstract

一种通过反射式高能电子衍射仪（以下简称RHEED）原位实时探测薄膜粗糙度的方法。该方法通过采集外延薄膜衍射图案的形状参数，将衍射图案形状参数和薄膜表面粗糙度建立起明确的函数关系，通过该函数关系得到薄膜的表面粗糙度，从而使得在生长过程中便能依据外延薄膜的衍射图案得到其精确的表面粗糙度，拓展了RHEED在薄膜生长中的应用。

Description

一种利用RHEED原位实时定量探测薄膜粗糙度的方法 技术领域
本发明涉及凝聚态物质结构探测领域，尤其涉及一种原位实时探测薄膜表面粗糙度的方法。
背景技术
薄膜表面粗糙度一直是凝聚态物理中研究表面和界面物理中非常基础同时也十分重要的一个信息。表面例如在单晶SrTiO 3(001)衬底表面生长缓冲层，缓冲层是否平整直接关系到后续薄膜的质量；界面例如LaAlO 3/SrTiO 3界面的二维电子气，对于生长时两种材料的界面平整度要求很高，因此薄膜表面的粗糙度是直接关系到外延薄膜的质量的。而且，对于绝大多数依赖于界面的电子器件来说，界面的平整度对器件的性能有着至关重要的影响，比如磁性隧道结、铁电隧道结以及量子级联激光器等。
在表面和界面物理的研究中，样品的制备一般都在真空中完成。而在样品制备过程中，反射式高能电子衍射仪(以下简称RHEED)是被广泛应用的原位表征手段。但当前大都只是用来定性地观察生长情况，比如生长模式、生长层数等。而目前对于薄膜表面粗糙度的探测手段，比如原子力显微镜、椭偏仪等仪器都需要将样品从真空设备中取出再进行测试，而测量界面的主要手段如透射电子显微镜也需要将样品从真空设备中取出，甚至需要对样品进行进一步的处理。但许多薄膜在空气中并不稳定，从真空设备中取出到空气中后往往性质会改变甚至样品直接被破坏，如铝、铅等活泼金属，硅烯，大多数硒化物和碲化物等，导致无法探测薄膜本征信息。所以发展原位实时探测表面和界面粗糙度的技术手段是极为重要的。
发明内容
本发明的目的是：提供一种基于RHEED的原位且实时地探测表面和界面粗糙度的方法。
为了达到上述目的，本发明的技术方案是提供了一种利用RHEED原位实时 定量探测薄膜粗糙度的方法，其特征在于，用于原位实时且定量化地得到外延薄膜的表面粗糙度，包括以下步骤：
a)在真空镀膜装置系统中，在单晶衬底上外延生长薄膜；
b)利用RHEED电子束照射外延薄膜，投射在荧光屏上，通过CCD图像传感器对其摄像得到衍射图案；
c)获得衍射图案的亮度分布；
d)通过衍射图案的亮度分布获得衍射图案的形状参数A；
e)通过衍射图案的形状参数A和表面粗糙度的函数关系得到薄膜的表面粗糙度。
优选地，所述步骤b)中，在单晶衬底上外延生长薄膜的过程中或者在单晶衬底上外延生长薄膜后，利用RHEED电子束照射外延薄膜。
优选地，所述步骤b)中，利用RHEED电子束照射外延薄膜时，RHEED采用较小角度入射，在0.1度到10度之间适宜，这样可以使得RHEED对薄膜表面进行较好的探测且得到较为明显的衍射图案。
优选地，所述步骤b)中，利用RHEED电子束照射外延薄膜时，RHEED的电压设置为5到50kV之间，这样可以使得RHEED获得较好的衍射图案。
优选地，所述步骤b)中，控制RHEED灯丝电流大小将衍射图案控制为大于CCD图像传感器的分辨率(最小像素点)，便于之后的特征参数的提取。
优选地，所述步骤b)中，所述衍射图案应包括衍射斑点、线或菊池线等所有的衍射特征，这使得之后的特征参数的提取更加精确。
优选地，所述步骤c)中，控制RHEED灯丝电流大小将衍射图案的亮度控制在CCD图像传感器所能采集的亮度范围之内，便于之后获得准确的亮度。衍射图案的亮度分布是将CCD图像传感器所获取的图案转为灰度图，得到灰度在空间像素点大小分布
优选地，所述步骤e)中，所述衍射图案的形状参数A和表面粗糙度的函数关系是基于衍射条件方程计算得到的。
优选地，所述步骤e)中，所述衍射图案的形状参数A和表面粗糙度的函数关系为：
Figure PCTCN2021138645-appb-000001
式中，形状参数A为衍射斑的长宽比，σ是薄膜表面的粗糙度，k是反射式高能电子衍射仪入射波矢，d 0、σ 0分别为单晶衬底表面的倒空间柱子宽度和表面粗糙度，θ为反射式高能电子衍射仪入射角度。
优选地，所述粗糙度σ定义为外延薄膜表面所有粒子在垂直衬底方向坐标的方均根值，表达式为：
