CN113758955A - Method for observing sample without conducting layer on surface by using scanning electron microscope - Google Patents
Method for observing sample without conducting layer on surface by using scanning electron microscope Download PDFInfo
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- CN113758955A CN113758955A CN202010484280.3A CN202010484280A CN113758955A CN 113758955 A CN113758955 A CN 113758955A CN 202010484280 A CN202010484280 A CN 202010484280A CN 113758955 A CN113758955 A CN 113758955A
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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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/225—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 measuring secondary emission from the material using electron or ion
- G01N23/2251—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 measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/102—Different kinds of radiation or particles beta or electrons
Abstract
The present disclosure relates to a method for observing a sample having a surface free of a conductive layer using a scanning electron microscope, comprising the steps of: providing a sample, wherein the sample comprises the nano silver wire, and the surface of the sample is free of the conductive layer; fixing a sample on a sample stage of a scanning electron microscope; adjusting parameters of the scanning electron microscope, including an accelerating voltage of between 0.5kV and 3 kV; and observing the sample, wherein an image of the nano silver wire is displayed under the visual field. The method of the disclosure improves the resolution of observing the nano silver lines in the poor conductivity sample through the scanning electron microscope, saves the pretreatment process (such as conductive treatment) and time of the conventional poor conductivity sample, avoids the interference of the surface conductive layer, and directly observes a more real appearance of the nano silver lines.
Description
Technical Field
The invention relates to the field of Scanning Electron Microscope (SEM) observation, in particular to a method for observing nano silver wires in a sample with poor conductivity without conducting treatment.
Background
When a scanning electron microscope is used for observing a sample, incident electrons are emitted through a cathode, after the incident electrons reach the surface of the sample through acceleration, a series of physical signals are excited, and a probe (or called a detector) receives secondary electron and back scattered electron signals to obtain microstructure information of the sample.
Although the nano silver wire is a conductive material, when the nano silver wire is coated in a non-conductive organic material and the surface of the nano silver wire is covered by a non-conductive protective layer, the nano silver wire becomes a poor conductive sample.
If a poor conductive sample is observed by using a scanning electron microscope (see figure 1), incident electrons are continuously accumulated on the surface of the sample, a negative surface electric field is enhanced, the incident electrons are repelled, secondary electrons are deflected, the electric field on the surface of the sample is unstable, a serious charge effect is generated, white or black areas with abnormal contrast appear in an image, even distortion and irregular stripes are generated, and the observation quality is seriously influenced.
For the observation of poor conductivity samples, a continuous conductive layer is generally plated on the surface of the sample, but no matter which conductive material is plated as the conductive layer, the conductive layer can cover the real micro-morphology to a certain extent.
Therefore, how to observe the nano silver wires in the sample with poor conductivity by using a scanning electron microscope without plating a conductive layer is a problem to be solved.
Disclosure of Invention
In order to achieve the objective of observing the nano silver wires in the sample with poor conductivity without plating the conductive layer, one aspect of the present disclosure is a method for observing the sample without the conductive layer on the surface by using a scanning electron microscope, comprising the following steps: providing a sample, wherein the sample comprises a silver nanowire and the surface of the sample is free of a conductive layer; fixing the sample on a sample stage of a scanning electron microscope; adjusting the parameters of the scanning electron microscope to make the accelerating voltage between 0.5kV and 3 kV; and observing the sample, and displaying the image of the nano silver wire under the visual field.
The technical scheme of the disclosure achieves the beneficial effects of improving the resolution of the nano silver wire in the poor conductivity sample observed through the scanning electron microscope, saving the pretreatment process (such as conductive treatment) and time of the conventional poor conductivity sample, avoiding the interference of the surface conductive layer and directly observing the more real appearance of the nano silver wire.
