CN114034528A - Preparation method of TEM (transverse electric and magnetic) section sample and TEM section sample - Google Patents
Preparation method of TEM (transverse electric and magnetic) section sample and TEM section sample Download PDFInfo
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- CN114034528A CN114034528A CN202111312641.7A CN202111312641A CN114034528A CN 114034528 A CN114034528 A CN 114034528A CN 202111312641 A CN202111312641 A CN 202111312641A CN 114034528 A CN114034528 A CN 114034528A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
本发明的实施例提供了一种TEM截面样品的制备方法和TEM截面样品，涉及纳米材料技术领域，其首先制备带有标记槽的待处理样品，且待处理样品的观测区域与标记槽在待处理样品的延展方向上间隔设置，然后对待处理样品上具有标记槽的表面进行减薄处理，以扩大标记槽的宽度和深度，当标记槽的边缘到达观测区域时，停止离子束减薄处理。相较于现有技术，本发明在观测区域附近引入标记槽，从而实现对样品进行定向减薄，进而实现减薄样品的厚度可控，当标识槽底部到达观测时，停止离子束减薄，有效解决了减薄过程中截面样品观测处被去除掉的问题，极大提高了截面样品的制备成功率和测试效率，有效降低了截面样品的制备成本，缩短了制备时间。
Embodiments of the present invention provide a method for preparing a TEM cross-section sample and a TEM cross-section sample, which relate to the technical field of nanomaterials. First, a to-be-processed sample with a marking groove is prepared, and the observation area of the to-be-processed sample and the marking groove are in the waiting area. The samples are arranged at intervals in the extending direction, and then the surface with the marking grooves on the sample to be processed is thinned to expand the width and depth of the marking grooves. When the edge of the marking grooves reaches the observation area, the ion beam thinning processing is stopped. Compared with the prior art, the present invention introduces a marking groove near the observation area, so as to realize the directional thinning of the sample, thereby realizing the controllable thickness of the thinned sample, and when the bottom of the marking groove reaches the observation, the ion beam thinning is stopped, It effectively solves the problem that the observation part of the cross-section sample is removed during the thinning process, greatly improves the preparation success rate and testing efficiency of the cross-section sample, effectively reduces the preparation cost of the cross-section sample, and shortens the preparation time.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a TEM (transverse electric and magnetic field) section sample and the TEM section sample.
Background
With the development and application of nanotechnology, Transmission Electron Microscopy (TEM) is a main characterization tool for nano materials and devices, which is used to observe the microstructure of materials and the film morphology, size and characteristics of devices. Sample preparation is carried out before TEM section sample test, and the quality of the prepared sample is directly related to the test result. The thickness of the sample can be tested when the electron transparency is achieved below 100nm, so that the thinning is the most important link in the preparation process of the TEM section sample. The mechanical grinding and ion beam thinning technology is the main method for preparing the existing TEM section sample.
In the prior art, no matter mechanical grinding or ion beam thinning is carried out, the TEM section sample is uniformly thinned, the situation that the observation position is completely removed due to the fact that the sample is thinned to pass through the head is easy to occur, the sample can not be tested any more, the prepared sample becomes a waste sample, and the sample needs to be prepared again. Thus, it takes a lot of time and effort to prepare the sample only, which greatly increases the preparation time and cost of the sample and also reduces the TEM testing rate and efficiency.
Disclosure of Invention
The invention aims to provide a TEM cross-section sample preparation method and a TEM cross-section sample, which effectively solve the problem that the observation position of the TEM cross-section sample is removed in the thinning process, greatly improve the preparation success rate and the test efficiency of the TEM cross-section sample, effectively reduce the preparation cost of the TEM cross-section sample and shorten the preparation time.
Embodiments of the invention may be implemented as follows:
in a first aspect, the present invention provides a method for preparing a TEM cross-section sample, comprising:
preparing a sample to be processed with a marking groove on the surface;
thinning the surface of the sample to be processed, which is provided with the marking groove, so as to enlarge the width and the depth of the marking groove;
stopping thinning processing when the edge of the marking groove reaches the observation area;
wherein the observation region and the marking groove are arranged at intervals in the extending direction of the sample to be processed.
In an alternative embodiment, the step of thinning the surface of the sample to be processed, which has the mark groove, includes:
emitting ion beams to the surface of the sample to be processed to thin the sample to be processed;
wherein the ion beam covers the marker slot.
In an alternative embodiment, the step of emitting an ion beam to the surface of the sample to be processed comprises:
emitting an ion beam with an initial incident angle to the surface of the sample to be processed;
linearly decreasing an incident angle of the ion beam as a depth and a width of the mark trench increase.
