CN112834539B - Transmission electron microscope power electric heating in-situ sample rod - Google Patents
Transmission electron microscope power electric heating in-situ sample rod Download PDFInfo
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- CN112834539B CN112834539B CN202011636775.XA CN202011636775A CN112834539B CN 112834539 B CN112834539 B CN 112834539B CN 202011636775 A CN202011636775 A CN 202011636775A CN 112834539 B CN112834539 B CN 112834539B
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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
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
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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
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
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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
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
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- Radiology & Medical Imaging (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the field of transmission electron microscope in-situ sample rods, and discloses a transmission electron microscope force electric heating in-situ sample rod which comprises a handle, a rod body, a movable rod and a rod head, wherein the rod head is provided with: a mechanical probe and a mechanical chip; the mechanical probe and the sample connector are arranged close to each other, and the mechanical probe and the sample connector are matched and used for extruding and powering up a sample; the mechanical chip is fixedly connected with the mechanical probe and is used for powering up the probe and measuring a force feedback signal from the mechanical probe; the sample joint is provided with: the electric heating device is used for heating the sample joint and changing the temperature of the microenvironment of the sample joint area; meanwhile, the sample joint can be powered on and is matched with a powered mechanical probe for use: the sample was powered. The in-situ sample rod can directly apply force, electricity and heat environment, and the experimental operation process of in-situ test is simplified.
Description
Technical Field
The invention relates to the field of transmission electron microscope in-situ sample rods, in particular to a transmission electron microscope force electric heating in-situ sample rod.
Background
With the continuous maturation and development of electron microscope in-situ technology, a transmission electron microscope (transmission electron microscope or TEM) does not only represent the structure of a material, but also can realize high-precision nanometer processing and performance testing, and the structural evolution of the material is related to the change of various properties (such as force, electricity and heat) of the material.
The above functions must be accomplished by means of a series of in situ physical property test sample rods, but due to the limitations of the size (in millimeter order) of the sample chamber of the transmission electron microscope, the in situ technology in the transmission electron microscope has difficulty in not only accurately loading various physical fields on the sample, but also ensuring a series of harsh conditions, such as keeping the sample extremely high mechanical stability, keeping the electron microscope system extremely high vacuum, not having too much influence on the imaging electrons, having to be compact to adapt to the size of the small electron microscope sample chamber, etc. Therefore, achieving force, electrical, thermal environmental settings under transmission electron microscopy remains a very challenging topic.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention is to provide a transmission electron microscope force electrothermal in-situ sample rod, which can directly apply force, electricity and heat through the sample rod, so as to simplify the experimental operation process of in-situ test.
In order to achieve the above object, the present invention provides a three-dimensional force electric heating sample rod for a transmission electron microscope, comprising a handle, a rod body, a moving rod and a rod head, wherein one end of the rod body is fixed on the handle, the other end of the rod body is fixed with the rod head, the moving rod is arranged in the rod body, moves in the rod body, and one end of the moving rod is provided with a sample joint;
The club head is provided with: a mechanical probe and a mechanical chip; the mechanical probe and the sample connector are arranged close to each other, and the mechanical probe and the sample connector are matched and used for extruding and powering up a sample; the mechanical chip is fixedly connected with the mechanical probe and is used for powering up the probe and measuring a force feedback signal from the mechanical probe;
The sample joint is provided with: the electric heating device is used for heating the sample joint and changing the temperature of the microenvironment of the sample joint area; meanwhile, the sample joint can be powered on and is matched with a powered mechanical probe for use: the sample was powered.
Further, the sample connector is a needle tip or a sample carrier.
Further, the electric heating device is a resistance wire, the resistance wire is arranged in an insulating manner with the sample joint, and the resistance wire is led out through two electrodes arranged on the sample joint.
Further, the mechanical chip comprises a stress part, a first electrode, a second electrode and a third electrode, wherein one end of the stress part is fixed with the mechanical probe; the stress part is arranged on the mechanical chip through a cantilever structure; electrodes with a feathered structure are arranged on two sides of the stress part; the electrode that is provided with the feather structure in the unilateral of first electrode the second electrode, the feather structure electrode of atress portion is crisscross with the feather structure electrode of first electrode, second electrode respectively and is set up, atress portion along the atress direction with the third electrode is close to the setting, works as atress portion is when receiving pressure, presents two kinds of states: the feather-shaped structure electrode of the stress part is parallel and close to the feather-shaped structure electrodes of the first electrode and the second electrode, and a pressure feedback signal is output; the stress part is in abutting connection with the third electrode, and the third electrode energizes the stress part.
Further, the head is further provided with: the circuit board is arranged at the groove on the surface of the club head; the contact pins are respectively lapped on the circuit board and the electrodes of the mechanical chip; the gland is used for fixing the circuit board and the mechanical chip on the rod head.