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 shows an image of a sample without a conductive layer sputtered on the surface, with the acceleration voltage of a scanning electron microscope set at 10kV, wherein the surface of the sample does not contain the conductive layer;
FIG. 2 is a flow chart illustrating a method of observing a sample having a surface that is free of a conductive layer, according to some embodiments of the present disclosure;
FIGS. 3A and 3B are images of a SEM at a working distance of 8.0 mm and at different acceleration voltages, wherein the acceleration voltage of FIG. 3A is 1.0kV and the acceleration voltage of FIG. 3A is 0.7kV, according to some embodiments of the present disclosure;
FIGS. 4A and 4B are diagrams illustrating adjusting images of a Hitachi cold field scanning electron microscope in different electron reception modes at a working distance of 8.0 mm and an acceleration voltage of 0.7kV, in which FIG. 4A is a diagram illustrating the probe receiving secondary electron signals, and FIG. 4B is a diagram illustrating the adjustment of the plate voltage on the objective lens to-75 volts (SE (LA50)), according to some embodiments of the present disclosure;
FIGS. 5A and 5B are images of a SEM at different working distances, with FIG. 5A being at a working distance of 8 mm and FIG. 5B being at a working distance of 2.5 mm, according to some embodiments of the present disclosure;
FIGS. 6A and 6B are images of a Hitachi Cold field scanning Electron microscope in the increased decelerating electric field mode at a working distance of 2.5 mm, an accelerating voltage of 2.2kV, a decelerating voltage of 1.5kV, and a plate voltage on the objective lens adjusted to-75 volts (SE (LA50)), according to some embodiments of the present disclosure;
fig. 7A-7C are images showing observation of a sample including silver nanowires of different diameters using a Hitachi cold field scanning electron microscope in an increased decelerating electric field mode with a working distance of 2.5 mm, an accelerating voltage of 2.2kV, a decelerating voltage of 1.5kV, and a plate voltage on an objective lens adjusted to-75 volts (SE (LA50)), wherein the silver nanowires in fig. 7A have a diameter between 20 nm and 30 nm, the silver nanowires in fig. 7B have a diameter between 12.5 nm and 20 nm, and the silver nanowires in fig. 7C have a diameter between 10 nm and 15 nm, according to some embodiments of the present disclosure.
Description of the symbols
100 method for observing sample without conducting layer on surface by using scanning electron microscope
S110. step
S120, step
S130, step
S140 step
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. 2, a method 100 for observing a sample without a conductive layer on a surface by using a scanning electron microscope according to some embodiments of the present disclosure includes steps S110 to S140.
First, step S110 is performed to provide a sample, in some embodiments, the sample includes a nano silver wire, the sample is a poor conductive sample, and the surface of the sample does not include a conductive layer. In some embodiments, the surface of the sample is covered with a protective layer, and the material of the protective layer may include a non-conductive organic material, and the silver nanowires are not directly exposed to the surface of the sample through the isolation of the protective layer. In some embodiments, the nanosilver lines are formed on a non-conductive substrate (e.g., an organic material). In some embodiments, the nanosilver wire has a diameter between 10 nanometers and 30 nanometers, such as between 10 nanometers and 20 nanometers, or between 20 nanometers and 30 nanometers.
Next, step S120 is performed to fix the sample on the sample stage of the scanning electron microscope. In some embodiments, the scanning electron microscope may comprise a Hitachi cold field scanning electron microscope, wherein the model may comprise, for example, S-4800, Regulus8200 series (Regulus8220, Regulus8230, or Regulus8240), or Regulus 8100. In some embodiments, the sample is in a sheet-like structure of 1 cm x 1 cm. In some embodiments, the sample can be fixed to the sample stage using a double-sided carbon conductive adhesive. In some embodiments, liquid nitrogen can be added into the cold trap, so as to improve the vacuum degree of the equipment of the scanning electron microscope and reduce the pollution of the equipment and the sample.
Then, in step S130, the parameters of the scanning electron microscope are adjusted to make the accelerating voltage between 0.5kV and 3kV, such as 0.5kV, 0.7kV, 1kV, 1.5kV, 2kV, 2.2kV, 3kV or any of the above two values. Next, step S140 is performed to observe the sample, and the image of the nano-silver wire is displayed under the visual field, in some embodiments, a slow-scan shooting mode may be used to improve the resolution of the shot image. Generally, when a sample with a conductive surface is observed by using an electron microscope, under the control of proper parameters, the acceleration voltage is at least higher than 10kV, so that a clear image can be observed. If a poor conductive sample is observed, the higher the acceleration voltage is, the higher the charge effect is, and the image is interfered. Therefore, the acceleration voltage should be reduced to below 10kV, for example, between 0.5kV and 3kV (including but not limited to 0.5kV, 0.7kV, 1kV, 2kV, 2.5kV, 3kV, or any of the above values), so as to improve the resolution of the silver nanowires in the poor conductive sample. In one embodiment, referring to fig. 3A and 3B, fig. 3A and 3B show the images of the silver nanowires observed under the same parameters of the sem (including the working distance of 8.0 mm) when the acceleration voltage is 1.0kV and 0.7kV, respectively, and the lower the acceleration voltage, the sharper the image.
In some embodiments, after the step of adjusting the acceleration voltage to be between 0.5kV and 3kV, the step of performing an electronic-optical system alignment is further included, where the electronic-optical system alignment refers to adjusting mechanical or electrical parameters so that optical axes of parts (e.g., components such as an electron gun or a lens) in the electronic-optical system are aligned on the same axis. In one embodiment, the optical system axis comprises electron beam electrical centering, diaphragm electrical centering, astigmatic X/Y electrical centering, or a combination thereof.
