CN113834831A - Method for preparing transmission electron microscope sample - Google Patents

Method for preparing transmission electron microscope sample Download PDF

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Publication number
CN113834831A
CN113834831A CN202010513567.4A CN202010513567A CN113834831A CN 113834831 A CN113834831 A CN 113834831A CN 202010513567 A CN202010513567 A CN 202010513567A CN 113834831 A CN113834831 A CN 113834831A
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oxide layer
layer
forming
carbon film
electron microscope
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CN113834831B (en
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郑义明
杨詠钧
杨培华
谢忠诚
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Quande Technology Xiamen Co ltd
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TPK Touch Solutions Xiamen Inc
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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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The present disclosure relates to the preparation of transmission electron microscope samples, and provides a method of preparing a transmission electron microscope sample comprising: providing an initial transmission electron microscope sample, wherein the initial transmission electron microscope sample comprises a metal layer and an oxide layer, and the oxide layer is positioned on the metal layer; forming a protection structure on the upper surface of the oxide layer to obtain a transmission electron microscope sample; forming an amorphous protective layer on the upper surface of the oxide layer when the protective structure is formed on the upper surface of the oxide layer, and then forming a conductive layer on the amorphous protective layer to obtain a transmission electron microscope sample; or when the protective structure is formed on the upper surface of the oxide layer, a carbon film is formed on the upper surface of the oxide layer. In some embodiments of the present disclosure, the protection structure is formed on the oxide layer to protect the oxide layer, thereby satisfying the requirement of highly distinguishing the metal layer, the oxide layer and the conductive layer and accurately measuring the thickness of each layer.

Description

Method for preparing transmission electron microscope sample
Technical Field
The invention relates to the technical field of Transmission Electron Microscope (TEM) sample preparation, in particular to a method for reserving an oxide layer in a TEM sample and improving the resolution of each layer boundary.
Background
The transmission electron microscope is an important tool for observing microstructures, has high spatial resolution and can be accurately used for measuring the thickness of a nanometer grade. The transmission electron microscope uses a high-energy electron beam as a light source and an electromagnetic field as a lens, when the electron beam penetrates through a sample, electrons collide with atoms in the sample, and an electron image is presented according to differences of the amount of the passing electrons, scattering angles and the like. Generally, tem samples are prepared by conducting a conductive layer over the sample to help achieve clearer imaging of the sample.
If the sample is a metal material, an oxidation layer is formed on the surface of the sample due to oxidation reaction, and the oxidation layer has a significant influence on the electrical and thermal conductivity of the metal material. Therefore, accurate measurement of the thickness of each layer of the metal material, particularly the oxide layer thickness, is important for subsequent control of the properties of the finished product.
However, in the image of the tem sample prepared by the conventional method, the oxide layer often disappears after the conductive treatment of the sample, and the metal material and the conductive layer formed by the subsequent conductive treatment are difficult to distinguish under the condition that the oxide layer cannot be used as a boundary.
The thickness of each layer is accurately measured, so that the performance of the metal material can be accurately evaluated, and the properties of a finished product after processing can be mastered. Therefore, how to solve the problems that the oxide layer in the transmission electron microscope sample disappears after conducting treatment and the interface between the metal layer and the conductive layer cannot be highly resolved is a problem to be solved in the technical field of sample preparation.
Disclosure of Invention
In order to solve the above-mentioned problems that the oxide layer disappears after the conductive treatment and the interface between the metal layer and the conductive layer in the tem sample cannot be highly resolved, one aspect of the present disclosure is to provide a method for preparing the tem sample, in which a protection structure is formed on the oxide layer, so that the oxide layer can be protected, the requirements for highly resolving the metal layer, the oxide layer and the conductive layer and accurately measuring the thickness of each layer can be satisfied.
The technical scheme adopted by the disclosure is as follows: providing an initial transmission electron microscope sample, wherein the initial transmission electron microscope sample comprises a metal layer and an oxide layer, and the oxide layer is positioned on the metal layer; forming a protection structure on the upper surface of the oxide layer to obtain a transmission electron microscope sample; forming an amorphous protection layer on the upper surface of the oxide layer when the protection structure is formed on the upper surface of the oxide layer, and then forming a conductive layer on the amorphous protection layer; or forming a carbon film on the upper surface of the oxide layer when forming the protection structure on the upper surface of the oxide layer.
In some embodiments, the protective structure has a thickness between 1 and 1000 nm.
In some embodiments, the composition of the amorphous protective layer comprises carbon.
In some embodiments, the step of forming the carbon film on the upper surface of the oxide layer includes forming the carbon film on the upper surface of the oxide layer by an evaporation method.
In some embodiments, the step of forming a carbon film on the top surface of the oxide layer by evaporation comprises placing an initial tem sample in a carbon-jet evaporator chamber and performing carbon evaporation.