In an alternative embodiment, the step of emitting an ion beam to the surface of the sample to be processed comprises:
emitting an ion beam with an initial incident angle to the surface of the sample to be processed for a first preset time t 1;
emitting an ion beam at a first incident angle to the surface of the sample to be processed for a second preset time t 2;
emitting an ion beam at a second incident angle to the surface of the sample to be processed for a third preset time t 3;
wherein the initial incident angle is greater than the first incident angle, which is greater than the second incident angle.
In an alternative embodiment, the step of emitting an ion beam to the surface of the sample to be processed further comprises:
emitting an ion beam with initial electron energy to the surface of the sample to be processed;
decreasing an electron energy of the ion beam as a depth and a width of the mark trench increase.
In an alternative embodiment, the step of emitting an ion beam to the surface of the sample to be processed comprises:
emitting an ion beam of initial electron energy to the surface of the sample to be processed for a first preset time t 1;
emitting an ion beam of a first electron energy to the surface of the sample to be processed for a second preset time t 2;
emitting an ion beam of a second electron energy to the surface of the sample to be processed for a third preset time t 3;
wherein the initial electron energy is greater than the first electron energy, which is greater than the second electron energy.
In an alternative embodiment, the step of preparing a sample to be treated having a labeled groove on a surface thereof comprises:
preparing a sample to be treated;
and forming marking grooves on the surfaces of two sides of the sample to be processed.
In an alternative embodiment, the step of preparing the sample to be treated comprises:
cutting an initial sample to be tested into a rectangle;
washing the initial sample;
and adhering one side surfaces of the two initial samples together by using glue to form the sample to be treated.
In an alternative embodiment, the depth of the marker groove is 1/10-1/7 of the thickness of the sample to be treated.
In a second aspect, the present invention provides a TEM cross-section sample prepared by the method for preparing a TEM cross-section sample according to any one of the above embodiments.
The beneficial effects of the embodiment of the invention include, for example:
the preparation method of the TEM section sample and the TEM section sample provided by the embodiment of the invention comprise the steps of firstly preparing a to-be-processed sample with a mark groove on the surface, arranging the observation region and the mark groove at intervals in the extension direction of the to-be-processed sample, then thinning the surface of the to-be-processed sample with the mark groove to enlarge the width and the depth of the mark groove, and stopping thinning when the edge of the mark groove reaches the observation region. Compared with the prior art, the marking groove is introduced near the observation area, the directional thinning of the sample is realized, the thickness of the thinned sample is controllable, when the bottom of the marking groove reaches the observation, the ion beam thinning is stopped, the problem that the observation position of the TEM cross-section sample is removed in the thinning process is effectively solved, the preparation success rate and the test efficiency of the TEM cross-section sample are greatly improved, the preparation cost of the TEM cross-section sample is effectively reduced, and the preparation time is shortened.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a block diagram illustrating the steps of a method for preparing a TEM cross-section sample according to an embodiment of the present invention;
fig. 2 to 6 are process flow charts of a method for preparing a TEM cross-section sample according to an embodiment of the present invention.
Icon: 100-a sample to be treated; 110-a marker slot; 130-observation area; 200-ion beam.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that if the terms "upper", "lower", "inside", "outside", etc. indicate an orientation or a positional relationship based on that shown in the drawings or that the product of the present invention is used as it is, this is only for convenience of description and simplification of the description, and it does not indicate or imply that the device or the element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention.
Furthermore, the appearances of the terms "first," "second," and the like, if any, are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
It is noted that, as disclosed in the background art, the prior art generally employs ion beam bombardment atomic thinning for TEM cross-section sample preparation, and since TEM cross-section sample observation needs to be performed below 100nm in thickness, the degree of ion beam thinning is critical to sample preparation. The defects that the thinning process cannot be stopped in time due to the fact that the thinning thickness is difficult to control in the prior art are mainly caused by the fact that positioning marks cannot be carried out on observation positions of TEM section samples in the ion beam thinning process and the thickness of the TEM samples cannot be accurately controlled at the final stage of ion beam thinning.
In order to solve the problems, the invention provides a novel TEM cross-section sample and a preparation method thereof, which effectively solve the problem that the observation position of the TEM cross-section sample is removed in the thinning process, greatly improve the preparation success rate and the test efficiency of the TEM cross-section sample, effectively reduce the preparation cost of the TEM cross-section sample and shorten the preparation time. It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Referring to fig. 1, this embodiment provides a method for preparing a TEM cross-section sample, which is a TEM cross-section sample that can be observed by a transmission electron microscope. Meanwhile, the method effectively solves the problem that the observation position of the TEM cross-section sample is removed in the thinning process in the prior art, greatly improves the preparation success rate and the test efficiency of the TEM cross-section sample, effectively reduces the preparation cost of the TEM cross-section sample, and shortens the preparation time.
The preparation method of the TEM cross section sample provided in this embodiment includes the following steps:
s1: a sample to be processed 100 having a marking groove 110 on the surface thereof is prepared.