In some embodiments, the step of adjusting the parameters of the sem further comprises adjusting a mode of receiving backscattered Electrons and Secondary Electrons to a setting capable of receiving both backscattered Electrons and Secondary Electrons, wherein Secondary Electrons (SE) are free Electrons that escape from the surface of the sample atom after excitation of outer Electrons by the incident Electrons, and backscattered Electrons (BSE) are part of incident Electrons that escape from the surface of the sample atom after collision with the sample atom and elastic and inelastic scattering occurs. It should be emphasized that reducing the secondary electron signal, increasing the receiving ratio of the backscattered electrons, or both, will avoid the charging effect and increase the resolution of the image of the silver nanowires in the poor conductive sample. In some embodiments, for example, in Hitachi cold field scanning electron microscope, the plate voltage of the objective lens may be set to any value within 0 to-150V (SE (LA0) to SE (LA100)) depending on the diameter of the nano-silver wire, for example, the plate voltage may be set to 0V, -45V, -75V, -105V, -150V, or any range thereof, so as to obtain a clear image. In one embodiment, please refer to fig. 4A and 4B, fig. 4A and 4B show images obtained by adjusting different electron receiving modes under the same conditions of the same parameters (working distance is 8.0 mm and accelerating voltage is 0.7kV) in a Hitachi cold field scanning electron microscope, wherein fig. 4A is an se (u) mode in which the plate voltage on the objective lens is +50 v, and in this setting, the upper probe only receives secondary electron signals; in fig. 4B, compared to fig. 4A, the receiving of the backscattered electrons is added, and the plate voltage on the objective lens is adjusted to the SE (LA50) mode of-75 v, so that the backscattered electrons and the secondary electrons can be received simultaneously, and the image comparison result shows that when the mode is set to SE (LA50), the image of the silver nanowire is clearer.
In some embodiments, the step of adjusting the parameters of the sem further comprises adjusting the working distance to be between 1.5 mm and 3 mm, for example, 1.5 mm, 2 mm, 2.5 mm, 3 mm, or any interval of the two. The working distance is reduced, so that the sample can be close to the sample, and the image of the nano silver wire is clearer. In one embodiment, referring to fig. 5A and 5B, under the condition that other parameters are fixed, when the working distance of fig. 5A is 8 mm and the working distance of fig. 5B is 2.5 mm, the shorter the working distance is, the clearer the image is.
In some embodiments, in the step of adjusting the parameters of the sem, if the surface of the sample is flat, the deceleration electric field mode may be directly increased without tilting the sample stage, wherein the values of the acceleration voltage and the deceleration voltage are set such that the difference between the acceleration voltage and the deceleration voltage (also referred to as the landing voltage) is between 0.7kV and 1.5kV, for example, 3kV and 2.3kV, 3kV and 1.5kV, 2.2kV and 0.7kV, or 2.2kV and 1.5 kV. In one embodiment, when the deceleration electric field mode is increased, the upper probe is selected for use by the probe, so that the influence of different electronic signal ratio differences on the image can be reduced, and the definition of the image can be improved.
In some embodiments, adjusting the parameters of the sem further comprises selecting a suitable probe, an electronic signal receiving mode, and an electric field mode, and adjusting parameters such as a focal length, a working distance, a brightness, and a contrast to observe a clear image.
In some embodiments, the parameters for improving the resolution of the silver nanowires in the poor conductivity sample, including but not limited to acceleration voltage, deceleration voltage, backscattered electrons, secondary electrons, working distance, or the selection of the probe, can be set to obtain a clearer image of the silver nanowires. In one embodiment, please refer to fig. 6A and 6B, which are images of SE (LA50) mode in which a decelerating electric field mode is added in a Hitachi cold field scanning electron microscope, and a working distance is set to be 2.5 mm, an accelerating voltage is set to be 2.2kV, a decelerating voltage is set to be 1.5kV, and a plate voltage on an objective lens is set to be-75 v. Compared with the method of adjusting only a single parameter (for example, fig. 3A, only setting the acceleration voltage to 1kV, and not setting the SE (LA50) mode, the set-down working distance, or the newly added deceleration electric field mode), setting a plurality of parameters that can improve the resolution at the same time, the observed nano silver lines will be clearer. In addition, referring to fig. 7A to 7C, fig. 7A to 7C show images of different widths of the silver nanowires in the poor conductivity sample according to the same parameter settings as fig. 6A and 6B, wherein the diameter of the silver nanowires in fig. 7A is between 20 nm and 30 nm, the diameter of the silver nanowires in fig. 7B is between 12.5 nm and 20 nm, and the diameter of the silver nanowires in fig. 7C is between 10 nm and 15 nm. That is, in one embodiment of the present disclosure, by setting the adjustment parameters, the poor conductivity sample can clearly observe the internal nano-silver wire and the microscopic topography of the surface of the nano-silver wire without the surface conductive layer treatment, wherein the diameter of the nano-silver wire may be, for example, less than 15 nm, 20 nm, 30 nm, 40 nm, 50 nm, 60 nm or between the two values, or between 10 nm and 60 nm (e.g., between 20 nm and 30 nm, between 12.5 nm and 20 nm, or between 10 nm and 15 nm).