In some embodiments, carbon evaporation is performed for between 50 seconds and 300 seconds.
In some embodiments, the step of forming the carbon film on the upper surface of the oxide layer includes forming the carbon film on the upper surface of the oxide layer with a focused ion beam.
In some embodiments, the ion beam conditions of the focused ion beam include an acceleration voltage between 30keV and 50keV, and a size of the aperture is 80 μm.
In some embodiments, the step of forming the carbon film on the upper surface of the oxide layer by using the focused ion beam includes forming a deposition layer on the upper surface of the oxide layer by using an electron beam system, and then forming the carbon film on the deposition layer by using the focused ion beam.
In some embodiments, the step of forming the conductive layer on the amorphous protection layer or the step of forming the carbon film on the upper surface of the oxide layer comprises the following steps: cutting off a specific area of the transmission electron microscope sample to obtain a transferable area; securing the transferable region to the supporting copper sheet; and thinning the transferable region with an ion beam.
The technical scheme of the disclosure achieves the beneficial effects of avoiding the loss of the oxide layer after the transmission electron microscope sample is subjected to conductive treatment, improving the resolution of each layer interface in the transmission electron microscope sample and more accurately measuring the thickness of each layer.
Drawings
Aspects of the present disclosure are best understood from the following detailed description when read with the accompanying drawings. It is noted that, in accordance with common practice in the industry, various features are not drawn to scale. In fact, the dimensions of the various features may be arbitrarily increased or reduced for clarity of illustration and discussion.
FIG. 1 is a flow chart illustrating a method of preparing a transmission electron microscope sample, according to some embodiments of the present disclosure;
FIG. 2 is a schematic diagram illustrating a finished TEM sample prepared according to some embodiments of the present disclosure;
FIG. 3 is an image of a finished TEM sample prepared according to some embodiments of the present disclosure;
fig. 4A to 4C are component analysis images of a finished tem sample prepared according to some embodiments of the present disclosure, and fig. 4A to 4C respectively analyze different components of the same tem sample, from bottom to top, respectively a metal layer, an oxide layer, and an amorphous protection layer.
Description of the symbols
100 method for preparing transmission electron microscope sample
S110. step
S120, step
S122, step
S130, step
200 initial transmission electron microscope sample
210 metal layer
220 oxide layer
222 upper surface of
230 amorphous protective layer
240 conductive layer
250 carbon film
300 transmission electron microscope sample
Detailed Description
In order to make the objects, technical solutions and advantages of the present disclosure more apparent, the present disclosure is further described in detail below with reference to the accompanying drawings, embodiments and examples. It should be understood that the detailed description and examples described herein are intended for purposes of illustration only and are not intended to limit the scope of the claims.
Referring to fig. 1, a flowchart of a method 100 for preparing a tem sample according to some embodiments of the present disclosure is shown, including steps S110, S120, and S122, or S110 and S130.
The following is further described with reference to the embodiment of fig. 1, and please refer to fig. 2.
Fig. 2 is a schematic diagram of a finished tem sample 300, particularly including steps S110, S120, and S122, or including steps S110 and S130, according to some embodiments of the present disclosure.
In step S110, an initial tem sample 200 is provided, wherein the initial tem sample 200 includes a metal layer 210 and an oxide layer 220, and the oxide layer 220 is disposed on the metal layer 210.
In some embodiments, the material of the metal layer 210 includes a metal, particularly a metal that is easily oxidized, such as magnesium, aluminum, manganese, zinc, chromium, iron, cobalt, nickel, tin, lead, or a combination thereof, but is not limited thereto.
Next, to achieve the effect of protecting the oxide layer 220, a protection structure may be formed on the upper surface 222 of the oxide layer 220 to obtain the tem sample 300, specifically, the steps of the first embodiment (including step S120 and step S122) or the second embodiment or the third embodiment (including step S130) may be respectively adopted to obtain the tem sample 300.
In some embodiments, the thickness of the protective structure is on the order of nanometers and may be between 1 and 1000nm, such as 1nm to 100nm, 100nm to 200nm, 200nm to 300nm, 300nm to 400nm, 400nm to 500nm, 500nm to 600nm, 600nm to 700nm, 700nm to 800nm, 800nm to 900nm, or 900nm to 1000 nm. In one embodiment, the thickness of the protective structure is between 1nm and 20nm, such as between 1nm and 5nm, between 5nm and 10nm, between 10nm and 15nm, or between 15nm and 20 nm.
First, an amorphous passivation layer is formed to protect the oxide layer
In the first embodiment, referring to fig. 1 and fig. 2, after the step S110, the step S120 is continued to form an amorphous passivation layer 230 on the upper surface 222 of the oxide layer 220; then, in step S122, a conductive layer 240 is formed on the amorphous passivation layer 230 to obtain the tem sample 300.
