CN114252309A - Preparation method and device of transmission electron microscope sample - Google Patents
Preparation method and device of transmission electron microscope sample Download PDFInfo
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- CN114252309A CN114252309A CN202011017805.9A CN202011017805A CN114252309A CN 114252309 A CN114252309 A CN 114252309A CN 202011017805 A CN202011017805 A CN 202011017805A CN 114252309 A CN114252309 A CN 114252309A
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
- H01J37/305—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching
- H01J37/3053—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching
- H01J37/3056—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching for microworking, e.g. etching of gratings, trimming of electrical components
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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
- G01N2001/2873—Cutting or cleaving
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Abstract
The disclosure provides a method and a device for preparing a transmission electron microscope sample. The preparation method of the transmission electron microscope sample comprises the following steps: preparing a mask plate with a preset size; stacking the mask plate on a first area of the surface of a semiconductor sample; and thinning a second area on the surface of the semiconductor sample by utilizing focused ion beam cutting, wherein the second area is adjacent to the first area so as to obtain the transmission electron microscope sample with a specific thin area. The scheme has the advantages that: when the focused ion beam cuts a sample, a mask plate is adopted for protection, and the corrugated damage generated by the cutting of the focused ion beam in the new product development process can be controlled. The transmission electron microscope sample manufactured has no corrugated damage and high quality, thereby improving the problem that the image quality of the sample to be analyzed is poor, reducing the analysis period and improving the research and development efficiency.
Description
Technical Field
The disclosure relates to the technical field of semiconductors, in particular to a method and a device for preparing a transmission electron microscope sample.
Background
With the continuous reduction of the feature size of the super-large scale integrated circuit, the reliability problem of the electronic component is more and more emphasized, and the requirements of corresponding component failure analysis and semiconductor process test analysis are more and more urgent.
In the process of semiconductor process test analysis, FIB (Focused Ion beam) technology is used for TEM (Transmission electron microscope) sample preparation, such as TEM plane samples and TEM section samples. Then, TEM analysis is carried out to complete the semiconductor process test analysis work. When a sample is prepared by FIB technology, a ripple damage (rippling damage) is generated in a cross section of the sample due to a type of a sample material, an ion beam current density, an ion beam cutting height, and the like, and as shown in fig. 1, image quality of the sample to be analyzed is deteriorated.
The conventional method for improving the waviness damage caused by FIB cutting is to use a protective layer made of various materials such as platinum Pt, tungsten W, and silicon SiO2Carbon C, etc. are analyzed by special methods such as reverse bevel milling (tip milling) and low voltage milling (low kV milling), but it is difficult to make a sample because of the skill of an operator, complicated analysis steps, and increased analysis period. On the other hand, a silicon Mask (Si Mask) product commercialized by the existing patent is available only from a research and development manufacturer and is not easy to use.
Disclosure of Invention
The invention aims to provide a method and a device for preparing a transmission electron microscope sample.
The first aspect of the present disclosure provides a method for preparing a transmission electron microscope sample, including:
preparing a mask plate with a preset size;
stacking the mask plate on a first area of the surface of a semiconductor sample;
and thinning a second area on the surface of the semiconductor sample by utilizing focused ion beam cutting, wherein the second area is adjacent to the first area so as to obtain the transmission electron microscope sample with a specific thin area.
The second aspect of the present disclosure provides a device for preparing a transmission electron microscope sample, including:
the mask plate module is used for preparing a mask plate with a preset size;
the sample module is used for stacking the mask plate on a first area on the surface of a semiconductor sample; and thinning a second area on the surface of the semiconductor sample by utilizing focused ion beam cutting, wherein the second area is adjacent to the first area so as to obtain the transmission electron microscope sample with a specific thin area.
This disclosure compares advantage with prior art and lies in:
1. according to the method, the mask plate is adopted for protection when the focused ion beam cuts a sample, and the corrugated damage generated by the focused ion beam cutting in the new product research and development process can be controlled.
2. The mask plate is manufactured by using the monocrystalline silicon substrate, so that the cost is reduced.
3. The transmission electron microscope sample manufactured has no corrugated damage and high quality, thereby solving the problem that the image quality of the sample to be analyzed is poor, reducing the analysis period and improving the research and development efficiency.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the disclosure. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 shows a schematic view of a prior art corrugated lesion;
FIG. 2 shows a flow chart of a method for preparing a transmission electron microscope sample provided by the present disclosure;
fig. 3 shows a detailed operation diagram corresponding to the flowchart of fig. 2.