Referring to fig. 2 in combination, specifically, when step S1 is executed, it is first necessary to prepare a sample 100 to be processed, and then to form the marking grooves 110 on both side surfaces of the sample 100 to be processed. The forming method of the mark groove 110 may be etching or laser grooving. In preparing a sample to be treated 100, a plurality of initial samples to be tested, i.e., initial samples in the form of sheets, are first provided; cutting an initial sample to be tested into a rectangular shape, and cleaning the initial sample to remove dust or external impurities generated in the cutting process; the samples 100 to be treated are then formed by gluing together one side surface of the two initial samples. And then grooving the other side surfaces of the two initial samples to form a marking groove 110, and preparing and forming the sample to be processed 100 with the marking groove 110.
It should be noted that in the present embodiment, the depth of the marking groove 110 is 1/10-1/7 of the thickness of the sample 100 to be processed, specifically, the overall thickness of the sample 100 to be processed is between 700 and 800 μm, and the depth of the marking groove 110 is 100 and 110 μm.
It should be further noted that, in the embodiment, the observation region 130 is preset in the sample to be processed 100, and the observation region 130 may be calibrated according to an image of an observation computer, so as to facilitate the subsequent observation of whether the marking groove 110 reaches the observation region 130.
In the present embodiment, the observation region 130 and the marker groove 110 are provided at a distance in the extending direction of the sample 100 to be processed. The extending direction of the sample 100 to be processed refers to the extending direction of the surface of the sample 100 to be processed, which has the marking groove 110, i.e. the horizontal direction. The mark groove 110 and the observation region 130 are arranged at intervals, so that the difficulty in controlling the thickness of the observation region 130 caused by the fact that the mark groove 110 directly extends from the bottom to the observation region 130 can be avoided.
S2: the surface of the sample 100 to be processed having the marking groove 110 is subjected to a thinning process to enlarge the width and depth of the marking groove 110.
Referring to fig. 3 to 5 in combination, specifically, when step S2 is performed, the ion beam 200 is emitted to the surface of the sample to be processed 100 to thin the sample to be processed 100, wherein the ion beam 200 covers the marking slot 110. Preferably, the thinning process can be performed on the area near the mark slot 110 by taking the mark slot 110 as the bombardment center, because the mark slot 110 is prepared in advance, the mark slot 110 can guide the ion beam 200 to perform directional thinning, and the setting of the mark slot 110 can omit the process of partial ion bombardment, thereby further improving the thinning speed.
In this embodiment, the step of emitting the ion beam 200 on the surface of the sample 100 to be processed specifically includes: emitting the ion beam 200 of the initial incident angle to the surface of the sample 100 to be processed for a first preset time t1, and then emitting the ion beam 200 of the first incident angle to the surface of the sample 100 to be processed for a second preset time t 2; then, emitting the ion beam 200 with the second incident angle on the surface of the sample 100 to be processed for a third preset time t 3; wherein the initial incident angle is greater than the first incident angle, which is greater than the second incident angle. That is, as the ion beam 200 thinning process proceeds, the ion beam 200 having a smaller incident angle may be used.
Specifically, the initial incident angle is 9 °, the first incident angle is 7 °, and the second incident angle is 5 °, which is only illustrative and not limiting.
It should be noted that the first preset time t1, the second preset time t2, and the third preset time t3 may be set according to the material and the electron energy of the ion beam 200, and the values may be empirical values or obtained through simulation experiments.
In this embodiment, the step of emitting the ion beam 200 to the surface of the sample 100 to be processed further includes: emitting an ion beam 200 of initial electron energy to the surface of a sample 100 to be processed for a first preset time t 1; then emitting the ion beam 200 of the first electron energy to the surface of the sample 100 to be processed for a second preset time t 2; emitting the ion beam 200 of the second electron energy to the surface of the sample 100 to be processed for a third preset time t 3; the initial electron energy is greater than the first electron energy, and the first electron energy is greater than the second electron energy.
Specifically, the initial electron energy is 4keV, the first electron energy is 2keV, and the second electron energy is 0.5keV, again by way of example only and not by way of limitation.
It should be noted that, here, the ion beam 200 with the initial electron energy and the ion beam 200 with the initial incident angle are in a parallel condition, while the ion beam 200 with the first electron energy and the ion beam 200 with the first incident angle are in a parallel condition, the ion beam 200 with the second electron energy and the ion beam 200 with the second incident angle are also in a parallel condition, that is, the ion beam 200 with the initial electron energy and the initial incident angle is emitted on the surface of the sample 100 to be processed within the first preset time t1, the ion beam 200 with the first electron energy and the first incident angle is emitted on the surface of the sample 100 to be processed within the second preset time t2, and the ion beam 200 with the second electron energy and the second incident angle is emitted on the surface of the sample 100 to be processed within the third preset time t 3.
