CN111024733A - Transmission electron microscope double-inclined sample rod - Google Patents
Transmission electron microscope double-inclined sample rod Download PDFInfo
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- CN111024733A CN111024733A CN201911357081.XA CN201911357081A CN111024733A CN 111024733 A CN111024733 A CN 111024733A CN 201911357081 A CN201911357081 A CN 201911357081A CN 111024733 A CN111024733 A CN 111024733A
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- sample
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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
- 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
- G01N23/20025—Sample holders or supports therefor
-
- 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
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a transmission electron microscope double-inclination sample rod, which comprises a sample table, a sample rod shell, a sample rod inner core and a handle, wherein the sample table is provided with a rotatable sample crucible, a detachable pressing piece and a fine adjustment gear, a sample can rotate around the incident direction of an electron beam along with the rotatable crucible, the sample rod shell is fixedly connected with the sample table, the shell part can be reasonably matched with an electron microscope angle measuring table, the front end of the sample rod inner core is provided with a transmission rack matched with the fine adjustment gear, the rear section of the sample rod inner core is connected with a linear servo motor in the handle through a coupler, the inner core moves linearly to drive the rotatable crucible to rotate, and a linear servo motor and a transmission mechanism for controlling the movement of the inner core are arranged in the handle.
Description
Technical Field
The invention relates to a novel double-inclined sample rod for a transmission electron microscope, relates to the technical field of transmission electron microscope related accessories and nano scientific test research, and can allow large-angle crystal band axis adjustment by adopting a novel tilting mode.
Background
In recent years, with the more and more intensive research on the field of nano science, the importance of the transmission electron microscope is increasingly highlighted. The widespread use of electron microscopes (electron microscopes) and the rapid development of electron microscopy have greatly facilitated the development of materials science, physics, chemistry and life sciences. Since the 60 s of the 20 th century, the basic principles and experimental techniques of electron microscopy have been rapidly developed, and in particular, the improvement of electron microscope manufacturing techniques and laboratory techniques, the development of vacuum techniques, and the application of high-coherence field emission electron guns have greatly improved the spatial resolution and microscopic analysis capability of electron microscopes, and in particular, the use of spherical aberration correctors and monochromators have made the resolution of transmission electron microscopes step into the sub-angstrom era.
The sample rod is a container for carrying the transmission electron microscope sample. To view the sample, it is necessary to load the sample on a sample rod and insert it together into the goniometer stage of the transmission electron microscope. The sample rod is in direct contact with the sample and must enable adjustment of the experimental parameters loaded on the sample, the most essential requirement being that it should be possible to move the sample laterally (X-direction) to view the different zones; secondly, for optimal imaging, it should also be able to move in the vertical direction (Y-axis direction). However, in the study of crystalline materials, the most common operation is to tilt the material in two orthogonal directions (axial and radial) so that different facets are parallel to the electron beam. At present, two types of commonly used sample rods are a single-inclination sample rod and a double-inclination sample rod. Wherein, the single-inclined sample rod can only rotate around the rod shaft through the rotation of the angle measuring table; the double-inclination sample rod can realize axial rotation and radial overturning of the sample so as to flexibly control the orientation of the sample, so the double-inclination sample rod is the most commonly used sample rod.
However, the rotation angle of the double-tilting sample rod is limited by the structural design of the angle measuring table and the rod, and the tilting angle can not completely meet the test requirement, and the common double-tilting rod rotates around the axial direction (tilting in the α direction) by an angle of-50 degrees to +50 degrees, and rotates along the axial direction (tilting in the β direction) by an angle of-30 degrees to +30 degrees.
Disclosure of Invention
The invention aims to provide a novel transmission electron microscope double-inclined sample rod, and aims to realize a larger-angle and safer crystal belt axis direction adjusting scheme so as to overcome the defects of the conventional equipment.
