CN113299529B - Secondary electron probe and high-temperature scanning electron microscope - Google Patents
Secondary electron probe and high-temperature scanning electron microscope Download PDFInfo
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- CN113299529B CN113299529B CN202110563286.4A CN202110563286A CN113299529B CN 113299529 B CN113299529 B CN 113299529B CN 202110563286 A CN202110563286 A CN 202110563286A CN 113299529 B CN113299529 B CN 113299529B
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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
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
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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
- H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
- H01J37/06—Electron sources; Electron guns
- H01J37/073—Electron guns using field emission, photo emission, or secondary emission electron sources
Abstract
The invention discloses a secondary electron probe and a high-temperature scanning electron microscope, wherein the secondary electron probe comprises a high-pressure electron tube, the high-pressure electron tube comprises an inner collecting layer and an outer collecting layer which are oppositely arranged, the outer collecting layer is arranged on the inner collecting layer in a circumferential angle-adjustable manner, a gap is formed between the inner collecting layer and the outer collecting layer, a plurality of electron collecting holes are uniformly distributed on the inner collecting layer and the outer collecting layer, the electron collecting holes on the inner collecting layer and the outer collecting layer are correspondingly arranged, a shielding part is arranged between every two adjacent electron collecting holes, and the area of the shielding part is not smaller than that of the electron collecting holes which are oppositely arranged on the inner collecting layer or the outer collecting layer. Under the normal atmospheric temperature environment, the electron collecting hole on interior collecting layer and the outer collecting layer is relative, and the at utmost collects secondary electron, under the high temperature environment, rotates outer collecting layer to the state that shielding portion sheltered from the electron collecting hole on with the interior collecting layer completely to shelter from a large amount of visible light and infrared ray, avoid the influence of visible light and infrared ray.
Description
Technical Field
The invention relates to the technical field of electron microscopes, in particular to a secondary electron probe and a high-temperature scanning electron microscope.
Background
With the rapid development of material science and technology, how to represent various physical, chemical and mechanical properties of materials, structures and devices under the action of a high-temperature field from a microscopic perspective becomes a leading research edge and a hotspot in the technical field of material science, so that the research of the test system based on the high-temperature scanning electron microscope is particularly important in the aspect of seeking new materials, new technologies and new processes.
Under the high-temperature environment, a large amount of visible light and infrared rays are generated by a tested sample, and the detection effect of the secondary electron probe is influenced. The scanning electron microscope sold in the market at present has weak capability in the aspect of realizing high-temperature mechanical property test, and can not meet the requirements of research and service performance evaluation of the high-temperature material at present. Based on this, the invention patent application with application number 201310592456.7 discloses a high-temperature secondary electron detector collection assembly and a high-temperature scanning electron microscope, which prevent a standard secondary electron detector collection assembly from absorbing visible light and infrared rays and further avoid white spots by arranging a light-blocking sleeve capable of blocking visible light and infrared rays on a secondary electron detector, thereby ensuring that an image generated by the standard secondary electron detector collection assembly can normally reflect the change of the surface of a sample in a high-temperature state. However, the grid structure adopted by the electron incidence end of the high-temperature secondary electron detector collecting assembly still enables a large amount of visible light and infrared rays to be incident, and the monitoring effect is still influenced to a certain extent.
Disclosure of Invention
The invention aims to provide a secondary electron probe and a high-temperature scanning electron microscope, which are used for solving the problems in the prior art, and the high-voltage electron tube is arranged to comprise an inner collecting layer and an outer collecting layer which are oppositely arranged, and the outer collecting layer is arranged on the inner collecting layer in a mode of being adjustable in circumferential angle, so that electron collecting holes in the inner collecting layer and the outer collecting layer are opposite to each other in normal temperature environment, secondary electrons are collected to the maximum extent, and the outer collecting layer is rotated to a state that a shielding part completely shields the electron collecting holes in the inner collecting layer in high-temperature environment, so that a large amount of visible light and infrared rays are shielded, and the secondary electrons are collected, and the influence of the visible light and the infrared rays is avoided.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a secondary electron probe, which comprises a high-voltage electron tube arranged at an electron inlet end, wherein the high-voltage electron tube comprises an inner collecting layer and an outer collecting layer which are oppositely arranged, the outer collecting layer is arranged on the inner collecting layer in a circumferential angle adjustable manner, a gap is formed between the inner collecting layer and the outer collecting layer, a plurality of electron collecting holes are uniformly distributed on the inner collecting layer and the outer collecting layer, the electron collecting holes on the inner collecting layer and the outer collecting layer are correspondingly arranged, a shielding part is arranged between every two adjacent electron collecting holes, and the area of the shielding part is not smaller than that of the electron collecting holes which are oppositely arranged on the inner collecting layer or the outer collecting layer.
