CN110320191A - The device and method of in-situ study ion irradiation damage optical signature depth distribution - Google Patents
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Abstract
本发明公开了一种原位分析离子辐照损伤光学特征深度分布的装置及方法，其中装置包括：光阑、静电透镜、样品控制台、光学透镜和光谱仪，离子束依次经过光阑、静电透镜后聚焦在设置于样品控制台上的样品表面，样品经离子束辐照激发出的光经光学透镜射入至光谱仪。本发明避免了传统研究方案样品辐照后辐照损伤的恢复以及二次测量对辐照损伤的破坏，实现离子辐照损伤光学特征的深度分布的原位表征。
The invention discloses a device and method for in-situ analysis of the depth distribution of optical features damaged by ion irradiation, wherein the device includes: an aperture, an electrostatic lens, a sample console, an optical lens and a spectrometer, and the ion beam passes through the aperture and the electrostatic lens in sequence. After focusing on the surface of the sample set on the sample console, the light excited by the sample by ion beam irradiation enters the spectrometer through the optical lens. The invention avoids the recovery of radiation damage after irradiation of samples in traditional research schemes and the destruction of radiation damage by secondary measurement, and realizes the in-situ characterization of the depth distribution of optical characteristics of ion radiation damage.
Description
技术领域technical field
本发明属于离子辐照损伤技术领域，更具体的说是涉及一种原位分析离子辐照损伤光学特征深度分布的装置及方法。The invention belongs to the technical field of ion irradiation damage, and more specifically relates to a device and method for in-situ analysis of the optical characteristic depth distribution of ion irradiation damage.
背景技术Background technique
由于发光光谱超高的灵敏度(探测精度可达十亿分之一量级)，因此在现有的材料离子辐照损伤研究中，一种有效的测试方法即是通过测试材料的发光光谱(通常探测波段为紫外、可见及近红外波段)来表征辐照损伤的光学特征。常规的思路为先进行对材料进行不同条件下的离子辐照，随后利用光致发光(PL，采用激光作激发源)、阴极荧光(CL，采用电子束作激发源)等常见的测试方法进行光学特征测量。这类型研究方法属于离线分析测试方法，材料在离子辐照后的内部微观结构会有所恢复，且采用激光作为激发源时存在着激发波长受限的影响，无法表征能级差高于激光能量的缺陷结构；而采用电子束作为激发源则存在着二次激发的影响，会对原有的损伤结构造成破坏。因此，此类型研究方法获得的离子辐照损伤光学特征的准确性可能存在一定的问题。解决此类型离线分析测试方法的问题可采用离子激发发光法(Ion Beam Induced Luminescence，IBIL)的方法，直接采用进行离子辐照的离子束作为激发源，在离子辐照的同时测量发光光谱，从而实现离子辐照损伤光学特征的原位分析。Due to the ultra-high sensitivity of the luminescence spectrum (the detection accuracy can reach the order of one billionth), an effective test method in the existing research on material ion radiation damage is to test the luminescence spectrum of the material (usually The detection bands are ultraviolet, visible and near-infrared bands) to characterize the optical characteristics of radiation damage. The conventional idea is to first irradiate the material with ions under different conditions, and then use common test methods such as photoluminescence (PL, using a laser as an excitation source) and cathodoluminescence (CL, using an electron beam as an excitation source). Optical Characterization Measurements. This type of research method belongs to the off-line analysis and test method. The internal microstructure of the material will be restored after ion irradiation, and when the laser is used as the excitation source, the excitation wavelength is limited, and it is impossible to characterize the energy level difference higher than the laser energy. The defect structure; and the use of electron beams as the excitation source has the influence of secondary excitation, which will cause damage to the original damage structure. Therefore, there may be certain problems in the accuracy of the optical characteristics of ion irradiation damage obtained by this type of research method. To solve the problem of this type of off-line analysis and test method, the method of ion beam induced luminescence (Ion Beam Induced Luminescence, IBIL) can be used, and the ion beam for ion irradiation is directly used as the excitation source, and the luminescence spectrum is measured while the ion is irradiated, thereby Realize the in-situ analysis of the optical characteristics of ion irradiation damage.
