CN111537529A - Silicon mesh for attaching transmission electron microscope sample and preparation method thereof - Google Patents
Silicon mesh for attaching transmission electron microscope sample and preparation method thereof Download PDFInfo
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- CN111537529A CN111537529A CN202010275256.9A CN202010275256A CN111537529A CN 111537529 A CN111537529 A CN 111537529A CN 202010275256 A CN202010275256 A CN 202010275256A CN 111537529 A CN111537529 A CN 111537529A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
Abstract
The application provides a silicon mesh for attaching a transmission electron microscope sample and a preparation method thereof, wherein the silicon mesh can have a set shape and comprises the following components: the preparation method comprises the following steps of: providing a semiconductor wafer, processing the wafer into a silicon substrate and an attachment part extending from the silicon substrate to form a silicon net for attaching the transmission electron microscope sample. The silicon mesh provided by the application can replace the traditional metal mesh, the quality of sample analysis is improved, and the silicon mesh as a consumable is lower in cost.
Description
Technical Field
The application relates to the technical field of preparation of transmission electron microscope samples, in particular to a silicon mesh for attaching the transmission electron microscope samples and a preparation method thereof.
Background
When a Focused Ion Beam (FIB) device is used to fabricate a Transmission Electron Microscope (TEM) sample, a consumable product, i.e., a copper mesh (Cu grid), is used in a widely used sample extraction (lift-out) process. Conventionally, samples were attached (attach) to a copper mesh and analyzed by transmission electron microscopy after fine milling (fine milling). However, in a work such as a specific failure point (fail point) composition analysis, the metal mesh material may be detected, i.e. copper element may be detected, which may cause confusion and inaccuracy of the analysis result.
Disclosure of Invention
In order to solve the problem that a metal net material can be detected in transmission electron microscope analysis, a semiconductor wafer is processed to be made into a silicon net (Si grid), and the silicon net is used as a substitute of metal nets such as a copper net, so that the problems in the prior art are well solved.
According to one or more embodiments, a silicon mesh for attaching a transmission electron microscope sample includes: a silicon substrate, and an attachment portion extending from the silicon substrate; and the attachment part is used for placing the transmission electron microscope sample.
According to one or more embodiments, a method of preparing a silicon mesh for attaching a transmission electron microscope sample, comprises the steps of: providing a semiconductor wafer; and processing the wafer into a silicon substrate and an attachment part extending from the silicon substrate to form a silicon net for attaching the transmission electron microscope sample.
The beneficial effect of this application does: the silicon mesh provided by the application can replace a metal mesh (such as a copper mesh, a molybdenum mesh or a nickel mesh), the quality of sample analysis is improved, and the cost of the silicon mesh as a consumable is lower. For example, in the composition analysis of the specific failure point (fail point), the quality of the analysis of copper element, molybdenum element, or nickel element can be significantly improved, the silicon mesh processed by using the semiconductor wafer can reduce the cost, and the cost can be reduced again by using the silicon substrate of the semiconductor wafer for debugging or damage. In addition, the method can be used for processing silicon nets in various forms in a customized manner, such as single or multiple narrow/wide columns and the like, and has the outstanding advantages that the silicon nets in complex forms can be easily processed, and the method is very suitable for a sample extraction (lift-out) process and the like.
Drawings
Fig. 1 shows a silicon mesh (five narrow columns) for attaching a transmission electron microscope sample in an embodiment of the present application.
Fig. 2 shows a silicon mesh (single wide column) for attaching a transmission electron microscope sample in the example of the present application.
Fig. 3 shows a silicon mesh (double wide column) for attaching a transmission electron microscope sample in an embodiment of the present application.
Fig. 4 is a schematic flow chart of the method for preparing the silicon mesh for attaching the transmission electron microscope sample shown in fig. 1.
Fig. 5 shows a Scanning Electron Microscope (SEM) image of the backside and narrow columns of a silicon web milled using a focused ion beam.
Fig. 6 shows a Scanning Electron Microscope (SEM) image of the back surface and wide columns of a silicon web milled using a focused ion beam.
In the figure, the position of the upper end of the main shaft,
100. a silicon substrate;
101. an attachment section;
102. a through hole;
Detailed Description
Hereinafter, embodiments of the present application will be described with reference to the accompanying drawings. It is to be understood that such description is merely illustrative and not intended to limit the scope of the present application. 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 application.
Various structural schematics according to embodiments of the present application are shown in the drawings. 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 this application, 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.
The transmission electron microscope sample Preparation (specific Preparation) technology is the most important factor influencing the detection result, and the copper mesh is an indispensable tool in the sample extraction (lift-out) process; good samples need to meet the following conditions: there must be a thin area that can be penetrated by a transmission electron microscope (thin area refers to a specific location where an observation and analysis is required), the thin area must not have contaminants or artificial impurities (artifacts), and the thin area must not have scratches.