Preferably, the distribution and size of the electron collecting holes on the inner and outer collecting layers are the same.
Preferably, the electron collecting hole has a width gradually increasing from a central portion of the inner collecting layer or the outer collecting layer toward the outside.
Preferably, a positioning structure is further arranged between the inner collecting layer and the outer collecting layer.
Preferably, an annular wall is arranged on the outer collecting layer, the outer collecting layer is sleeved with the inner collecting layer through the annular wall, a positioning hole is formed in the annular wall, the positioning structure is a positioning bolt, and the positioning bolt penetrates through the positioning hole and abuts against the side wall of the inner collecting layer tightly.
Preferably, the high-voltage electron tube further comprises an insulating connecting tube, a sealing connecting tube, a mounting flange, a fixing tube and an electron receiver which are sequentially connected to the rear of the high-voltage electron tube along the electron incidence direction.
The invention also aims to provide a high-temperature scanning electron microscope, which comprises an electron microscope chamber, an XYZ moving platform arranged in the electron microscope chamber, an electron gun arranged outside the electron microscope chamber and communicated with the electron microscope chamber, and a secondary electron probe; and the XYZ moving table is provided with a high-temperature stretching table.
Preferably, a back scattering probe and an EBSD probe are further disposed on the secondary electron probe side of the electron microscope chamber.
Preferably, the device further comprises an active vibration isolation table, and the electron microscope chamber is arranged on the active vibration isolation table.
Preferably, the electron microscope cavity is provided with a cleaning ion source above for cleaning a detection sample and the electron microscope cavity, and the electron microscope cavity is provided with a molecular pump below for vacuumizing the electron microscope cavity.
Compared with the prior art, the invention achieves the following technical effects:
1. through setting up the high-pressure electron tube into including the relative interior collection layer that sets up and outer collection layer, and the form on the collection layer including the installation of collection layer circumference angularly adjustable outward, make under normal atmospheric temperature environment, the electron collecting hole on interior collection layer and the outer collection layer is relative, furthest's collection secondary electron, and under high temperature environment, rotate outer collection layer to the state that shielding portion sheltered from the electron collecting hole on with interior collection layer completely, thereby shelter from a large amount of visible light and infrared ray, collect secondary electron, thereby avoid the influence of visible light and infrared ray.
2. The distribution form and the size of the electron collecting holes in the inner collecting layer and the outer collecting layer are set to be the same, so that the situation that when the electron collecting holes in the inner collecting layer and the outer collecting layer are opposite, the positions of the electron collecting holes and the edges are not shielded is guaranteed, and the maximum collection of secondary electrons is guaranteed.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is an exploded view of a high-pressure electron tube of a secondary electron probe;
FIG. 2 is a schematic diagram of the overall structure of a secondary electron probe;
FIG. 3 is a schematic view of a first view structure of a high temperature SEM;
FIG. 4 is a schematic view of a second structure of the high temperature SEM;
wherein, 1, a high-voltage electron tube; 2. an inner collecting layer; 3. an outer collection layer; 4. an electron collection well; 5. a shielding portion; 6. an annular wall; 7. positioning holes; 8. insulating connecting pipes; 9. sealing the connecting pipe; 10. installing a flange; 11. a fixed tube; 12. an electronic receiver; 13. an electron microscope chamber; 14. an XYZ moving stage; 15. an electron gun; 16. a secondary electron probe; 17. a backscatter probe; 18. an EBSD probe; 19. an active vibration isolation table; 20. cleaning an ion source; 21. a molecular pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a secondary electron probe and a high-temperature scanning electron microscope, which are used for solving the problems in the prior art, the high-pressure electron tube is arranged to comprise an inner collecting layer and an outer collecting layer which are oppositely arranged, and the outer collecting layer is arranged on the inner collecting layer in a mode of adjustable circumferential angle, so that electron collecting holes in the inner collecting layer and the outer collecting layer are opposite to each other in a normal-temperature environment, secondary electrons are collected to the maximum degree, and the outer collecting layer is rotated to a state that a shielding part completely shields the electron collecting holes in the inner collecting layer in a high-temperature environment, so that a large amount of visible light and infrared rays are shielded, and the secondary electrons are collected, and the influence of the visible light and the infrared rays is avoided.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Please refer to fig. 1-4.