Detailed Description
Hereinafter, embodiments of the present disclosure will be described with reference to the accompanying drawings. It should be understood that the description is illustrative only and is not intended to limit the scope of the present disclosure. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present disclosure.
Various structural schematics according to embodiments of the present disclosure are shown in the figures. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity of presentation. The shapes of various regions, layers, and relative sizes and positional relationships therebetween shown in the drawings are merely exemplary, and deviations may occur in practice due to manufacturing tolerances or technical limitations, and a person skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions, as actually required.
In the context of the present disclosure, when a layer/element is referred to as being "on" another layer/element, it can be directly on the other layer/element or intervening layers/elements may be present. In addition, if a layer/element is "on" another layer/element in one orientation, then that layer/element may be "under" the other layer/element when the orientation is reversed.
Focused Ion Beam (FIB) is a micro-nano machining technology, the basic principle of which is similar to that of a Scanning Electron Microscope (SEM), and the ion beam emitted by an ion source is used as an incident beam after accelerated focusing, and solid atoms can be sputtered and peeled off in the process of collision between high-energy ions and solid surface atoms, so that FIB is more used as a tool for directly machining micro-nano structures. In combination with a Gas Injection System (GIS), the FIB can assist in chemical vapor deposition, positioning, induced deposition and growth of micro-nano materials and structures, or assist in selective enhanced etching of specific materials and structures.
With the continuous reduction of the feature size of the super large scale integrated circuit, the reliability problem of the electronic components is more and more emphasized, and the requirements of corresponding device failure analysis, semiconductor process test, research and development analysis are more and more urgent.
In the process of semiconductor process test analysis, TEM samples, such as TEM plane samples and TEM section samples, are prepared by using an FIB technology. Then, TEM analysis is carried out to complete the semiconductor process test analysis work. When the FIB technique is used to prepare a sample, due to the type of sample material (such as porous material, rough surface material or soft-hard composite material), the current density of the ion beam, and the cutting height of the ion beam, a wavy damage may be generated on the cross section of the sample, as shown in fig. 1, which results in the degradation of the quality of the electron microscope image of the sample to be analyzed.
In order to solve the problems in the prior art, embodiments of the present disclosure provide a method and an apparatus for preparing a transmission electron microscope sample, which are described below with reference to the accompanying drawings.
Fig. 2 shows a flowchart of a method for preparing a transmission electron microscope sample according to the present disclosure, and fig. 3 shows a detailed operation diagram corresponding to the flowchart, as shown in fig. 2 and fig. 3, the method includes the following steps:
step S101: and preparing a mask plate with a preset size.
The mask plate is used as a mask when a focused ion beam cuts a semiconductor sample so as to improve the flatness of a cutting surface.
The size of the mask plate can be set according to actual needs, and is set to be a cuboid shape with a width of 50 micrometers, a length of 100 micrometers and a height of 50 micrometers, for example.
The mask plate preparation step can be specifically realized as follows:
providing a substrate; cutting a target area of the substrate according to a preset operation flow by using a focused ion beam; and stripping the cut target area by using a sampling probe to obtain a mask plate with a preset size.
The substrate may be a single crystal silicon material, that is, a silicon substrate. The focused ion beam may contain gallium ions, i.e., a gallium ion beam, and the required equipment may employ existing FIB equipment that removes ripples generated when the thinned sample is cut by the gallium ions.
Step S102: and stacking the mask plate on a first area of the surface of the semiconductor sample. As shown in fig. 3, the mask plate superposing area is the first area.
Step S103: and thinning a second area on the surface of the semiconductor sample by utilizing focused ion beam cutting, wherein the second area is adjacent to the first area so as to obtain the transmission electron microscope sample with a specific thin area. As shown in fig. 3, by using the protection of the mask plate, ion beam cutting can be rapidly performed on a specific area of the surface of the sample, so as to obtain the transmission electron microscope sample. As can be seen from the image of the cutting surface of the electron microscope sample, the cutting surface of the electron microscope sample has no corrugated damage and has high image quality. Furthermore, after a transmission electron microscope sample is obtained, the mask plate can be quickly taken off through the sampling probe, and compared with the prior art that the protective layer is firstly covered through a complex process and then removed through the complex process, the method is simple and efficient in process steps.