Further, an electric rough adjusting module is arranged in the handle, and the electric rough adjusting module is connected with one end of the movable rod and used for carrying out three-dimensional movement control of micrometer precision on the movable rod.
Further, the moving rod comprises XY two-axis piezoceramics and Z-axis piezoceramics, and the XY two-axis piezoceramics and the Z-axis piezoceramics are used for carrying out three-dimensional movement control of nanometer precision on the sample joint.
Furthermore, an O-shaped sealing ring is further arranged in the rod head and sleeved on the sample joint connecting seat for stabilizing movement of the sample joint and sealing of the sample rod.
Further, the sample joint connecting seat of the movable rod
The invention realizes the following technical effects:
According to the transmission electron microscope force electric heating in-situ sample rod, the electric heating device arranged on the sample joint, the mechanical chip arranged on the rod head and the mechanical probe can directly apply force, electricity and heat to the sample to be detected, so that the experimental operation process of in-situ test is simplified.
Drawings
FIG. 1 is a block diagram of a transmission electron microscope force electrothermal in-situ sample rod according to a preferred embodiment of the present invention;
FIG. 2 is a cross-sectional view of FIG. 1;
FIG. 3 is an enlarged view of a portion of the sample club head of FIG. 1;
FIG. 4 is an exploded schematic view of FIG. 3;
FIG. 5 is a schematic diagram of the structure of the sample tab and the mechanical chip.
Wherein:
100-handle; 101-an electric coarse adjustment module; 200-shaft; 202-O type sealing ring; 300-club head; 301-capping; 302-a stylus; 303-mechanical chip; 304-mechanical probe; 305-a circuit board; 306-a through hole; 400-moving the rod; 401-XY biaxial piezoelectric ceramic; 402-Z axis piezoceramic; 403-sample joint connection base; 404-sample joint; 405-an electrical heating assembly; 3031-a force receiving part; 3032-a first electrode; 3033-a second electrode; 3034-a third electrode; 4051-a first heating electrode; 4052-a second heating electrode.
Detailed Description
For further illustration of the various embodiments, the invention is provided with the accompanying drawings. The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate embodiments and together with the description, serve to explain the principles of the embodiments. With reference to these matters, one of ordinary skill in the art will understand other possible embodiments and advantages of the present invention. The components in the figures are not drawn to scale and like reference numerals are generally used to designate like components.
The invention will now be further described with reference to the drawings and detailed description.
Example 1
As shown in fig. 1 to 5, the invention discloses a transmission electron microscope force electric heating in-situ sample rod, which mainly comprises a handle 100, a rod body 200, a rod head 300 and a movable rod 400, wherein one end of the rod body 200 is fixed on the handle 100, the other end of the rod body 200 is fixed with the rod head 300, the movable rod 400 is arranged inside the rod body 200 and moves inside the rod body 200, one end of the movable rod 400 is provided with a sample joint 404, and the sample joint 404 is in different forms such as a sample joint or a sample carrier and can be replaced according to application scenes.
Specifically, the head 300 is provided with: a mechanical probe 304, a mechanical chip 303; the mechanical probe 304 and the sample joint 404 are arranged close to each other, and the mechanical probe 304 and the sample joint 404 are matched to squeeze and power up the sample; the mechanical chip 303 is fixedly connected with the mechanical probe 304 (specifically, the mechanical probe 304 is fixed at the end part of the mechanical chip 303), and is used for powering up the mechanical probe 304 and measuring a force feedback signal returned from the mechanical probe 304.
Specifically, the sample tab 404 is provided with: an electrical heating device 405. In this embodiment, the electric heating device 405 is specifically a resistance wire, which may be disposed on the sample connector 404 in a manner such as silk-screening of a circuit board, and a first heating electrode 4051 and a second heating electrode 4052 are disposed on the sample connector 404, and when the sample connector 404 is mounted on the sample connector socket 403, a heating circuit can be directly established through the two electrodes. The electrical heating device 405 electrically heats the sample connection 404 to change the temperature of the microenvironment in the region of the sample connection 404. The resistance wire has simple structure and small size, is easy to produce and manufacture and control heating, and can rapidly heat the sample joint.