The sample extraction (lift-out) process is to cut the sample directly in the region to be observed, and then place the sample (with thickness of tens of nanometers) on a copper net by using a micromanipulator (which is a nanometer manipulator commonly used at present). The specific steps may include: finding a region of interest, depositing a metal strip layer for protecting the cross section of the sample, such as a tungsten layer, in the region of interest, and milling two grooves on two sides of the tungsten layer to expose the sample layer to be processed; milling the center of the sample layer to reduce the thickness of the center film of the sample layer, such as to reach about 1 micron; electropolishing both sides of the central membrane, for example, to a thickness of about 0.3 microns; the central film is then subjected to a final polishing step to bring the thickness of the central film to an electronic transparency level, which may be, for example, between 50 nm and 120 nm; the film (i.e., sample) is then released from the trench, and a micromanipulator is used to control the glass needle (or so-called nanoprobe) to move the sample, and the sample is placed on a copper mesh, under the driving of the micromanipulator, the extremely narrow tip of the glass needle can realize an extremely fine motion, and the transmission electron microscope sample can be electrostatically adsorbed on the glass needle.
The nanometer manipulator (omniprobe) is a nanometer manipulator installed on a Focused Ion Beam (FIB) device and/or a Scanning Electron Microscope (SEM) device port, is operated by using a closed loop system, is completely independent of positioning of an electron microscope sample stage, and can provide extra degree of freedom for sample operation, for example, a prepared sample is accurately placed on the attachment part 101 of the silicon mesh of the application, and the nanometer manipulator has the characteristics of accuracy, flexibility, easiness in use and the like.
In the sample extraction (lift-out) process, when a sample is processed by using a focused ion beam device, a metal mesh is selected according to elements to be subjected to component analysis, the metal mesh serving as a consumable needs to be purchased periodically, although a molybdenum mesh (Mo grid) or a nickel mesh (Ni grid) can be used instead of the copper mesh, different budget costs (cost: copper mesh < molybdenum mesh < nickel mesh) are set according to different types of the metal mesh, the problems that the metal mesh elements (copper elements, molybdenum elements or nickel elements) are always detected in the copper mesh, the TEM analysis result is disordered exist, and the bad composition analysis work is difficult to perform are still existed in the copper mesh. The silicon mesh provided by the application can not only avoid the problem that the metal net element is detected, but also has lower cost; according to the method, the silicon net is manufactured in a mode of processing a wafer sample, a metal net does not need to be purchased periodically, the silicon substrate of the semiconductor wafer for debugging or damage can be used, the silicon net replaces a copper net or a molybdenum net or a nickel net, and the cost can be reduced once again.
The application develops a silicon mesh (Sigrid) which is different from a traditional copper mesh and used for attaching a transmission electron microscope sample, and the silicon mesh can be matched with a nanometer manipulator (omniprobe) arranged on Focused Ion Beam (FIB) equipment for use to finish a sample extraction (lift-out) process. In one or more embodiments of the present application, a semiconductor wafer may be used as a material; the silicon net material is silicon, including: a silicon substrate 100, and an attachment portion 101 extending from the silicon substrate, wherein the attachment portion 101 may be a convex portion above the semicircular silicon substrate 100, and the silicon substrate 100 may be a net shape; the attachment portion is used for placing a transmission electron microscope sample, and the silicon mesh may be, for example, a processed semiconductor wafer, and the wafer sample is processed into a desired shape by loading the wafer sample on a transmission electron microscope sample holder (TEM holder), and it should be understood that the silicon mesh proposed in the present application includes, but is not limited to, the shape illustrated in the drawings, and the shape of the silicon mesh may be a circular mesh, an elliptical mesh, a square mesh, or the like. The silicon mesh obtained by the method has the outstanding advantages of high success rate, high speed, low cost and the like, is suitable for being used in the preparation process of a transmission electron microscope sample, and is particularly suitable for the occasion of manufacturing the sample by a sample extraction (lift-out) process.
As shown in fig. 1, the attaching portion 101 may be a plurality of narrow pillars (narrow posts) extending from the silicon substrate 100, and when the silicon mesh has the plurality of narrow pillars, the silicon mesh is comb-shaped, and the width or thickness of each narrow pillar may be the same or different, and the plurality of narrow pillars form comb teeth of the comb-shaped silicon mesh. In the silicon substrate 100 according to one or more embodiments of the present application, the through hole 102 is formed thereon, the through hole 102 may be disposed on the left half portion of the silicon substrate 100, and of course, may also be disposed on the middle portion or the right half portion of the silicon substrate 100, and the through hole on the silicon substrate 100 may be used as a distinguishing mark for different series of products, so as to facilitate a sample analysis operator to quickly distinguish silicon nets that are similar in structure but may have different purposes.
As shown in fig. 2, the attachment portion 101 is a single wide pillar (single wide post) extending from a silicon substrate for placing a transmission electron microscope sample.
As shown in fig. 3, the attachment portion 101 is a double wide pillar (wide post) extending from a silicon substrate, and the width or thickness of the two wide pillars may be the same or different, and may be used for placing two samples of the transmission electron microscope. The silicon substrate 100, on which a through hole is formed, is disposed in the middle of the silicon substrate 100, and certainly may be disposed in the left half or the right half of the silicon substrate 100, and the shape of the through hole may be reasonably and judiciously set according to the requirement, such as a circle, a square, or a special shape.