目前的离子激发发光分析获得的结果是离子入射范围内的所有缺陷的发光光谱，由于离子种类或者能量的差异，对应的核阻止本领和电子阻止本领存在明显的差异，使得离子损伤的深度分布并不均匀；温度等因素也会影响特定类型缺陷的迁徙和演变，造成离子辐照损伤深度分布的变化。The results obtained by the current ion excitation luminescence analysis are the luminescence spectra of all defects within the incident range of ions. Due to the difference in ion type or energy, there are obvious differences in the corresponding nuclear stopping power and electronic stopping power, so that the depth distribution of ion damage is not the same. Inhomogeneity; factors such as temperature will also affect the migration and evolution of specific types of defects, resulting in changes in the depth distribution of ion irradiation damage.
因此，如何提供一种原位分析离子辐照损伤光学特征深度分布的装置及方法成为了本领域技术人员亟需解决的问题。Therefore, how to provide a device and method for in-situ analysis of the depth distribution of optical features damaged by ion irradiation has become an urgent problem to be solved by those skilled in the art.
发明内容Contents of the invention
有鉴于此，本发明提供了一种原位分析离子辐照损伤光学特征深度分布的装置及方法，避免了传统研究方案样品辐照后辐照损伤的恢复以及二次测量对辐照损伤的破坏，实现离子辐照损伤光学特征的深度分布的原位表征。In view of this, the present invention provides a device and method for in-situ analysis of the depth distribution of optical characteristics of ion irradiation damage, which avoids the recovery of radiation damage after sample irradiation in traditional research programs and the destruction of radiation damage by secondary measurement , to realize the in situ characterization of the depth distribution of ion irradiation damage optical features.
为了实现上述目的，本发明采用如下技术方案：In order to achieve the above object, the present invention adopts the following technical solutions:
一种原位分析离子辐照损伤光学特征深度分布的装置，包括：光阑、静电透镜、样品控制台、光学透镜和光谱仪，离子束依次经过所述光阑、所述静电透镜后聚焦在设置于所述样品控制台上的样品表面，样品经离子束辐照激发出的光经所述光学透镜射入至光谱仪。A device for in-situ analysis of the depth distribution of optical features damaged by ion irradiation, comprising: an aperture, an electrostatic lens, a sample console, an optical lens, and a spectrometer, and the ion beam sequentially passes through the aperture and the electrostatic lens and focuses on the On the surface of the sample on the sample control console, the light excited by the sample through ion beam irradiation enters the spectrometer through the optical lens.
优选的，所述光阑与所述静电透镜间沿离子束传输方向依次设置有第一偏转电极、第二偏转电极。离子束通过第一偏转电极和第二偏转电极后，能够调节离子束的发散度，保证离子束的传输品质。Preferably, a first deflection electrode and a second deflection electrode are sequentially arranged between the diaphragm and the electrostatic lens along the ion beam transmission direction. After the ion beam passes through the first deflection electrode and the second deflection electrode, the divergence of the ion beam can be adjusted to ensure the transmission quality of the ion beam.
优选的，所述第一偏转电极采用四极偏转电极，所述第二偏转电极采用八极偏转电极，通过光阑、四极偏转电极、八极偏转电极、静电透镜后，可将离子束聚焦至纳米级宽度。Preferably, the first deflection electrode is a quadrupole deflection electrode, and the second deflection electrode is an octapole deflection electrode. After passing through a diaphragm, a quadrupole deflection electrode, an octapole deflection electrode, and an electrostatic lens, the ion beam can be focused to nanometer widths.
优选的，还包括CCD相机，所述CCD相机设置于所述离子束聚焦点的正上方。利用聚焦的离子束辐照样品控制台上的荧光材料，根据CCD相机观察到的荧光斑尺寸及位置信息，结合样品控制台的调节，确保离子束聚焦在样品表面。Preferably, a CCD camera is also included, and the CCD camera is arranged directly above the focus point of the ion beam. The focused ion beam is used to irradiate the fluorescent material on the sample console, and according to the size and position information of the fluorescent spot observed by the CCD camera, combined with the adjustment of the sample console, it is ensured that the ion beam is focused on the sample surface.
优选的，所述样品控制台采用高精度可移动控制台，可实现样品控制台纳米级步长的移动，最小步长可达5纳米。Preferably, the sample console adopts a high-precision movable console, which can realize the movement of the sample console in nanometer steps, and the minimum step size can reach 5 nanometers.