The technical scheme of the invention is as follows:
a transmission electron microscope double-inclination sample rod comprises a sample table, a sample rod shell, a sample rod inner core and a handle, and further comprises a sample table 1, a sample rod shell 2, an inner core 3, a handle 4, a rotatable crucible 5, a detachable pressing piece 6, a fine adjustment gear 7, a transmission rack 8, an air valve switch 9, a vacuum sealing ring 10, a positioning pin 11, a fastening groove 12, a detaching groove 13, a linear servo motor 14 and a flexible coupling 15;
the tilting mode of the transmission electron microscope double-tilting sample rod adopts a mode of combining axial tilting, namely α tilting, and rotation around the incident direction of an electron beam, namely theta rotation, wherein:
the front end of the sample platform 1 is provided with a transmission hole for passing through electron beams, and a rotatable crucible 5 which can rotate around the transmission hole is matched in the aperture of the transmission hole; the rotatable crucible 5 and the fine adjustment gear 7 are of an integrated structure and are connected through a bushing, so that the rotatable crucible 5 and the fine adjustment gear 7 are ensured to be in the same motion state and rotate around the Z axis; the top of the rotatable crucible 5 is fixedly connected with the gasket and is used for positioning the rotatable crucible 5 in the direction vertical to the sample table 1; three rectangular fastening grooves 12 are arranged on the outer ring of the gasket and are matched with three claws on the detachable pressing sheet 6; the inner ring of the gasket is provided with a square disassembly groove 13 for disassembling the detachable pressing sheet 6; the sample table 1 and the sample rod shell 2 are of an integrated structure;
the shell 2 of the sample rod is matched with a transmission electron microscope angle measuring table, the shell 2 is divided into a large-diameter part and a small-diameter part, the small-diameter part is provided with an air valve switch 9 for opening an air valve of the electron microscope, the front end of the large-diameter part is provided with a groove for installing a vacuum sealing ring 10, and the vacuum sealing ring 10 is matched with the electron microscope angle measuring table; the rear end of the large-diameter part is fixedly connected with a handle 4; the front end and the rear end inside the large-diameter part are respectively provided with an annular groove for radially positioning the inner core 3;
the inner core 3 is a transmission shaft which is connected with the sample table 1 and a linear servo motor 14 in the handle 4, and the front end of the inner core is fixedly connected with a transmission rack 8 matched with the fine adjustment gear 7, and the transmission rack 8 moves along with the axial movement of the inner core 3; the radial positioning of the inner core 3 respectively passes through positioning grooves positioned in the front section and the rear end of the large-diameter part of the sample rod shell 2; the rear end of the inner core 3 is connected with a linear servo motor 14 in the handle 4 through a flexible coupling 15;
the handle 4 is internally provided with a transmission mechanism for driving the inner core 3 to move, and mainly comprises a linear servo motor 14 capable of realizing linear motion and a flexible coupling 15, wherein the linear servo motor 14 is fixed on a support frame in the handle 4; the flexible coupling 15 connects the motor spindle with the inner core 3 to realize the control of the linear servo motor 14 on the inner core 3; the front end of the handle 4 is fixed with a sample rod shell 2 and a positioning pin 11.
(1) The tilting direction of the sample rod alpha is along the axial direction (Y axis) of the sample rod, and the tilting angle range is between-50 degrees and +50 degrees;
(2) the rotation direction of the sample rod theta is around the direction of the electron beam (Z axis), and the tilting angle range is-180 degrees to +180 degrees;
(3) when a sample is installed, firstly, a copper mesh is placed on a sample groove of the rotatable crucible 5, three claws on the detachable pressing sheet 6 are respectively aligned with fastening grooves 12 on the rotatable crucible 5, and the sample and the rotatable crucible 5 are installed and fixed by utilizing the elastic clamping of the detachable pressing sheet 6; the detachable type can be realized by using a sampling needle to jack up the detachable pressing sheet 6 from the detachable groove 13 and taking out a sample.
(4) And during tilting, the crystal belt shaft is rotated forwards to be perpendicular to the axial direction (Y axis) and then tilted alpha to be collinear with the incident direction of the electron beam, or the crystal belt shaft is tilted alpha to be collinear with the axial direction (Y axis) and then rotated theta to be collinear with the incident direction of the electron beam.