Example one
As shown in fig. 1-2, the present embodiment provides a secondary electron probe 16, which includes a high voltage electron tube 1 disposed at an electron entrance end, the high voltage electron tube 1 includes an inner collecting layer 2 and an outer collecting layer 3 disposed oppositely, the outer collecting layer 3 is mounted on the inner collecting layer 2 with adjustable circumferential angle; a rotating shaft can be arranged between the inner collecting layer 2 and the outer collecting layer 3, the outer collecting layer 3 is arranged on the inner collecting layer 2 through the rotating shaft, and the outer collecting layer 3 can rotate relative to the inner collecting layer 2, so that the relative angle can be adjusted; or the inner collection layer 2 and the outer collection layer 3 can be both circular, the outer collection layer 3 is sleeved on the side wall of the inner collection layer 2, the side wall of the inner collection layer 2 is used as a rotating shaft, and the outer collection layer 3 can rotate relative to the inner collection layer 2; a plurality of clamping devices can be arranged between the inner collection layer 2 and the outer collection layer 3, when the circumferential angle of the outer collection layer 3 needs to be adjusted, the outer collection layer 3 is separated from the clamping devices, and after the angle is adjusted, the outer collection layer is fixed through the corresponding clamping devices; in summary, any solution that allows the circumferential angle of the outer collection level 3 relative to the inner collection level 2 to be adjusted is possible; a gap is arranged between the inner collection layer 2 and the outer collection layer 3, a plurality of electron collection holes 4 are uniformly distributed on the inner collection layer 2 and the outer collection layer 3, and the electron collection holes 4 are used for collecting and collecting secondary electrons; the electron collecting holes 4 on the inner collecting layer 2 and the outer collecting layer 3 are correspondingly arranged, a shielding part 5 is arranged between the adjacent electron collecting holes 4, and the area of the shielding part 5 is not less than that of the electron collecting holes 4 which are oppositely arranged on the inner collecting layer 2 or the outer collecting layer 3; the sizes of the electron collecting holes 4 on the inner collecting layer 2 and the outer collecting layer 3 can be the same or different, as long as the electron collecting holes 4 between the inner collecting layer 2 and the outer collecting layer 3 can be opposite to each other, so that secondary electrons can pass through the electron collecting holes, and after the angle is adjusted, the electron collecting holes 4 on the inner collecting layer 2 and the outer collecting layer 3 are staggered with each other, and the opposite electron collecting holes 4 can be shielded by the shielding part 5; when the secondary electron probe 16 is detected at normal temperature, the electron collecting holes 4 on the inner collecting layer 2 and the outer collecting layer 3 are adjusted to be opposite to each other, so that secondary electrons can enter the secondary electron probe 16 through the electron collecting holes 4 to the maximum extent, and secondary electrons are collected, when the detection needs to be performed in a high-temperature environment, because a sample to be detected can generate a large amount of visible light and infrared rays, the visible light and the infrared rays which are transmitted along a straight line are blocked by adjusting the circumferential angle of the outer collecting layer 3 relative to the inner collecting layer 2 and enabling the blocking parts 5 on the inner collecting layer 2 and the outer collecting layer 3 to form blocking on the electron collecting holes 4 opposite to each other, so that the visible light and the infrared rays are prevented from entering the secondary electron probe 16, and the secondary electrons can pass through the electron collecting holes 4 on the outer collecting layer 3, the gap between the outer collecting layer 3 and the inner collecting layer 2 and the electron collecting holes 4 on the inner collecting layer 2 to enter the secondary electron probe 16, therefore, secondary electrons are collected under the influence of visible light and infrared rays, and the high-precision imaging effect in a high-temperature environment, even a high-temperature environment of 1500 ℃ is realized.
Furthermore, in order to ensure that the secondary electrons can be maximally collected when passing through the electron collecting holes 4, the distribution form and the size of the electron collecting holes 4 on the inner collecting layer 2 and the outer collecting layer 3 are the same, so that when the electron collecting holes 4 on the inner collecting layer 2 and the outer collecting layer 3 are opposite, the electron collecting holes 4 and the edges are not shielded; in this embodiment, the electron collecting holes 4 may be arranged in one or more radial directions of the inner collecting layer 2 or the outer collecting layer 3, and in order to maximize the secondary electron collection, one is preferably arranged in the radial direction.