In some embodiments, the amorphous protection layer 230 has a different composition and a different crystalline form than the metal layer 210. The amorphous passivation layer 230 is formed on the oxide layer 220 to achieve the effect of interfacial separation. In one embodiment, the composition of the amorphous protective layer 230 comprises carbon.
In some embodiments, a conductive layer 240 is formed on the amorphous protection layer 230, i.e. a conductive treatment is performed to improve the visibility and contrast, wherein the composition of the conductive layer 240 may include gold. It should be noted that the amorphous passivation layer 230 covers the oxide layer 220 to protect the oxide layer 220, so as to prevent the thickness of the oxide layer 220 from being lost due to sputtering during the conductive process for forming the conductive layer 240, which makes it difficult to observe the boundary between the metal layer 210 and the conductive layer 240 by using a transmission electron microscope.
Fig. 3 is an image of a finished tem sample 300, which is a metal layer 210, an oxide layer 220, and an amorphous passivation layer 230 from bottom left to top right, according to a first step of the present disclosure. By the method provided by the present disclosure, the boundaries between the layers can be clearly distinguished under the visual field, and the oxide layer 220 with a thickness of about 3.5nm can be clearly observed.
Fig. 4A to 4C are component analysis images of a finished tem sample 300 prepared according to a first embodiment of the present disclosure, wherein different components are analyzed by Energy-dispersive X-ray spectroscopy (Energy-dispersive X-ray spectroscopy) in the same tem sample 300. The images are respectively the metal layer 210, the oxide layer 220, and the amorphous passivation layer 230 from bottom to top, and it can be observed that the three-layered structure respectively shows three different components contained in each layer, and the oxide layer 220 is completely retained and does not disappear due to the conductive treatment.
Example II vapor deposition method for forming carbon film to protect oxide layer
Referring to fig. 1 and fig. 2, the difference between the second embodiment and the first embodiment is that, after step S110, step S130 is performed to form a carbon film 250 on the upper surface 222 of the oxide layer 220 to obtain the tem sample 300, wherein forming the carbon film 250 on the upper surface 222 of the oxide layer 220 may include forming the carbon film 250 by an evaporation method, for example, placing the tem sample 200 into a carbon-jet evaporator chamber to perform carbon evaporation. It should be noted that the carbon film 250 can serve as a protection structure to protect the oxide layer 220 from being lost due to sputtering, and in addition, the carbon film 250 has conductivity, so that the conventional conductive processing step in the preparation of the TEM sample can be replaced. That is, the tem sample 300 obtained after forming the carbon film 250 may be optionally processed (e.g., cut or thinned) in a conventional manner without forming the conductive layer 240 on the tem sample 300, and then observed by tem.
Generally, the existence of the carbon film 250 can be distinguished from the oxide layer, and one skilled in the art can adjust the carbon evaporation time according to the required thickness of the process. In one embodiment, the carbon film 250 may be greater than 10nm thick, such as between 10nm and 3 μm thick. In one embodiment, the carbon evaporation is performed for 50 seconds to 300 seconds, for example, 50 seconds to 150 seconds, or 150 seconds to 300 seconds, and the longer the carbon film is, the thicker the carbon film is. In one embodiment, the carbon deposition is performed for more than 100 seconds, such as more than 100 seconds, 110 seconds, 120 seconds, 130 seconds, 140 seconds, and 150 seconds, so as to obtain a better protection effect of the oxide layer 220.
EXAMPLE III method of Forming carbon film to protect oxide layer-focused ion Beam
The difference between the third embodiment and the second embodiment is that the second embodiment uses an evaporation method to form a carbon film, and the third embodiment forms a carbon film by a focused ion beam, and those skilled in the art can also use other methods to form a carbon film to protect the oxide layer 220 as required.
In some embodiments, the step of forming the carbon film 250 on the upper surface 222 of the oxide layer 220 includes forming the carbon film 250 on the upper surface 222 of the oxide layer 220 with a focused ion beam. In one embodiment, the focused ion beam passes through a reducing C4H10So that the carbon is densely distributed on the upper surface 222 of the oxide layer 220. In one embodiment, the ion beam conditions (beam conditions) include an acceleration voltage between 30keV and 50keV (e.g., 30keV, 40keV, or 50keV), and a beam aperture size of 80 μm. In one embodiment, the acceleration voltage for the ion beam conditions (beam condition) is 40keV and the size of the aperture is 80 μm.
In addition, in one embodiment, a deposition layer may be formed on the upper surface 222 of the oxide layer 220 by an electron beam system, and then a carbon film 250 is formed on the deposition layer by a focused ion beam, covering the oxide layer 220 with two layers, so as to achieve a better protection effect of the oxide layer 220.