Figure PCTCN2021138645-appb-000002
式中，z(k)为薄膜表面第k个粒子垂直于表面的空间坐标值，n为外延薄膜表面所有粒子的总数。
本发明中，真空装置系统可以采用脉冲激光沉积、分子束外延、磁控溅射或化学气相沉积系统等，这些系统能较为成熟地生长外延薄膜且适合安装RHEED。单晶衬底采用硅、砷化镓等各类半导体、金属及其化合物，钙钛矿以及上述各类掺杂单晶，这些单晶衬底易于获取且适合生长外延薄膜。
为了能够原位且实时地探测表面和界面粗糙度的信息，本发明利用能原位实时监测薄膜生长的RHEED。通过薄膜RHEED衍射图案的亮度分布，本发明提供的方法从中提取出特征参数，并基于衍射方程推出衍射图案特征参数与表面粗糙度的函数关系，从而实现了原位实时探测表面和界面粗糙度这一重要功能。
附图说明
图1为560℃、580℃、600℃、620℃、640℃温度下生长的LaCoO 3薄膜和SrTiO 3衬底的RHEED图像。
图2为不同温度下生长的LaCoO 3薄膜RHEED衍射图案的特征值；
图3为原子力显微镜测试与基于本方法获得的不同生长温度下LaCoO 3薄膜的粗糙度；
图4为实时的薄膜表面粗糙度以及RHEED衍射斑强度的震荡。
具体实施方式
下面结合具体实施例进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例(1)
通过脉冲激光沉积在SrTiO 3(001)单晶衬底上生长LaCoO 3薄膜，生长条件为通入纯氧，氧气气压10Pa，激光能量密度为2J/cm 2，激光频率为1Hz，RHEED电压设置为30kV、入射角设置为2°。
加热衬底，在不同的温度下生长出不同表面的LaCoO 3薄膜，生长温度分别是560℃、580℃、600℃、620℃、640℃。
待生长过后，截取CCD获取的RHEED衍射图像，如图1所示。
然后获得RHEED衍射图像的亮度分布图，从衍射图案中提取出表面粗糙度的特征参数A，并计算其值，如图2所示。
将A值取值带入表面粗糙度的函数关系式中：
Figure PCTCN2021138645-appb-000003
查找此函数关系表得到薄膜的粗糙度σ值，如图3。
实施例(2)
通过脉冲激光沉积在SrTiO 3(001)单晶衬底上生长LaCoO 3薄膜，生长条件为衬底温度650℃，氧压20Pa，激光能量密度1.5J/cm 2，RHEED电压为30kV、入射角为1.8°。
在生长过程中每间隔5秒获取一张RHEED衍射图，实时获得衍射图案的亮度分布，同时提取衍射图案的特征参数A。
将A值取值带入表面粗糙度的函数关系式中：
Figure PCTCN2021138645-appb-000004
依据此函数关系表实时得到薄膜的粗糙度σ值，如图4所示。
实施例(3)
通过金属有机化学气相沉积系统(MOCVD)在硅单晶衬底上生长InGaN/GaN多量子阱薄膜，在400～500℃生长AlN缓冲层，在500～700℃生长非掺杂GaN层，在700～800℃生长InGaN/GaN多量子阱。RHEED电压为15kV、入射角为0.5°。
在生长过程中每间隔3秒获取一张RHEED衍射图，实时获得衍射图案的亮度分布，同时提取衍射图案的特征参数A。
将A值取值带入表面粗糙度的函数关系式中：
Figure PCTCN2021138645-appb-000005
依据此函数关系表实时得到薄膜的粗糙度σ值。
实施例(4)
通过分子束外延在蓝宝石衬底上生长Bi 2Se 3薄膜，衬底温度为390℃，Bi、Se蒸发温度分别为600℃、400℃，RHEED电压为15kV、入射角为0.5°。
待生长过后，截取CCD获取的RHEED衍射图像。
然后获得RHEED衍射图像的亮度分布图，从衍射图案中提取出表面粗糙度的特征参数A，并计算其值。
将A值取值带入表面粗糙度的函数关系式中：
Figure PCTCN2021138645-appb-000006
查找此函数关系表得到薄膜的粗糙度σ值。
实施例(5)
通过在磁控溅射在金衬底上生长钛薄膜，生长条件为气压0.5Pa，RHEED电压为20kV、入射角为3°。
在生长后获取一张RHEED衍射图，获得衍射图案的亮度分布，同时提取衍射图案的特征参数A。
将A值取值带入表面粗糙度的函数关系式中：
Figure PCTCN2021138645-appb-000007
依据此函数关系表实时得到薄膜的粗糙度σ值。

