CN114429894B - Scanning imaging fixing device and method using E-T secondary electron detector - Google Patents

Scanning imaging fixing device and method using E-T secondary electron detector Download PDF

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Publication number
CN114429894B
CN114429894B CN202111538506.4A CN202111538506A CN114429894B CN 114429894 B CN114429894 B CN 114429894B CN 202111538506 A CN202111538506 A CN 202111538506A CN 114429894 B CN114429894 B CN 114429894B
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secondary electron
imaging
sample
electron detector
component
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CN114429894A (en
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戴志晖
王雷
朱钦舒
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Nanjing Normal University
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Nanjing Normal University
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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
    • H01J37/02—Details
    • H01J37/244—Detectors; Associated components or circuits therefor
    • 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
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses a scanning imaging fixing device and a method thereof by using an E-T secondary electron detector, wherein the device comprises a first component, a second component, screws and a copper mesh sample, wherein a row of locking holes and a row of grooves are arranged on the second component; the first assembly is provided with sample placement grooves, wherein copper mesh samples are placed on each sample placement groove, and screws penetrate through corresponding locking holes to fix the second assembly on the top of the first assembly. According to the method, a copper mesh transmission sample is placed in a groove-type sample stage, and a relative closed space is formed between the groove-type design and the bottom of the objective pole shoe to inhibit an E-T type secondary electron detector from obtaining surface information from the upper surface of the sample, so that the aim of scanning transmission imaging is fulfilled. The method has the advantages of simple process, good imaging effect and strong repeatability, and is suitable for various scanning electron microscopes.