In a preferred embodiment, the electron collecting hole 4 has a fan-like structure with gradually increasing width from the middle of the inner collecting layer 2 or the outer collecting layer 3, and the structure of the electron collecting hole 4 further ensures that more secondary electrons can be collected.
Further, in order to ensure that the relative position between the inner collection layer 2 and the outer collection layer 3 is fixed after the angle is adjusted, in this embodiment, a positioning structure is further disposed between the inner collection layer 2 and the outer collection layer 3.
Preferably, in a specific embodiment, the outer collection layer 3 is provided with an annular wall 6, the outer collection layer 3 is sleeved with the inner collection layer 2 through the annular wall 6, the annular wall 6 is provided with a positioning hole 7, the positioning structure is a positioning bolt, the positioning bolt penetrates through the positioning hole 7 to be tightly abutted against the side wall of the inner collection layer 2, and of course, the positioning structure can also be any other positioning structure such as a clamping structure and the like which can ensure that the relative position between the inner collection layer 2 and the outer collection layer 3 is fixed.
Further, the secondary electron probe 16 further comprises an insulating connection pipe 8, a sealing connection pipe 9, a mounting flange 10, a fixing pipe 11 and an electron receiver 12 which are sequentially connected to the rear of the high-voltage electron tube 1 along an electron incidence direction, the insulating connection pipe 8 ensures that when the high-voltage electron tube 1 collects secondary electrons in a power-on state, the insulating connection pipe is insulated from other structures, the sealing connection pipe 9 ensures the sealing performance inside the secondary electron probe 16, the mounting flange 10 is used for mounting the secondary electron probe 16 on other devices, and the fixing pipe 11 is used for mounting and fixing the electron receiver 12.
Example two
As shown in fig. 1-4, the present embodiment provides a high temperature scanning electron microscope, which includes a electron microscope chamber 13, an XYZ moving stage 14 disposed in the electron microscope chamber 13, an electron gun 15 disposed outside the electron microscope chamber 13 and communicating with the electron microscope chamber 13, and a secondary electron probe 16 in the first embodiment; be provided with the tensile platform of high temperature on the XYZ mobile station 14, when using, place the testing sample at the tensile bench of high temperature, heat the testing sample through the tensile platform of high temperature, realize the mechanical properties test of testing sample under the high temperature environment, secondary electron probe 16 is collected, is surveyed the secondary electron under the high temperature state, can avoid the influence of visible light and infrared ray to formation of image, under 1500 ℃ high temperature environment, still can realize fine imaging effect, thereby guarantee that the aassessment to testing sample mechanical properties is more accurate.
Furthermore, a back scattering probe 17 and an EBSD probe 18 are further disposed on the secondary electron probe 16 side of the electron microscope chamber 13, and the back scattering probe 17 and the EBSD probe 18 are used for auxiliary imaging.
Further, the testing device further comprises an active vibration isolation platform 19, the electron microscope cavity 13 is arranged on the active vibration isolation platform 19, and the influence of vibration on the whole testing process is eliminated through the active vibration isolation platform 19.
In a preferred embodiment, a cleaning ion source 20 is arranged above the electron microscope chamber 13 and used for cleaning the detection sample and the electron microscope chamber 13, and a molecular pump 21 is arranged below the electron microscope chamber 13 and used for vacuumizing the electron microscope chamber 13, wherein the vacuum degree can reach 2.0 × 10 -4 Pa, thereby realizing the test of the detection sample in the vacuum environment.
The adaptation according to the actual needs is within the scope of the invention.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A secondary electron probe, comprising: including setting up the high-pressure electron tube at electron entry end, the high-pressure electron tube is including the relative inner collecting layer and the outer collecting layer that sets up, outer collecting layer circumference angle adjustable installs on the inner collecting layer, the inner collecting layer with the clearance has between the outer collecting layer, the inner collecting layer with it has a plurality of electron collecting holes to equally divide on the outer collecting layer, the inner collecting layer with on the outer collecting layer electron collecting hole corresponds the setting, it is adjacent on the outer collecting layer shielding portion has between the electron collecting hole, it is adjacent on the inner collecting layer shielding portion also has between the electron collecting hole, shielding portion's area is not less than relative setting up the inner collecting layer or on the outer collecting layer the area of electron collecting hole.