In summary, the embodiments of the present disclosure provide a method for observing a nano silver line inside a poor conductivity sample by using a scanning electron microscope, and by optimizing operation parameters (an acceleration voltage, a deceleration voltage, backscattered electrons, secondary electrons, a working distance, and a probe), a resolution is greatly improved, so that the internal nano silver line can be clearly observed by the scanning electron microscope without conducting the poor conductivity sample, and a conventional pretreatment process and time of the poor conductivity sample are saved. In addition, the interference of the surface conducting layer can be eliminated, and the more real appearance of the nano silver wire can be observed.
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 for observing a sample without a conductive layer on the surface by using a scanning electron microscope, which is characterized by comprising the following steps:
providing a sample, wherein the sample comprises a nano silver wire, and one surface of the sample does not contain a conductive layer;
fixing the sample on a sample stage of a scanning electron microscope;
adjusting parameters of the scanning electron microscope, including adjusting an accelerating voltage between 0.5kV and 3 kV; and
observing the sample, and displaying the image of the nano silver wire under the visual field.
2. The method of claim 1, wherein the nanosilver wire has a diameter of between 10 nm and 30 nm.
3. The method of claim 1, wherein the silver nanowires are formed on a non-conductive substrate.
4. The method of claim 1, wherein the surface of the sample is covered with a protective layer, the protective layer being made of a non-conductive organic material.
5. The method of claim 1, further comprising performing electron-optical system alignment after the step of bringing the acceleration voltage between 0.5 and 3 kV.
6. The method of claim 1, wherein the step of adjusting the parameters of the sem further comprises adjusting a mode of receiving backscattered electrons and secondary electrons to a setting that allows for simultaneous reception of backscattered electrons and secondary electrons.
7. The method of claim 6, wherein the setting to receive both backscattered and secondary electrons simultaneously comprises adjusting a plate voltage on the objective lens to between 0 and-150 volts.
8. The method of claim 1, wherein the step of adjusting the parameters of the sem further comprises adjusting a working distance to between 1.5 mm and 3 mm.
9. The method of claim 1, wherein the step of adjusting the parameters of the sem further comprises increasing a deceleration electric field pattern and setting values of the acceleration voltage and the deceleration voltage such that a difference between the acceleration voltage and the deceleration voltage is between 0.7kV and 1.5 kV.
10. The method of claim 9, wherein the step of adding a retarding electric field pattern comprises adjusting a probe to be an upper probe.
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Citations (5)
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| US20060011834A1 (en) * | 2004-07-13 | 2006-01-19 | Masako Nishimura | Low vacuum scanning electron microscope |
| US20080203301A1 (en) * | 2007-02-28 | 2008-08-28 | Hitachi High-Technologies Corporation | Electron Microscope |
| JP2011258573A (en) * | 2011-08-26 | 2011-12-22 | Hitachi High-Technologies Corp | Charged particle beam device |
| CN103733299A (en) * | 2011-09-07 | 2014-04-16 | 株式会社日立高新技术 | Scanning electron microscope |
| US20200234914A1 (en) * | 2017-11-21 | 2020-07-23 | Focus-Ebeam Technology (Beijing) Co., Ltd. | Low voltage scanning electron microscope and method for specimen observation |
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2020
- 2020-06-01 CN CN202010484280.3A patent/CN113758955A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060011834A1 (en) * | 2004-07-13 | 2006-01-19 | Masako Nishimura | Low vacuum scanning electron microscope |
| US20080203301A1 (en) * | 2007-02-28 | 2008-08-28 | Hitachi High-Technologies Corporation | Electron Microscope |
| JP2011258573A (en) * | 2011-08-26 | 2011-12-22 | Hitachi High-Technologies Corp | Charged particle beam device |
| CN103733299A (en) * | 2011-09-07 | 2014-04-16 | 株式会社日立高新技术 | Scanning electron microscope |
| US20200234914A1 (en) * | 2017-11-21 | 2020-07-23 | Focus-Ebeam Technology (Beijing) Co., Ltd. | Low voltage scanning electron microscope and method for specimen observation |
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| 戎咏华等: ""碳纳米管的结构、性能、合成及其应用"", vol. 1, 上海交通大学出版社, pages: 106 - 107 * |
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