一种原位分析离子辐照损伤光学特征深度分布的方法，包括如下步骤：A method for in-situ analysis of the depth distribution of optical features damaged by ion irradiation, comprising the following steps:
(1)离子束经过光阑后，利用静电透镜将离子束进一步聚焦，获得纳米级宽度的离子束；(1) After the ion beam passes through the diaphragm, the ion beam is further focused by an electrostatic lens to obtain an ion beam with a nanoscale width;
(2)调节样品控制台，确保离子束聚焦在样品表面；(2) Adjust the sample console to ensure that the ion beam is focused on the sample surface;
(3)调节光学透镜的位置及角度，确保光谱仪光路的焦点与离子束在样品表面聚焦的焦点在同一位置；(3) Adjust the position and angle of the optical lens to ensure that the focus of the optical path of the spectrometer is at the same position as the focus of the ion beam on the sample surface;
(4)调节样品控制台使共聚焦点处于样品的不同深度，实现离子辐照损伤光学特征深度分布的原位表征。(4) Adjust the sample console so that the confocal points are at different depths of the sample, so as to realize the in-situ characterization of the depth distribution of the optical features damaged by ion irradiation.
优选的，所述光阑与所述静电透镜间沿离子束传输方向依次设置有第一偏转电极、第二偏转电极，离子束通过第一偏转电极和第二偏转电极调节离子束发散度，保证了离子束的传输品质。Preferably, a first deflection electrode and a second deflection electrode are sequentially arranged between the diaphragm and the electrostatic lens along the ion beam transmission direction, and the ion beam passes through the first deflection electrode and the second deflection electrode to adjust the divergence of the ion beam to ensure the transmission quality of the ion beam.
优选的，所述步骤(2)中利用聚焦的离子束辐照样品控制台上的荧光材料，根据CCD相机观察到的荧光斑尺寸及位置信息，结合样品控制台的调节，确保离子束聚焦在样品表面。Preferably, in the step (2), the focused ion beam is used to irradiate the fluorescent material on the sample console, and according to the fluorescent spot size and position information observed by the CCD camera, combined with the adjustment of the sample console, it is ensured that the ion beam is focused on sample surface.
优选的，所述步骤(3)中利用激光笔从光谱仪光纤接口处反向照射，利用光路的可逆性，根据CCD相机观察到的荧光斑尺寸及位置信息，调节光学透镜位置和角度，确保光谱仪光路的焦点与步骤(2)中离子束聚焦的焦点在样品表面同一位置。Preferably, in the step (3), the laser pointer is used to irradiate backward from the optical fiber interface of the spectrometer, and the reversibility of the optical path is used to adjust the position and angle of the optical lens according to the fluorescent spot size and position information observed by the CCD camera to ensure that the spectrometer The focus of the optical path and the focus of the ion beam in step (2) are at the same position on the sample surface.
本发明的有益效果在于：The beneficial effects of the present invention are:
本发明结构简单，操作方便，利用光阑、第一偏转电极、第二偏转电极以及静电透镜，将离子束聚焦至纳米级宽度；利用光学透镜聚焦荧光，通过调试使得聚焦离子束的焦点和光谱仪的焦点共于一个焦点，实现公共焦点处离子辐照损伤光学特征的测量，随后利用高精度的样品控制台实现样品纳米级步长的移动，从而实现样品不同深度的离子辐照损伤光学特征的原位分析。本发明利用原位表征技术避免了传统研究方案样品辐照后辐照损伤的恢复以及二次测量对辐照损伤的破坏；结合共聚焦原理，实现离子辐照损伤光学特征的深度分布的原位表征。The invention is simple in structure and easy to operate. The ion beam is focused to a nanoscale width by using the diaphragm, the first deflection electrode, the second deflection electrode and the electrostatic lens; the optical lens is used to focus the fluorescence, and the focus of the focused ion beam and the spectrometer The focal points are shared in one focal point to realize the measurement of the optical characteristics of the ion irradiation damage at the common focal point, and then use the high-precision sample console to realize the movement of the sample in nanometer steps, so as to realize the measurement of the optical characteristics of the ion irradiation damage at different depths of the sample in situ analysis. The invention utilizes in-situ characterization technology to avoid the recovery of radiation damage after irradiation of samples in traditional research programs and the damage to radiation damage caused by secondary measurement; combined with the principle of confocal, the in-situ in-situ analysis of the depth distribution of optical characteristics of ion radiation damage is realized characterization.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据提供的附图获得其他的附图。In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only It is an embodiment of the present invention, and those skilled in the art can also obtain other drawings according to the provided drawings on the premise of not paying creative efforts.
图1附图为本发明的结构示意图。Fig. 1 accompanying drawing is the structural representation of the present invention.