Claims (10)

  1. 一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，用于原位实时且定量化地得到外延薄膜的表面粗糙度，包括以下步骤：
    a)在真空镀膜装置系统中，在单晶衬底上外延生长薄膜；
    b)利用反射式高能电子衍射仪电子束照射外延薄膜，投射在荧光屏上，通过CCD图像传感器对其摄像得到衍射图案；
    c)获得衍射图案的亮度分布；
    d)通过衍射图案的亮度分布获得衍射图案的形状参数A；
    e)通过衍射图案的形状参数A和表面粗糙度的函数关系得到薄膜的表面粗糙度。
  2. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤b)中，在单晶衬底上外延生长薄膜的过程中或者在单晶衬底上外延生长薄膜后，利用反射式高能电子衍射仪电子束照射外延薄膜。
  3. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤b)中，利用反射式高能电子衍射仪电子束照射外延薄膜时，反射式高能电子衍射仪的入射角度选择范围在0.1度到10度之间。
  4. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤b)中，利用反射式高能电子衍射仪电子束照射外延薄膜时，反射式高能电子衍射仪的电压设置范围在5kV到50kV之间。
  5. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤b)中，CCD图像传感器得到的所述衍射图案大于CCD图像传感器的分辨率。
  6. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤b)中，所述衍射图案包括所有的衍射特征。
  7. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤c)中，所述衍射图案的亮度在CCD图像传感器所能采集的亮度范围之内。
  8. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤e)中，所述衍射图案的形状参数A和表面粗糙度的函数 关系是基于衍射条件方程计算得到的。
  9. 如权利要求1所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述步骤e)中，所述衍射图案的形状参数A和表面粗糙度的函数关系为：
    Figure PCTCN2021138645-appb-100001
    式中，形状参数A为衍射斑的长宽比，σ是薄膜表面的粗糙度，k是反射式高能电子衍射仪入射波矢，d 0、σ 0分别为单晶衬底表面的倒空间柱子宽度和表面粗糙度，θ为反射式高能电子衍射仪入射角度。
  10. 如权利要求8所述的一种利用RHEED原位实时定量探测薄膜粗糙度的方法，其特征在于，所述粗糙度σ定义为外延薄膜表面所有粒子在垂直衬底方向坐标的方均根值，表达式为：
    Figure PCTCN2021138645-appb-100002
    式中，z(k)为薄膜表面第k个粒子垂直于表面的空间坐标值，n为外延薄膜表面所有粒子的总数。
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