The method is carried out in a way similar to the process for manufacturing the FIB-TEM test piece on the silicon surface of the semiconductor substrate, and simplifies the manufacturing process.
According to the method, due to the protection of the mask plate, when the transmission electron microscope sample is prepared by cutting with the focused ion beam, large current can be adopted, and the sample preparation efficiency is further improved.
In order to more clearly illustrate the method, the following operation flow is proposed:
1) a silicon substrate is prepared.
2) A silicon substrate was loaded on FIB equipment.
3) And carrying out ion beam cutting operation on the silicon substrate on FIB equipment under the process condition of preparing a silicon mask plate.
4) The silicon mask plate was peeled from the silicon substrate using a sampling probe on a micromanipulator.
5) A silicon mask plate is placed on a sample to be analyzed for ion beam milling.
Compared with the prior art, the embodiment has the advantages that:
1. according to the method, the mask plate is adopted for protection when the focused ion beam cuts a sample, and the corrugated damage generated by the focused ion beam cutting in the new product research and development process can be controlled.
2. The mask plate is manufactured by using the monocrystalline silicon substrate, so that the cost is reduced.
3. The transmission electron microscope sample manufactured has no corrugated damage and high quality, thereby improving the problem that the image quality of the sample to be analyzed is poor, reducing the analysis period and improving the research and development efficiency.
The embodiment of the present disclosure further provides a device for preparing a transmission electron microscope sample, the device includes:
the mask plate module is used for preparing a mask plate with a preset size;
the sample module is used for stacking the mask plate on a first area on the surface of a semiconductor sample; and thinning a second area on the surface of the semiconductor sample by utilizing focused ion beam cutting, wherein the second area is adjacent to the first area so as to obtain the transmission electron microscope sample with a specific thin area.
According to some embodiments of the present disclosure, the reticle module is specifically configured to:
providing a substrate;
cutting a target area of the substrate according to a preset operation flow by using a focused ion beam;
and stripping the cut target area by using a sampling probe to obtain a mask plate with a preset size.
According to some embodiments of the disclosure, the preset sizes are: width 50 microns, length 100 microns, height 50 microns.
According to some embodiments of the present disclosure, the substrate is a single crystalline silicon material.
According to some embodiments of the present disclosure, the focused ion beam comprises gallium ions.
As shown in fig. 3, by using the protection of the mask plate, ion beam cutting can be rapidly performed on a specific area of the surface of the sample, so as to obtain the transmission electron microscope sample. As can be seen from the image of the cutting surface of the electron microscope sample, the cutting surface of the electron microscope sample has no corrugated damage and has high image quality. Furthermore, after a transmission electron microscope sample is obtained, the mask plate can be quickly taken off through the sampling probe, compared with the prior art that the protective layer is firstly covered through a complex process and then removed through the complex process, the device is simple and efficient.
Compared with the prior art, the embodiment has the advantages that:
1. according to the method, the mask plate is adopted for protection when the focused ion beam cuts a sample, and the corrugated damage generated by the focused ion beam cutting in the new product research and development process can be controlled.
2. The mask plate is manufactured by using the monocrystalline silicon substrate, so that the cost is reduced.
3. The transmission electron microscope sample manufactured has no corrugated damage and high quality, thereby improving the problem that the image quality of the sample to be analyzed is poor, reducing the analysis period and improving the research and development efficiency.
In the above description, the technical details of patterning, etching, and the like of each layer are not described in detail. It will be appreciated by those skilled in the art that layers, regions, etc. of the desired shape may be formed by various technical means. In addition, in order to form the same structure, those skilled in the art can also design a method which is not exactly the same as the method described above. In addition, although the embodiments are described separately above, this does not mean that the measures in the embodiments cannot be used in advantageous combination.
The embodiments of the present disclosure have been described above. However, these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure. The scope of the disclosure is defined by the appended claims and equivalents thereof. Various alternatives and modifications can be devised by those skilled in the art without departing from the scope of the present disclosure, and such alternatives and modifications are intended to be within the scope of the present disclosure.