In some embodiments, particularly after the step of forming the conductive layer 240 on the amorphous passivation layer 230 in the first embodiment, or after the step of forming the carbon film 250 on the upper surface 222 of the oxide layer 220 in the second or third embodiment, the method may further include the following steps: cutting off a specific region of the transmission electron microscope sample 300 to obtain a transferable region; securing the transferable region to the supporting copper sheet; and thinning the transferable region with an ion beam.
In one embodiment, the TEM sample 300 is cut using a focused ion beam with a U-shape, the beam conditions including an acceleration voltage between 30keV and 50keV (e.g., 30keV, 40keV, or 50keV), and a beam fence aperture size of 550 μm. In one embodiment, the acceleration voltage for the beam conditions (beam conditions) for cutting through the TEM sample 300 in a U-shape is 40keV and the aperture size of the aperture is 550 μm.
In one embodiment, a protective layer (e.g., tungsten) may be deposited on a portion of the surface of the transferable region to prevent loss of the upper portion of the transferable region during the subsequent thinning step, and one skilled in the art can adjust the thickness of the protective layer as desired.
In one embodiment, the transferable region is thinned by an ion beam, wherein the step of thinning the sample may be divided into several stages, including coarse thinning, fine thinning, and low voltage cleaning. In one embodiment, the ion beam conditions for coarse thinning may include an acceleration voltage between 30keV and 50keV, such as 30keV, 40keV, or 50keV, and a beam fence aperture size of 80 μm or 150 μm; the ion beam conditions for the fine thinning may include an acceleration voltage between 30keV and 50keV, such as 30keV, 40keV, or 50keV, and a beam hole size of 30 μm; ion beam conditions for low voltage cleaning may include an acceleration voltage between 2.5keV and 10keV, such as 2.5keV, 3keV, 4keV or 5keV, and a beam hole size of 80 μm.
In summary, the embodiments of the disclosure can prevent the sputtering loss or even disappearance of the oxide layer caused by the conductive treatment during the process of preparing the tem sample by forming the protection structure (such as the amorphous protection layer or the carbon film) on the oxide layer, thereby achieving the effect of protecting the oxide layer, and satisfying the requirement of highly distinguishing the metal layer, the oxide layer and the conductive layer and accurately measuring the thickness of each layer. In addition, in some embodiments, the single layer of protection structure (e.g., carbon film) can also be used as a conductive layer at the same time, i.e., a conductive process is combined, so that it is not necessary to form a conductive layer on the protection structure, thereby saving the thickness of the tem sample and the manufacturing process.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A method of preparing a transmission electron microscope sample, comprising:
providing an initial transmission electron microscope sample, wherein the initial transmission electron microscope sample comprises a metal layer and an oxide layer, and the oxide layer is positioned on the metal layer; and
forming a protective structure on the upper surface of the oxide layer to obtain the transmission electron microscope sample; wherein,
forming an amorphous protection layer on an upper surface of the oxide layer when the protection structure is formed on the upper surface of the oxide layer, and then forming a conductive layer on the amorphous protection layer; or is
When the protection structure is formed on the upper surface of the oxide layer, a carbon film is formed on the upper surface of the oxide layer.
2. The method of claim 1, wherein the protective structure has a thickness between 1 and 1000 nm.
3. The method of claim 1, wherein a component of the amorphous protective layer comprises carbon.
4. The method of claim 1, wherein forming a carbon film on the top surface of the oxide layer comprises forming the carbon film on the top surface of the oxide layer by evaporation.
5. The method of claim 4, wherein the step of depositing the carbon film on the top surface of the oxide layer comprises placing the TEM sample in a carbon-jet evaporator chamber and performing carbon evaporation.
6. The method of claim 5, wherein carbon evaporation is performed for a time between 50 seconds and 300 seconds.
7. The method of claim 1, wherein forming a carbon film on the top surface of the oxide layer comprises forming the carbon film on the top surface of the oxide layer with a focused ion beam.
8. The method of claim 7, wherein the ion beam conditions of the focused ion beam comprise an acceleration voltage between 30keV and 50keV and a size of the aperture of the optical barrier is 80 μm.
9. The method of claim 7, wherein forming the carbon film on the upper surface of the oxide layer with the focused ion beam comprises forming a deposition layer on the upper surface of the oxide layer with an electron beam system, and then forming the carbon film on the deposition layer with the focused ion beam.
10. The method of claim 1, wherein the step of forming the conductive layer on the amorphous protective layer or the step of forming the carbon film on the upper surface of the oxide layer comprises the steps of:
cutting off a specific area of the transmission electron microscope sample to obtain a transferable area;
securing the transferable region to a supporting copper sheet; and
and thinning the transferable region by using an ion beam.
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