Description

Scanning imaging fixing device and method using E-T secondary electron detector
Technical Field
The invention relates to a scanning electron microscope sample stage design and scanning transmission application, in particular to application of a device for obtaining scanning transmission imaging by using an E-T type secondary electron detector in scanning transmission imaging.
Background
Scanning electron microscopy is commonly used to characterize the morphology, structure and composition of solid or quasi-solid materials and has been successfully applied to many fields such as materials science, life sciences, semiconductor industry, and geological sciences.
Currently, the most complete scanning electron microscope is generally configured with a secondary electron detector in a lens barrel, a back-scattering detector and a sample bin Everhart-Thornley (E-T) secondary electron detector for high resolution surface morphology, component structure and high stereoscopic morphology observation. In addition, part of high-configuration scanning electron microscopes are also provided with high-cost telescopic semiconductor scanning transmission probes for transmission electronic signal imaging. However, the telescopic semiconductor scanning transmission probe has the problems of high equipment cost, complex operation, poor operation safety, poor time resolution, operation under the condition of 10-30kV and the like. Therefore, developing a low-cost, easy to operate, high-time resolution low-voltage transmission electron imaging method is urgent, but is also a challenge.
The E-T secondary electron detector is a detector installed in a sample bin and attracts secondary electron signals by applying positive bias to the detector surface, and is a standard configuration detector for all scanning electron microscopes. The technology is developed. At present, few reports about the use of an E-T type secondary electron detector for scanning transmission imaging exist, and particularly, the research on scanning transmission imaging under the low voltage condition of below 5kV is not yet reported.
Disclosure of Invention
In order to solve the problems, the invention discloses a scanning imaging fixing device and a scanning imaging fixing method which are obtained by using an E-T type secondary electron detector, and a scanning transmission imaging effect is obtained under a low voltage condition by a method for blocking the E-T type secondary electron detector.
The scanning imaging fixing device is obtained by using an E-T secondary electron detector and comprises a first component, a second component, screws and a copper mesh sample, wherein a row of locking holes and a row of grooves are formed in the second component; the first assembly is provided with sample placement grooves, wherein copper mesh samples are placed on each sample placement groove, and screws penetrate through corresponding locking holes to fix the second assembly on the top of the first assembly.
The invention is further improved in that: a convex ring is arranged at the bottom of each groove; each convex ring is suitably matched with the sample placing groove card; the aperture of each groove is gradually reduced from top to bottom.
The invention is further improved in that: the bottom of the first assembly is mounted with nails or cylinders.
The scanning transmission imaging method is obtained by using an E-T type secondary electron detector, and is characterized in that: the method comprises the following steps:
step 1: placing a copper mesh sample on a sample placement groove of a fixing device on a first component; fixing a second component on the first component through screws;
step 2: the fixing device with the copper mesh sample in the step 1 is as close to the bottom of the objective pole shoe as possible, and an E-T type secondary electron detector is used for imaging;
step 3: and (3) the distance between the fixing device and the bottom of the objective pole shoe is increased, and secondary electron imaging or mixed signal imaging is obtained by using an E-T type secondary electron detector.
And obtaining the component contrast imaging by using a back scattering electron detector in the lens barrel.
Wherein the condition in the sample compartment can be observed in real time by an infrared camera or the like at the time of imaging.
According to the invention, the copper mesh sample is fixedly arranged in the device through the screw. The detection and collection of secondary electrons by the E-T type secondary electron probe are restrained by matching the groove depth design on the second component with a smaller working distance, and the transmission electrons below the sample are collected so as to achieve the purpose of scanning transmission imaging.
The invention aims to provide a method for obtaining scanning transmission imaging by using an E-T type secondary electron detector. The method adopts a designed groove-type copper mesh sample stage, can be seen in fig. 1-10, obtains scanning transmission imaging effect under low voltage condition by blocking the method of detecting secondary electrons by an E-T detector, has simple process, good imaging effect and strong repeatability, and is suitable for various scanning electron microscopes.
The invention has the beneficial effects that: the groove-type copper mesh sample stage is designed, the scanning transmission imaging effect is obtained under the low-voltage condition by the method of restraining secondary electrons detected by the E-T detector, the process is simple, the transformation of an optical path and a vacuum system of an electron microscope is not needed, the imaging effect is excellent, the repeatability is high, and the method is suitable for various scanning electron microscopes. The imaging effect of the low-voltage scanning transmission imaging effect and the imaging effect of other detectors of the device are examined. Compared with a commercial scanning transmission detector, the imaging method can be used for scanning transmission imaging under lower voltage, and the time resolution is superior to that of the commercial scanning transmission detector. With respect to light sensitive commercial semiconductor detectors,
drawings
Fig. 1 is an assembled schematic view and top view of the scanning transmission imaging device of the present invention.
Fig. 2 is an assembled schematic diagram and side view of a scanning transmission imaging device according to the present invention.
Fig. 3 is an assembled half-sectional view of a scanning transmission imaging apparatus according to the present invention, in a first direction.
Fig. 4 is an assembled half-sectional view of the scanning transmission imaging device of the present invention, in the second direction.