Compared with the prior art, the invention has the beneficial effects that:
(1) the double-inclination sample rod β designed by the invention can realize large-angle inclination, namely, the maximum inclination angle in the β direction is enlarged to the inclination range of-50 degrees to +50 degrees in the α direction;
(2) because the designed sample rod tilts in a mode of rotating around the injection direction of the electron beam (theta rotation), the phenomenon that the sample rod tilts in the direction of β and collides with a pole shoe of an electron microscope cannot occur, and the sample rod is safe to use;
(3) the sample is easy to mount and dismount;
(4) easy to process.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
Fig. 2(a) is a schematic front structural view of the sample stage 1; fig. 2(b) is a schematic diagram of the reverse structure of the sample stage 1.
Fig. 3 is a cross-sectional view of the present invention.
Fig. 4(a) is a schematic diagram of the most general case of the ribbon axis orientation, fig. 4(b) is a schematic diagram of the ribbon axis normal direction at an angle of 0 ° to the X-axis, fig. 4(c) is a schematic diagram of the ribbon axis normal direction at an angle of 0 ° to the Z-axis, fig. 4(d) is a schematic diagram of the rotatable crucible θ rotated by a °, and fig. 4(e) is a schematic diagram of the sample rod α tilted by b °.
FIG. 5(a) is a schematic view of the range of motion that can be achieved by a conventional double-tilt lever; fig. 5(b) is an equivalent schematic diagram of the range of motion that can be achieved by the double-tilt rod sample of the present invention.
In the figure: 1, a sample stage; 2 a sample rod housing; 3, a sample rod inner core; 4, a handle; 5 rotating the sample crucible; 6, detachable tabletting; 7 fine adjustment of the gear; 8 driving the rack; 9, an air valve switch; 10, vacuum sealing rings; 11 positioning pins; 12 fastening grooves; 13 disassembling the tank; 14 linear servo motor; 15 flexible coupling.
Detailed Description
The invention will be described in detail below with reference to the following figures and embodiments:
when the transmission electron microscope double-inclination sample rod is applied, a prepared sample is firstly placed on the rotatable crucible 5, three claws on the detachable pressing sheet 6 are respectively aligned with three fastening grooves 12 on the rotatable crucible 5 and then are pressed tightly, when the transmission electron microscope double-inclination sample rod works, the α -direction inclination is realized by the axial rotation of the transmission electron microscope angle measuring table, when the β -direction inclination is realized, the linear servo motor 14 starts to work, the inner core 3 is pushed to do linear motion through the flexible coupling 15, the stretching of the inner core 3 drives the transmission rack 8 meshed with the fine adjustment gear 7 to move, the rotatable crucible 5 with the sample is driven to rotate by the meshing motion as the rotatable crucible 5 is fixedly connected with the fine adjustment gear 7, the rotatable crucible 5 with the sample is driven to rotate together, as long as the number of the transmission rack 8 is enough, the rotatable crucible 5 can realize-180 degrees to +180 degrees, and the maximum inclination angle of the sample in the β direction can be enlarged to-50 degrees, and the detachable pressing sheet 6 can be taken out after the observation needle is detached and the observation needle which needs to be inclined more is completely.
When the ribbon axis of the sample is in the most general condition, the sample is tilted and adjusted, as shown in fig. 4a, the forward direction of the sample has a certain angle with the X axis, the Y axis and the Z axis, firstly, the rotatable crucible 5 is controlled by the linear servo motor control 14 to rotate (theta rotation) by a degrees (fig. 4d) around the Z axis until the included angle between the forward direction of the ribbon axis and the X axis is 0 degree, as shown in fig. 4b, and then, the sample rod is controlled by the transmission electron microscope goniometer to rotate (α tilt) by b degrees (fig. 4e) around the Y axis until the included angle between the forward direction of the ribbon and the Z axis is 0 degree (fig. 4c), and at this time, the ribbon axis is parallel to the incident direction of the electron beam.
Fig. 5 is an equivalent schematic diagram of the range of motion of the sample of the double-tilt rod of the prior art, which is the maximum range of motion of the sample of the double-tilt rod of the prior art, fig. 5a is an equivalent schematic diagram of the maximum range of motion of the sample of the double-tilt rod of the present invention, which is designed according to the present invention, fig. 5b is a schematic diagram of the tilt angle of α and β in comparison, but since the sample can rotate 360 ° around the Z-axis, each point on the copper mesh can be turned to the maximum angle of α direction.