In the embodiment, since the mark slots 110 are located at the upper and lower sides of the sample 100 to be processed, when the sample 100 to be processed having the mark slots 110 is thinned by the ion beam 200, two ion guns may be used to bombard the sample 100 to be processed, which includes the observation region 130 and forms the mark slots 110, with the ion beam 200 bombarding the mark slots 110 at an incident angle of 9 ° and an electron energy of 4keV, in order to rapidly knock off atoms near the mark slots 110 and further rapidly thin the mark slots 110. Ion beam 200 thinning is then continued, expanding the depth and width of the marker slot 110. The incident angle of the ion beam 200 is reduced to 7 deg., while also reducing the electron energy to 2keV to slow down the thinning rate of the mark trench 110. Then, in the final stage of thinning of the ion beam 200, the incident angle of the ion beam 200 is further decreased to 5 ° or less, and the electron energy is also further decreased to 0.5keV or less, so as to further slow down the thinning rate and prevent the edge trajectory of the mark slot 110 from passing through the observation region 130.
In other preferred embodiments of the present invention, the incident angle may be decreased in a linear manner, that is, in step S2, the ion beam 200 with the initial incident angle is first emitted onto the surface of the sample 100 to be processed, and then the incident angle of the ion beam 200 is linearly decreased as the depth and width of the mark slot 110 increase. For example, a linear relationship between the depth of the mark groove 110 and the incident angle may be established such that the incident angle is inversely proportional to the depth of the mark groove 110, and the incident angle is gradually decreased as the depth of the mark groove 110 increases.
In other preferred embodiments of the present invention, the electron energy of the ion beam 200 may be decreased in a linear manner, that is, the ion beam 200 with initial electron energy is first emitted to the surface of the sample 100 to be processed when step S2 is executed, and then the electron energy of the ion beam 200 is linearly decreased as the depth and width of the mark groove 110 are increased. For example, a linear relationship between the depth of the mark trench 110 and the electron energy of the ion beam 200 may be established such that the electron energy of the ion beam 200 is inversely proportional to the depth of the mark trench 110, and the electron energy of the ion beam 200 gradually decreases as the depth of the mark trench 110 increases.
S3: when the edge of the mark groove 110 reaches the observation region 130, the thinning process is stopped.
Referring to fig. 6, in particular, the thinning process can be observed by an observation computer, and when the edge of the marking slot 110 reaches the observation area, the ion gun is controlled to stop working. In the actual thinning, a through hole is formed just below the mark trench 110, and the thinning of the ion beam 200 is terminated when the edge of the mark trench 110 is observed to contact the observation region 130. This process allows for a sufficient viewing window time since the final stages of thinning of the ion beam 200 continue to reduce the angle of incidence of the ion beam 200 to 5 deg. or less while also continuing to reduce the electron energy to 0.5keV or less. That is, when the mark groove 110 forms a through hole under the mark groove 110 of the sample 100 to be processed and the edge of the mark groove 110 contacts the observation region 130, the ion beam 200 thinning of the observation region 130 is finished.
The present embodiment also provides a TEM cross section sample, which is prepared by the above-mentioned method for preparing a TEM cross section sample.
In summary, according to the preparation method of the TEM cross-section sample and the TEM cross-section sample provided by the embodiments of the present invention, the sample to be processed 100 having the mark groove 110 on the surface is prepared, the sample to be processed 100 has the observation region 130, the observation region 130 and the mark groove 110 are arranged at an interval in the extending direction of the sample to be processed 100, then the surface of the sample to be processed 100 having the mark groove 110 is thinned to expand the width and the depth of the mark groove 110, and when the edge of the mark groove 110 reaches the observation region 130, the thinning process is stopped. Compared with the prior art, the marking groove 110 is introduced near the observation area 130, so that the directional thinning of the sample 100 to be processed is realized, the thickness of the thinned sample is controllable, the thinning of the ion beam 200 is stopped when the bottom of the marking groove reaches the observation position, the problem that the observation position of the TEM cross-section sample is removed in the thinning process is effectively solved, the preparation success rate and the test efficiency of the TEM cross-section sample are greatly improved, the preparation cost of the TEM cross-section sample is effectively reduced, and the preparation time is shortened.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103776669A (en) * | 2012-10-26 | 2014-05-07 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of TEM (Transmission Electron Microscope) sample |
| CN112649624A (en) * | 2020-12-30 | 2021-04-13 | 广东省科学院半导体研究所 | Preparation method of planar TEM sample |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103776669A (en) * | 2012-10-26 | 2014-05-07 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of TEM (Transmission Electron Microscope) sample |
| CN112649624A (en) * | 2020-12-30 | 2021-04-13 | 广东省科学院半导体研究所 | Preparation method of planar TEM sample |
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Application publication date: 20220211 |