In this embodiment, the mechanical chip 303 includes a force receiving part 3031, a first electrode 3032, a second electrode 3033 and a third electrode 3034, and a mechanical probe 304 is fixed at one end of the force receiving part 3031; the force receiving portion 3031 is disposed on the mechanical chip by a cantilever structure, which provides an elastic connection, so that the force receiving portion 3031 can move when being pressed, and the cantilever structure can be considered as a high resistance state due to the thin cantilever structure. Electrodes with a feathered structure are arranged on two sides of the stress part 3031; the electrodes of the feather structure are arranged on one side of the first electrode 3032 and the second electrode 3033, the electrodes of the feather structure of the stress part 3031 are respectively staggered with the electrodes of the feather structure of the first electrode 3032 and the second electrode 3033, the stress part 3031 is arranged close to the third electrode 3034 along the stress direction, and when the stress part 3031 is under the action of the first pressure, the electrodes of the feather structure of the stress part 3031 are parallel and close to the electrodes of the feather structure of the first electrode 3032 and the second electrode 3033 to generate a pressure feedback signal; when the force receiving portion 3031 is under the action of the second pressure, the force receiving portion 3031 is also in abutting connection with the third electrode 3034, and the third electrode 3034 energizes the force receiving portion 3031.
More specifically, a gland 301, a contact pin 302 and a circuit board 305 are disposed on the club head 300, the contact pin 302 has three electrodes, and the gland 301 is used for electrically connecting the mechanical chip 303 and the circuit board 305 through the contact pin 302, and is used for powering the mechanical probe and collecting force feedback signals through the mechanical chip.
The movable lever 400 is provided in the shaft 200, and one end thereof is connected to the electric rough adjustment module 101 provided in the handle 100, and is controlled by the electric rough adjustment module 101 to perform three-dimensional movement with micrometer-scale accuracy.
Specifically, the electric coarse adjustment module 101 includes three motor modules that respectively operate in three dimensions XYZ to control movement of the movement bar 400 in XYZ three axes.
In this embodiment, the movable rod 400 preferably comprises an XY biaxial piezoceramic 401, a Z-axis piezoceramic 402, a sample joint connection mount 403, a sample joint 404, and some other connection members. The XY two-axis piezoceramics 401 and the Z-axis piezoceramics 402 are used for carrying out three-dimensional movement control of nanometer-scale precision on the sample joint 404. Thereby realizing the alignment of the sample joint 404 and the mechanical probe 304, stably clamping the sample, and performing the operations of extrusion, power-up and the like.
Because the whole sample rod adopts electric control, the position of the sample joint 404 stays at a specified position or automatically returns to the original point through the electric control of the electric rough adjustment module 101, the XY two-axis piezoceramic 401 and the Z-axis piezoceramic 402.
In this embodiment, preferably, an O-ring 202 is further disposed in the club head 300, and the O-ring 202 is sleeved on the sample joint connecting seat 403, so as to stabilize the movement of the sample joint 404 and the vacuum sealing of the shaft 200.
In this embodiment, the sample joint connection seat 403 is preferably designed to be detachable, and is connected by a screw, so that a through hole 306 is provided at a corresponding position between the side wall of the club head 300 and the fixing hole of the sample joint connection seat 403, so as to facilitate the detachment and installation of the sample joint connection seat 403. And further, the quick replacement of the sample joint 404 is realized, so that the operation requirements of different applications such as mechanical stretching, mechanical extrusion and electrochemical experiments of a sample are met, a heating environment is provided, and the reading of the force and electric data of the sample is performed.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. The transmission electron microscope force electric heating in-situ sample rod comprises a handle, a rod body, a movable rod and a rod head, wherein one end of the rod body is fixed on the handle, the other end of the rod body is fixed with the rod head, the movable rod is arranged in the rod body and moves in the rod body, and a sample joint is arranged at one end of the movable rod;
The method is characterized in that:
The club head is provided with: a mechanical probe and a mechanical chip; the mechanical probe and the sample connector are arranged close to each other, and the mechanical probe and the sample connector are matched and used for extruding and powering up a sample; the mechanical chip is fixedly connected with the mechanical probe and is used for powering up the probe and measuring a force feedback signal from the mechanical probe;
The sample joint is provided with: the electric heating device is used for heating the sample joint and changing the temperature of the microenvironment of the sample joint area; meanwhile, the sample joint can be powered on and is matched with a powered mechanical probe for use: powering up the sample;
The mechanical chip comprises a stress part, a first electrode, a second electrode and a third electrode, wherein one end of the stress part is fixed with the mechanical probe; the stress part is arranged on the mechanical chip through a cantilever structure; electrodes with a feathered structure are arranged on two sides of the stress part; the electrode that is provided with the feather structure in the unilateral of first electrode the second electrode, the feather structure electrode of atress portion is crisscross with the feather structure electrode of first electrode, second electrode respectively and is set up, atress portion along the atress direction with the third electrode is close to the setting, works as atress portion is when receiving pressure, presents two kinds of states: the feather-shaped structure electrode of the stress part is parallel and close to the feather-shaped structure electrodes of the first electrode and the second electrode, and a pressure feedback signal is output; the stress part is in abutting connection with the third electrode, and the third electrode is used for powering up the stress part;
the sample joint is a needle tip or a sample carrier.