As shown in fig. 4, in some embodiments, the present application provides a method for preparing a silicon mesh for attaching a transmission electron microscope sample, which may include the following steps: the wafer is prepared and processed, including cutting, grinding and milling the wafer, as described in detail below.
In step S1, a wafer (silicon substrate) of semiconductor wafers (Si wafers) is prepared and provided for processing into a silicon web.
In step S2, a wafer (silicon substrate) is processed by an Ultrasonic cutter (Ultrasonic cutter), and in some embodiments, the wafer may be cut to a diameter of 3 mm.
Step S3, polishing the wafer with a cutting tool (cutting tool) of a polishing machine (Polisher), which may be front polishing and/or back polishing (front/back side polishing) or single side polishing, to a predetermined thickness (t), where the predetermined thickness may be 25 μm to 35 μm or less than 30 μm, and in one or more embodiments, the thickness of the polished wafer may also be 30 μm.
Step S4, providing a designed silicon net morphology or making a silicon net morphology according to the field requirement, i.e. characteristics such as the shape of the silicon net, as shown in fig. 1 to 3 or fig. 5 to 6, as shown in fig. 5, which may be a Scanning Electron Microscope (SEM) image of the back surface and narrow columns of the silicon net milled by using a focused ion beam according to the present application; as shown in fig. 6, a Scanning Electron Microscope (SEM) image of the backside and wide columns of the silicon web, which may be milled using a focused ion beam for the present application, may be used.
In step S5, a wafer with a predetermined thickness may be loaded on a Focused Ion Beam (FIB) device having a Laser beam (Laser beam) device, and according to the above-mentioned silicon mesh form diagram, the wafer with a thickness of 25 μm to 35 μm is milled (milling) by the Focused Ion beam device, and unnecessary silicon portions are removed by milling, so that the wafer is processed into the silicon substrate 100 and the attachment portion 101 extending from the silicon substrate 100 to form a silicon mesh for attaching the transmission electron microscope sample, and the form of the silicon mesh is the same as that of the designed silicon mesh or the silicon mesh fabricated according to the field requirement, for example, the wafer may be milled into a structure having a single wide column or a double wide column or a single narrow column or multiple narrow columns by the Focused Ion beam device. Moreover, copper mesh often requires plating, whereas the silicon mesh of the present application is clearly not required; in addition, the copper mesh is easy to be damaged, but the silicon mesh provided by the application is not easy to be damaged and is more convenient to use, and the situation that the sample preparation and the detection result are influenced due to the problem of the traditional copper mesh is avoided, so that the application is favorable for improving the success rate and the efficiency of sample preparation.
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. In addition, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
The embodiments of the present application are described above. However, these examples are for illustrative purposes only and are not intended to limit the scope of the present application. The scope of the application 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 application, and such alternatives and modifications are intended to be within the scope of the present application.
Claims (10)
1. A silicon web for attaching a transmission electron microscope sample, comprising:
a silicon substrate, and
an attachment portion extending from the silicon substrate;
the attachment part is used for placing a transmission electron microscope sample.
2. The silicon web for attaching a transmission electron microscope sample according to claim 1,
the attachment portion is a plurality of narrow posts extending from the silicon substrate.
3. The silicon web for attaching a transmission electron microscope sample according to claim 2,
the silicon net is comb-shaped, and the narrow columns form comb teeth parts of the comb-shaped silicon net.
4. The silicon web for attaching a transmission electron microscope sample according to claim 1,
the attachment portion is a single wide column extending from the silicon substrate.
5. The silicon web for attaching a transmission electron microscope sample according to claim 1,
the attachment portion is a double wide column extending from the silicon substrate.
6. The silicon web for attaching a transmission electron microscope sample according to claim 1,
the silicon mesh is a processed silicon substrate for debugging or damaged semiconductor wafers.
7. The silicon web for attaching a transmission electron microscope sample according to claim 1,
the silicon substrate is provided with a through hole.
8. The silicon mesh for attaching a transmission electron microscope sample according to claim 7,
and the through holes are arranged on the left half part or the middle part or the right half part of the silicon substrate.
9. A preparation method of a silicon mesh for attaching a transmission electron microscope sample is characterized by comprising the following steps:
providing a semiconductor wafer;
and processing the wafer into a silicon substrate and an attachment part extending out of the silicon substrate to form a silicon net for attaching the transmission electron microscope sample.
10. The method for preparing a silicon mesh for attaching a transmission electron microscope sample according to claim 9,
the process of processing the wafer comprises the following steps: cutting, grinding and milling the wafer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010275256.9A CN111537529A (en) | 2020-04-09 | 2020-04-09 | Silicon mesh for attaching transmission electron microscope sample and preparation method thereof |
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| CN202010275256.9A CN111537529A (en) | 2020-04-09 | 2020-04-09 | Silicon mesh for attaching transmission electron microscope sample and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114460107A (en) * | 2020-10-22 | 2022-05-10 | 中国科学院微电子研究所 | Transmission electron microscope sample carries net |
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Inventor after: Li Deyuan Inventor after: Qu Yang Inventor after: Yu Jiahan Inventor after: Yu Fei Inventor before: Li Deyuan |