2. A secondary electron probe according to claim 1, wherein: the distribution form and the size of the electron collecting holes on the inner collecting layer and the outer collecting layer are the same.
3. A secondary electron probe according to claim 2, wherein: the electron collecting hole gradually increases in width from the middle of the inner collecting layer or the outer collecting layer toward the outside.
4. A secondary electron probe according to any of claims 1 to 3, wherein: and a positioning structure is also arranged between the inner collecting layer and the outer collecting layer.
5. A secondary electron probe according to claim 4, wherein: the outer collecting layer is provided with an annular wall, the outer collecting layer is sleeved with the inner collecting layer through the annular wall, a positioning hole is formed in the annular wall, the positioning structure is a positioning bolt, and the positioning bolt penetrates through the positioning hole to be tightly abutted to the side wall of the inner collecting layer.
6. A secondary electron probe according to claim 1, wherein: the high-voltage electron tube power supply further comprises an insulating connecting tube, a sealing connecting tube, a mounting flange, a fixing tube and an electron receiver which are sequentially connected to the rear of the high-voltage electron tube along the electron incidence direction.
7. A high temperature scanning electron microscope, characterized by: the secondary electron probe comprises an electron microscope chamber, an XYZ moving table arranged in the electron microscope chamber, an electron gun arranged outside the electron microscope chamber and communicated with the electron microscope chamber, and the secondary electron probe as claimed in any one of claims 1 to 6; and the XYZ moving table is provided with a high-temperature stretching table.
8. A high temperature scanning electron microscope according to claim 7 wherein: and a back scattering probe and an EBSD probe are also arranged on the secondary electron probe side of the electron microscope cavity.
9. A high temperature scanning electron microscope according to claim 8 wherein: the active vibration isolation platform is further included, and the electron microscope cavity is arranged on the active vibration isolation platform.
10. A high temperature scanning electron microscope according to claim 9 wherein: the device comprises an electron microscope cavity, and is characterized in that a cleaning ion source used for cleaning a detection sample and the electron microscope cavity is arranged above the electron microscope cavity, and a molecular pump used for vacuumizing the electron microscope cavity is arranged below the electron microscope cavity.
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| CN202110563286.4A CN113299529B (en) | 2021-05-24 | 2021-05-24 | Secondary electron probe and high-temperature scanning electron microscope |
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| US2408216A (en) * | 1942-03-06 | 1946-09-24 | Rca Corp | Beam deflection electron discharge device |
| JPS6316538A (en) * | 1986-07-07 | 1988-01-23 | Hitachi Ltd | Measuring method for vacuum inside electron microscope and device thereof and electron microscope itself |
| US4982091A (en) * | 1986-12-12 | 1991-01-01 | Texas Instruments Incorporated | Electron beam apparatus and method for detecting secondary electrons |
| CN103594310A (en) * | 2013-11-22 | 2014-02-19 | 北京中科科仪股份有限公司 | High-temperature secondary electronic detector collection assembly and high-temperature scanning electron microscope |
| CN109142414A (en) * | 2018-08-23 | 2019-01-04 | 中国工程物理研究院流体物理研究所 | A kind of metal surface secondary electron spectral distribution test method |
| CN209183498U (en) * | 2018-11-28 | 2019-07-30 | 上海欧波同仪器有限公司 | A kind of secondary electron detector |
-
2021
- 2021-05-24 CN CN202110563286.4A patent/CN113299529B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2408216A (en) * | 1942-03-06 | 1946-09-24 | Rca Corp | Beam deflection electron discharge device |
| JPS6316538A (en) * | 1986-07-07 | 1988-01-23 | Hitachi Ltd | Measuring method for vacuum inside electron microscope and device thereof and electron microscope itself |
| US4982091A (en) * | 1986-12-12 | 1991-01-01 | Texas Instruments Incorporated | Electron beam apparatus and method for detecting secondary electrons |
| CN103594310A (en) * | 2013-11-22 | 2014-02-19 | 北京中科科仪股份有限公司 | High-temperature secondary electronic detector collection assembly and high-temperature scanning electron microscope |
| CN109142414A (en) * | 2018-08-23 | 2019-01-04 | 中国工程物理研究院流体物理研究所 | A kind of metal surface secondary electron spectral distribution test method |
| CN209183498U (en) * | 2018-11-28 | 2019-07-30 | 上海欧波同仪器有限公司 | A kind of secondary electron detector |
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