Fig. 5 is an exploded view of a scanning transmission imaging apparatus according to the present invention.
Fig. 6 is a top view of the assembly 1 of fig. 1.
Fig. 7 is a bottom view of the assembly 1 of fig. 1.
Fig. 8 is a half cross-sectional view of the assembly 1 of fig. 1.
Fig. 9 is a top view of the assembly 2 of fig. 1.
Fig. 10 is a bottom view of the assembly 2 of fig. 1.
FIG. 11 shows the scan transmission imaging of Nb at 800V according to the present invention 2 O 5 Imaging of graphene composites.
FIG. 12 shows Nb obtained at a working distance of 9.9mm using the apparatus of the present invention 2 O 5 Mixed signal imaging of graphene composite material.
Fig. 13 shows secondary electron imaging results of cu@c composite material using an in-barrel secondary electron detector using the apparatus of the present invention.
Fig. 14 shows the result of back-scattered electron imaging of cu@c composite material using a back-scattered electron detector in a lens barrel using the apparatus of the present invention.
Fig. 15 is a schematic diagram and a plan view of an apparatus suitable for scanning transmission imaging of electronic brand electron microscopes in japan.
Fig. 16 is a schematic view of an apparatus for scanning transmission imaging suitable for electronic brand electron microscopy in japan, a bottom view.
Fig. 17 is a schematic diagram and side view of an apparatus suitable for scanning transmission imaging of a Hitachi brand electronic microscope.
Fig. 18 is a setup flow chart of the present invention.
Detailed Description
The present invention is further illustrated in the following drawings and detailed description, which are to be understood as being merely illustrative of the invention and not limiting the scope of the invention. It should be noted that the words "front", "rear", "left", "right", "upper" and "lower" used in the following description refer to directions in the drawings, and the words "inner" and "outer" refer to directions toward or away from, respectively, the geometric center of a particular component.
The embodiment provides a scanning imaging fixing device and a method for obtaining the scanning imaging fixing device by using an E-T type secondary electron detector,
the schematic structural diagram of the scanning imaging fixing device obtained by using the E-T secondary electron detector can be seen from fig. 1 to 10, and the scanning imaging fixing device comprises a first component 1, a second component 2, screws 3 and a copper mesh sample 4, wherein a row of locking holes 5 and a row of grooves 6 are arranged on the second component 2; the first assembly 1 is provided with sample placement grooves 7, wherein a copper mesh sample 4 is placed on each of the sample placement grooves 7, and wherein screws 3 pass through corresponding locking holes 5 to fix the second assembly 2 on top of the first assembly 1.
The detection and collection of secondary electrons by the E-T type secondary electron probe are inhibited by designing and matching a groove 6 with the depth of 1.8mm on the second component 2 with a smaller working distance, and the transmission electrons below the sample are collected so as to achieve the purpose of scanning transmission imaging.
Example 1E-T type secondary electron detector scanning transmission imaging.
The installed fixing device is arranged in a scanning electron microscope, the working distance is adjusted to be about 3.2mm, and the distance between the top of the device and the bottom of a pole shoe of the objective lens is about 1.4mm. At this time, nb can be obtained by using an E-T type secondary electron detector under a low voltage condition of 800V 2 O 5 Graphene composite scanning transmission imaging (as shown in fig. 11).
Example 2E-T secondary electron detector secondary electrons and transmission electrons were imaged in a hybrid.
The installed fixing device is arranged in a scanning electron microscope, the working distance is adjusted to be about 9.9mm, and the distance between the top of the device and the bottom of the pole shoe of the objective lens is about 8.1mm. At this time, the E-T type secondary electron detector detects a mixed signal of a proportion of the transmitted electrons and the secondary electron signal of the upper surface. As shown in FIG. 12, under the condition of 5kVObtained Nb 2 O 5 Mixed signal imaging of graphene composite material.
Example 3 in-barrel secondary electron detector imaging.
And (3) placing the mounted fixing device in a scanning electron microscope, and performing secondary electron imaging by using a secondary electron detector in the lens barrel. As shown in fig. 13, a surface topography image of the material can be obtained.
Example 4 in-barrel backscattered electron detector imaging.
And (3) the installed fixing device is arranged in a scanning electron microscope, and back scattering electron imaging is carried out by using a back scattering electron detector in the lens barrel. As shown in fig. 14, a component contrast imaging of the material may be obtained.
Example 5 simple modification of the first Assembly 1, as shown in FIGS. 15-16, mounted to a Japanese electronic branded electronic microscope
The scanning transmission imaging fixing device obtained by using an E-T type secondary electron detector under the first component 1 in fig. 1 is installed on a Japanese Electron (JEOL) brand electron microscope, and imaging is performed by using a sample bin secondary electron detector.
Example 6 simple modification of first Assembly 1, mounting to Hitachi brand electronic microscope
The nail below the first component 1 in fig. 1 was replaced with an M4 internal thread, as shown in fig. 17, mounted on a hitachi (Hitaichi) brand electron microscope, and imaged with a sample bin secondary electron detector.
The E-T type detector is light interference resistant, and the condition in the sample bin can be observed in real time through an infrared camera and the like during imaging. The groove type device has the advantages of low price, simple operation, capability of installing 6 copper mesh samples at one time and the like, and is expected to replace a commercial tungsten filament scanning transmission accessory. At present, low-voltage scanning transmission imaging obtained by the E-T type secondary electron detector is not reported yet, and the E-T type secondary electron detector has important application prospect in the field of scanning electron microscope transmission imaging.
The technical means disclosed by the scheme of the invention is not limited to the technical means disclosed by the embodiment, and also comprises the technical scheme formed by any combination of the technical features.