其中，图中，Among them, in the figure,
1-光阑；2-静电透镜；3-样品控制台；4-光学透镜；5-光谱仪；6-样品；7-第一偏转电极；8-第二偏转电极；9-CCD相机。1-diaphragm; 2-electrostatic lens; 3-sample console; 4-optical lens; 5-spectrometer; 6-sample; 7-first deflection electrode; 8-second deflection electrode; 9-CCD camera.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
请参阅附图1，本发明提供了一种原位分析离子辐照损伤光学特征深度分布的装置，包括：光阑1、静电透镜2、样品控制台3、光学透镜4和光谱仪5，离子束依次经过光阑1、静电透镜2后聚焦在设置于样品控制台3上的样品表面，样品6经离子束辐照激发出的光经光学透镜4射入至光谱仪5。其中光阑1可根据需求的不同选用不同的口径，利用光阑1能够减小离子束束斑直径。Please refer to accompanying drawing 1, the present invention provides a kind of device of in situ analysis ion radiation damage optical feature depth distribution, comprising: diaphragm 1, electrostatic lens 2, sample console 3, optical lens 4 and spectrometer 5, ion beam After sequentially passing through the aperture 1 and the electrostatic lens 2, it is focused on the sample surface set on the sample console 3, and the light excited by the sample 6 by ion beam irradiation enters the spectrometer 5 through the optical lens 4. The aperture 1 can be selected with different apertures according to different requirements, and the diameter of the ion beam spot can be reduced by using the aperture 1 .
在另一种实施例中，光阑1与静电透镜2间沿离子束传输方向依次设置有第一偏转电极7、第二偏转电极8。离子束通过第一偏转电极7和第二偏转电极8后，能够调节离子束的发散度，保证离子束的传输品质。In another embodiment, a first deflecting electrode 7 and a second deflecting electrode 8 are sequentially arranged between the aperture 1 and the electrostatic lens 2 along the ion beam transmission direction. After the ion beam passes through the first deflection electrode 7 and the second deflection electrode 8, the divergence of the ion beam can be adjusted to ensure the transmission quality of the ion beam.
在另一种实施例中，第一偏转电极7采用四极偏转电极，第二偏转电极8采用八极偏转电极，通过光阑1、四极偏转电极、八极偏转电极、静电透镜2后，可将离子束聚焦至纳米级宽度(大于5nm)。In another embodiment, the first deflection electrode 7 is a quadrupole deflection electrode, and the second deflection electrode 8 is an octapole deflection electrode. Ion beams can be focused to nanometer-scale widths (greater than 5nm).
本发明还包括CCD相机9，CCD相机9设置于离子束聚焦点的正上方。利用聚焦的离子束辐照样品控制台3上的荧光材料，根据CCD相机9观察到的荧光斑尺寸及位置信息，结合样品控制台3的调节，确保离子束聚焦在样品表面。The present invention also includes a CCD camera 9, and the CCD camera 9 is arranged directly above the focus point of the ion beam. The focused ion beam is used to irradiate the fluorescent material on the sample console 3, and according to the fluorescent spot size and position information observed by the CCD camera 9, combined with the adjustment of the sample console 3, it is ensured that the ion beam is focused on the sample surface.
在另一种实施例中，样品控制台3采用高精度可移动控制台，可实现样品控制台3纳米级步长的移动，最小步长可达5纳米。In another embodiment, the sample console 3 adopts a high-precision movable console, which can realize the movement of the sample console with a step size of 3 nanometers, and the minimum step size can reach 5 nanometers.
一种原位分析离子辐照损伤光学特征深度分布的方法，包括如下步骤：A method for in-situ analysis of the depth distribution of optical features damaged by ion irradiation, comprising the following steps:
(1)离子束经过光阑1后，利用静电透镜2将离子束进一步聚焦，获得纳米级宽度的离子束；(1) After the ion beam passes through the diaphragm 1, the ion beam is further focused by the electrostatic lens 2 to obtain an ion beam with a nanoscale width;
(2)调节样品控制台3，确保离子束聚焦在样品表面；(2) Adjust the sample console 3 to ensure that the ion beam is focused on the sample surface;
(3)调节光学透镜4的位置及角度，确保光谱仪5光路的焦点与离子束在样品表面聚焦的焦点在同一位置；(3) Adjust the position and angle of the optical lens 4 to ensure that the focus of the optical path of the spectrometer 5 is at the same position as the focus of the ion beam focusing on the sample surface;
(4)同步开启离子束发射装置和光谱仪5，进行共聚焦点处样品辐照损伤光学特征的光谱采集，调节样品控制台3使共聚焦点处于样品6的不同深度，实现离子辐照损伤光学特征深度分布的原位表征。(4) Turn on the ion beam emitting device and the spectrometer 5 synchronously to collect the spectrum of the optical characteristics of the radiation damage of the sample at the confocal point, adjust the sample console 3 so that the confocal point is at different depths of the sample 6, and realize the optical characteristic depth of the ion radiation damage In situ characterization of the distribution.