Claims (10)
1. A preparation method of a transmission electron microscope sample is characterized by comprising the following steps:
preparing a mask plate with a preset size;
stacking the mask plate on a first area of the surface of a semiconductor sample;
and thinning a second area on the surface of the semiconductor sample by utilizing focused ion beam cutting, wherein the second area is adjacent to the first area so as to obtain the transmission electron microscope sample with a specific thin area.
2. The method according to claim 1, wherein the step of preparing a mask plate of a preset size comprises:
providing a substrate;
cutting a target area of the substrate according to a preset operation flow by using a focused ion beam;
and stripping the cut target area by using a sampling probe to obtain a mask plate with a preset size.
3. The method according to claim 2, wherein the preset sizes are: width 50 microns, length 100 microns, height 50 microns.
4. The method of claim 2, wherein the substrate is a single crystal silicon material.
5. The method of claim 2, wherein the focused ion beam removes ripples generated when the thinned sample is cut by gallium ions.
6. The utility model provides a preparation facilities of transmission electron microscope sample which characterized in that includes:
the mask plate module is used for preparing a mask plate with a preset size;
the sample module is used for stacking the mask plate on a first area on the surface of a semiconductor sample; and thinning a second area on the surface of the semiconductor sample by utilizing focused ion beam cutting, wherein the second area is adjacent to the first area so as to obtain the transmission electron microscope sample with a specific thin area.
7. The apparatus according to claim 6, wherein the reticle module is specifically configured to:
providing a substrate;
cutting a target area of the substrate according to a preset operation flow by using a focused ion beam;
and stripping the cut target area by using a sampling probe to obtain a mask plate with a preset size.
8. The apparatus according to claim 7, wherein the preset dimensions are: width 50 microns, length 100 microns, height 50 microns.
9. The device of claim 7, wherein the substrate is a single crystal silicon material.
10. The apparatus of claim 7, wherein the focused ion beam removes ripples generated when the thinned sample is cut by gallium ions.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011017805.9A CN114252309A (en) | 2020-09-24 | 2020-09-24 | Preparation method and device of transmission electron microscope sample |
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| CN202011017805.9A CN114252309A (en) | 2020-09-24 | 2020-09-24 | Preparation method and device of transmission electron microscope sample |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114323827A (en) * | 2020-09-30 | 2022-04-12 | 中国科学院微电子研究所 | Preparation method and device of transmission electron microscope sample |
| CN114964590A (en) * | 2022-05-26 | 2022-08-30 | 中国工程物理研究院核物理与化学研究所 | Electronic microscopic analysis method for tritide nanoscale micro-area stress distribution |
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| CN103403520A (en) * | 2011-01-28 | 2013-11-20 | Fei公司 | Tem sample preparation |
| CN103868769A (en) * | 2014-02-21 | 2014-06-18 | 上海华力微电子有限公司 | Plane transmission electron microscope sample and preparation method thereof |
| CN104237567A (en) * | 2014-09-10 | 2014-12-24 | 武汉新芯集成电路制造有限公司 | Preparing method of ultra-thin plane transmission electron microscope sample |
| CN105241718A (en) * | 2015-10-13 | 2016-01-13 | 武汉新芯集成电路制造有限公司 | Transmission electron microscope (TEM) sample preparation method |
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Patent Citations (5)
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| KR20030046716A (en) * | 2001-12-06 | 2003-06-18 | 삼성전자주식회사 | Manufacturing Method Of Sample For TEM Analyzation |
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| CN103868769A (en) * | 2014-02-21 | 2014-06-18 | 上海华力微电子有限公司 | Plane transmission electron microscope sample and preparation method thereof |
| CN104237567A (en) * | 2014-09-10 | 2014-12-24 | 武汉新芯集成电路制造有限公司 | Preparing method of ultra-thin plane transmission electron microscope sample |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114323827A (en) * | 2020-09-30 | 2022-04-12 | 中国科学院微电子研究所 | Preparation method and device of transmission electron microscope sample |
| CN114964590A (en) * | 2022-05-26 | 2022-08-30 | 中国工程物理研究院核物理与化学研究所 | Electronic microscopic analysis method for tritide nanoscale micro-area stress distribution |
| CN114964590B (en) * | 2022-05-26 | 2023-08-18 | 中国工程物理研究院核物理与化学研究所 | Electron microscopic analysis method for tritide nano-scale micro-region stress distribution |
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