Claims (5)

1. The scanning transmission imaging fixing device is obtained by using an E-T type secondary electron detector and is characterized in that: the copper mesh sample locking device comprises a first component (1), a second component (2), screws (3) and a copper mesh sample (4), wherein a row of locking holes (5) and a row of grooves (6) are formed in the second component (2); the first assembly (1) is provided with sample placing grooves (7), wherein a copper mesh sample (4) is placed on each sample placing groove (7), and a screw (3) penetrates through a corresponding locking hole (5) to fix the second assembly (2) on the top of the first assembly (1); the bottom of each groove (6) is provided with a convex ring (8); each convex ring (8) is matched with the sample placing groove (7) in a clamping mode; the aperture of each groove (6) gradually reduces from top to bottom.
2. The scanning transmission imaging fixture obtained with an E-T type secondary electron detector as set forth in claim 1, wherein: the vertical straight depth of the groove (6) is 1.8mm.
3. The scanning transmission imaging fixture obtained with an E-T type secondary electron detector as set forth in claim 1, wherein: nails or cylinders are mounted at the bottom of the first component (1).
4. The scanning transmission imaging method using an E-T type secondary electron detector according to claim 1, wherein: the method comprises the following steps:
step 1: placing the copper mesh sample (4) on a sample placement groove (7) of the fixing device on the first component (1); fixing the second component to the first component (1) by means of screws (3);
step 2: raising the fixing device with the copper mesh sample (4) in the step 1 until the distance from the fixing device to the bottom of the objective pole shoe is less than or equal to 3.5 mm, and imaging by using an E-T type secondary electron detector;
step 3: and adjusting the distance between the fixing device and the bottom of the objective pole shoe to be less than or equal to 10 mm, and obtaining secondary electron imaging or mixed signal imaging by using an E-T type secondary electron detector.
5. A scanning transmission imaging method according to claim 4, obtained with an E-T type secondary electron detector, characterized in that: and obtaining the component contrast imaging by using a back scattering electron detector in the lens barrel.
CN202111538506.4A 2021-12-15 2021-12-15 Scanning imaging fixing device and method using E-T secondary electron detector Active CN114429894B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201142313Y (en) * 2008-01-17 2008-10-29 中国热带农业科学院分析测试中心 Collector of scanning electron microscope example bench
CN202930353U (en) * 2012-11-27 2013-05-08 郑州大学 SEM sample bench allowing same-plane testing of samples with different thickness
KR102029869B1 (en) * 2018-06-19 2019-10-08 한국표준과학연구원 Detachable Sample Chamber for Electron Microscope and Electron Microscope Comprising The Same
CN112782198A (en) * 2020-12-07 2021-05-11 上海大学 Multi-equipment combined three-dimensional atom probe sample universal interface device
CN214477325U (en) * 2021-05-06 2021-10-22 宁波新材料测试评价中心有限公司 Scanning electron microscope sample stage

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201142313Y (en) * 2008-01-17 2008-10-29 中国热带农业科学院分析测试中心 Collector of scanning electron microscope example bench
CN202930353U (en) * 2012-11-27 2013-05-08 郑州大学 SEM sample bench allowing same-plane testing of samples with different thickness
KR102029869B1 (en) * 2018-06-19 2019-10-08 한국표준과학연구원 Detachable Sample Chamber for Electron Microscope and Electron Microscope Comprising The Same
CN112782198A (en) * 2020-12-07 2021-05-11 上海大学 Multi-equipment combined three-dimensional atom probe sample universal interface device
CN214477325U (en) * 2021-05-06 2021-10-22 宁波新材料测试评价中心有限公司 Scanning electron microscope sample stage

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