在另一种实施例中，光阑1与静电透镜2间沿离子束传输方向依次设置有第一偏转电极7、第二偏转电极8，离子束通过第一偏转电极7和第二偏转电极8调节离子束发散度，保证了离子束的传输品质。In another embodiment, a first deflecting electrode 7 and a second deflecting electrode 8 are sequentially arranged between the diaphragm 1 and the electrostatic lens 2 along the ion beam transmission direction, and the ion beam passes through the first deflecting electrode 7 and the second deflecting electrode 8 The ion beam divergence is adjusted to ensure the transmission quality of the ion beam.
在另一种实施例中，步骤(2)中利用聚焦的离子束辐照样品控制台3上的荧光材料，根据CCD相机9观察到的荧光斑尺寸及位置信息，结合样品控制台3的调节，确保离子束聚焦在样品表面。In another embodiment, in step (2), the focused ion beam is used to irradiate the fluorescent material on the sample console 3, according to the size and position information of the fluorescent spot observed by the CCD camera 9, combined with the adjustment of the sample console 3 , to ensure that the ion beam is focused on the sample surface.
在另一种实施例中，步骤(3)中利用激光笔从光谱仪5的光纤接口处反向照射，利用光路的可逆性，根据CCD相机9观察到的荧光斑尺寸及位置信息，调节光学透镜4位置和角度，确保光谱仪5光路的焦点与步骤(2)中离子束聚焦的焦点在样品表面同一位置。In another embodiment, in step (3), the laser pointer is used to illuminate backwards from the optical fiber interface of the spectrometer 5, and the optical lens is adjusted according to the fluorescent spot size and position information observed by the CCD camera 9 by utilizing the reversibility of the optical path. 4 position and angle, ensure that the focus of the optical path of the spectrometer 5 and the focus of the ion beam focusing in step (2) are at the same position on the sample surface.
本发明结构简单，操作方便，利用光阑1、第一偏转电极7、第二偏转电极8以及静电透镜2，将离子束聚焦至纳米级宽度；利用光学透镜4聚焦荧光，通过调试使得聚焦离子束的焦点和光谱仪5的焦点共于一个焦点，实现公共焦点处离子辐照损伤光学特征的测量，随后利用高精度的样品控制台3实现样品纳米级步长的移动，从而实现样品不同深度的离子辐照损伤光学特征的原位分析。本发明利用原位表征技术避免了传统研究方案样品辐照后辐照损伤的恢复以及二次测量对辐照损伤的破坏；结合共聚焦原理，实现离子辐照损伤光学特征的深度分布的原位表征。The present invention is simple in structure and easy to operate. The ion beam is focused to a nanoscale width by using the diaphragm 1, the first deflection electrode 7, the second deflection electrode 8 and the electrostatic lens 2; The focal point of the beam and the focal point of the spectrometer 5 are in the same focal point to realize the measurement of the optical characteristics of the ion irradiation damage at the common focal point, and then use the high-precision sample console 3 to realize the movement of the sample in nanometer steps, so as to realize the measurement of the sample at different depths. In situ analysis of optical signatures of ion irradiation damage. The invention utilizes in-situ characterization technology to avoid the recovery of radiation damage after irradiation of samples in traditional research programs and the damage to radiation damage caused by secondary measurement; combined with the principle of confocal, the in-situ in-situ analysis of the depth distribution of optical characteristics of ion radiation damage is realized characterization.
本说明书中各个实施例采用递进的方式描述，每个实施例重点说明的都是与其他实施例的不同之处，各个实施例之间相同相似部分互相参见即可。对于实施例公开的装置而言，由于其与实施例公开的方法相对应，所以描述的比较简单，相关之处参见方法部分说明即可。Each embodiment in this specification is described in a progressive manner, each embodiment focuses on the difference from other embodiments, and the same and similar parts of each embodiment can be referred to each other. As for the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and for the related information, please refer to the description of the method part.
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。The above description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
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