2. The transmission electron microscope force electrothermal in-situ sample rod according to claim 1, wherein: the electric heating device is a resistance wire, the resistance wire is arranged in an insulating way with the sample joint, and the resistance wire is led out through two electrodes arranged on the sample joint.
3. The transmission electron microscope force electrothermal in-situ sample rod according to claim 1, wherein: the head is also provided with: the circuit board is arranged at the groove on the surface of the club head; the contact pins are respectively lapped on the circuit board and the electrodes of the mechanical chip; the gland is used for fixing the circuit board and the mechanical chip on the rod head.
4. The transmission electron microscope force electrothermal in-situ sample rod according to claim 1, wherein: an electric rough adjusting module is arranged in the handle, and is connected with one end of the movable rod and used for carrying out three-dimensional movement control of micrometer-scale precision on the movable rod.
5. The transmission electron microscope force electrothermal in-situ sample rod according to claim 1, wherein: the movable rod comprises XY two-axis piezoelectric ceramics and Z-axis piezoelectric ceramics, and the XY two-axis piezoelectric ceramics and the Z-axis piezoelectric ceramics are used for carrying out three-dimensional movement control of nanometer precision on the sample joint.
6. The transmission electron microscope force electrothermal in-situ sample rod according to claim 4 or 5, wherein: and an O-shaped sealing ring is further arranged in the rod head and sleeved on the sample joint connecting seat and used for stabilizing movement of the sample joint and sealing of the sample rod.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011636775.XA CN112834539B (en) | 2020-12-31 | 2020-12-31 | Transmission electron microscope power electric heating in-situ sample rod |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011636775.XA CN112834539B (en) | 2020-12-31 | 2020-12-31 | Transmission electron microscope power electric heating in-situ sample rod |
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| CN112834539A CN112834539A (en) | 2021-05-25 |
| CN112834539B true CN112834539B (en) | 2024-07-12 |
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| CN114199903B (en) * | 2021-10-26 | 2024-04-05 | 清华大学 | Thermoelectric mechanical integrated transmission electron microscope double-inclined in-situ sample rod |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110441334A (en) * | 2019-07-11 | 2019-11-12 | 安徽泽攸科技有限公司 | A kind of more in situ TEM specimen holders |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002134052A (en) * | 2000-10-25 | 2002-05-10 | Jeol Ltd | Sample holder |
| CN102262996B (en) * | 2011-05-31 | 2013-06-12 | 北京工业大学 | Comprehensive test sample rod for double-shaft tilting in-situ force and electric property of transmission electron microscope |
| US9476816B2 (en) * | 2011-11-14 | 2016-10-25 | Hysitron, Inc. | Probe tip heating assembly |
| EP2847573B1 (en) * | 2012-05-08 | 2017-11-15 | E.A. Fischione Instruments, Inc. | Radiation-heated in-situ tem-specimen holder assembly |
| WO2014085630A1 (en) * | 2012-11-28 | 2014-06-05 | Hysitron Incorporated | Micromachined comb drive for quantitative nanoindentation |
| CN105301027B (en) * | 2015-11-22 | 2017-11-14 | 北京工业大学 | A kind of transmission/ESEM power, the experiment porch in situ of thermal coupling field loading |
| CN205691611U (en) * | 2016-06-08 | 2016-11-16 | 中国科学院宁波材料技术与工程研究所 | A kind of complete two transmission electron microscopes of warm area thermoelectricity specimen holder in situ |
| CN105823908B (en) * | 2016-06-08 | 2018-09-11 | 中国科学院宁波材料技术与工程研究所 | Full warm area two transmission electron microscope original position specimen holders of thermoelectricity |
| CN106057618B (en) * | 2016-08-03 | 2017-11-24 | 兰州大学 | The electric two transmission electron microscope original position specimen holders of expansible power |
| CN108550513B (en) * | 2018-05-25 | 2024-05-28 | 兰州大学 | Three-dimensional force transmission electron microscope in-situ sample rod |
| US11069507B2 (en) * | 2019-03-05 | 2021-07-20 | University Of Maryland, College Park | Radio-frequency (RF) transmission systems, devices, and methods for in situ transmission electron microscopy |
| CN110021512B (en) * | 2019-04-04 | 2022-02-08 | 北京工业大学 | Electrothermal sample rod system for in-situ liquid environment transmission electron microscope |
| CN210534032U (en) * | 2019-06-19 | 2020-05-15 | 中国科学院金属研究所 | An electron microscope in-situ mechanical property test chip |
| CN210514128U (en) * | 2019-08-26 | 2020-05-12 | 镇江乐华电子科技有限公司 | Transmission electron microscope in-situ electrical sample rod |
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| CN110441334A (en) * | 2019-07-11 | 2019-11-12 | 安徽泽攸科技有限公司 | A kind of more in situ TEM specimen holders |
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