Claims (1)
1. A transmission electron microscope double-inclination sample rod is characterized by comprising a sample table, a sample rod outer shell, a sample rod inner core and a handle, and further comprising a sample table (1), a sample rod outer shell (2), an inner core (3), a handle (4), a rotatable crucible (5), a detachable pressing piece (6), a fine adjustment gear (7), a transmission rack (8), an air valve switch (9), a vacuum sealing ring (10), a positioning pin (11), a fastening groove (12), a dismounting groove (13), a linear servo motor (14) and a flexible coupling (15);
the tilting mode of the transmission electron microscope double-tilting sample rod adopts a mode of combining axial tilting, namely α tilting, and rotation around the incident direction of an electron beam, namely theta rotation, wherein:
the front end of the sample platform (1) is provided with a transmission hole for passing through electron beams, and a rotatable crucible (5) capable of rotating around the transmission hole is matched in the aperture of the transmission hole; the rotatable crucible (5) and the fine adjustment gear (7) are of an integrated structure and are connected through a bushing, so that the rotatable crucible (5) and the fine adjustment gear (7) are ensured to be in the same motion state and rotate around a Z axis; the top of the rotatable crucible (5) is fixedly connected with the gasket and used for positioning the rotatable crucible (5) in a direction vertical to the sample table (1); three rectangular fastening grooves (12) are formed in the outer ring of the gasket and are matched with three claws on the detachable pressing sheet (6); the inner ring of the gasket is provided with a square disassembly groove (13) for disassembling the detachable pressing sheet (6); the sample table (1) and the sample rod shell (2) are of an integrated structure;
the sample rod shell (2) is matched with a transmission electron microscope angle measuring table, the shell 2 is divided into a large-diameter part and a small-diameter part, the small-diameter part is provided with an air valve switch (9) for opening an electron microscope air valve, the front end of the large-diameter part is provided with a groove for installing a vacuum sealing ring (10), and the vacuum sealing ring (10) is matched with the electron microscope angle measuring table; the rear end of the large-diameter part is fixedly connected with a handle (4); the front end and the rear end of the inside of the large-diameter part are respectively provided with an annular groove for radially positioning the inner core (3);
the inner core (3) is a transmission shaft which is connected with a linear servo motor (14) in the sample table (1) and the handle (4), and the front end of the inner core is fixedly connected with a transmission rack (8) matched with the fine adjustment gear (7), and the transmission rack (8) moves along with the axial movement of the inner core (3); the radial positioning of the inner core (3) is respectively through positioning grooves positioned in the front section and the rear end of the large-diameter part of the sample rod shell (2); the rear end of the inner core (3) is connected with a linear servo motor (14) inside the handle (4) through a flexible coupling (15);
the handle (4) is internally provided with a transmission mechanism for driving the inner core (3) to move, and mainly comprises a linear servo motor (14) capable of realizing linear motion and a flexible coupling (15), wherein the linear servo motor (14) is fixed on a support frame in the handle (4); the flexible coupling (15) connects the motor spindle with the inner core (3) to realize the control of the linear servo motor (14) on the inner core (3); the front end of the handle (4) is fixed with a sample rod shell (2) and a positioning pin (11).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911357081.XA CN111024733A (en) | 2019-12-25 | 2019-12-25 | Transmission electron microscope double-inclined sample rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911357081.XA CN111024733A (en) | 2019-12-25 | 2019-12-25 | Transmission electron microscope double-inclined sample rod |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111024733A true CN111024733A (en) | 2020-04-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911357081.XA Withdrawn CN111024733A (en) | 2019-12-25 | 2019-12-25 | Transmission electron microscope double-inclined sample rod |
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| CN (1) | CN111024733A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112697818A (en) * | 2020-12-14 | 2021-04-23 | 兰州大学 | Magnetoelectric in-situ sample rod of transmission electron microscope suitable for FIB technology sample preparation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112697818A (en) * | 2020-12-14 | 2021-04-23 | 兰州大学 | Magnetoelectric in-situ sample rod of transmission electron microscope suitable for FIB technology sample preparation |
| CN112697818B (en) * | 2020-12-14 | 2023-07-25 | 兰州大学 | Magneto-electric in-situ sample rod of transmission electron microscope suitable for FIB (FIB field) technology sample preparation |
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Application publication date: 20200417 |
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