CN117030755A - Method for applying temperature gradient field in transmission electron microscope - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 37
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- 238000011065 in-situ storage Methods 0.000 claims abstract description 51
- 238000012360 testing method Methods 0.000 claims abstract description 51
- 229910052721 tungsten Inorganic materials 0.000 claims description 53
- 239000010937 tungsten Substances 0.000 claims description 53
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 49
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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
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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
- G01N23/20—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
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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
- G01N23/20—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
- G01N23/20033—Sample holders or supports therefor provided with temperature control or heating means
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Abstract
The invention relates to a method for applying an in-situ temperature gradient field in a transmission electron microscope, comprising the steps of: (1) Fixing a test chip loaded with a micro-nano sample to be tested with an in-situ sample rod, and enabling the micro-nano sample to be tested and the sample rod to form a passage; (2) Inserting an in-situ sample rod into a transmission electron microscope and connecting an external direct current source; (3) And (3) introducing a preset direct current into the test chip to form Joule heat and conducting the Joule heat to the micro-nano sample to be tested, so as to realize the application of an in-situ temperature gradient field to the micro-nano sample to be tested. Compared with the prior art, the invention realizes that the temperature gradient field is applied to the sample to be tested in the transmission electron microscope in-situ test platform, and has the advantages of simple processing, wide temperature rising range, real-time and real-space observation and the like.
Description
Technical Field
The invention belongs to the technical field of micro-nano material temperature gradient field application, and particularly relates to a method for applying an in-situ temperature gradient field in a transmission electron microscope.
Background
Transmission electron microscopes are widely used in the fields of material science, biology, physics and chemistry as a micro-nano material analysis characterization device with extremely high temporal and spatial resolution. The transmission electron microscope in-situ characterization technology can realize real-time and real-space observation of dynamic behavior of material evolution under complex conditions such as force, heat, light and electricity, and can simultaneously acquire basic information corresponding to the material, including crystal configuration, crystal plane parameters, element types, distribution and the like, so that an extremely important reference is provided for revealing an evolution mechanism of the material under the action of an external field. Wherein, the temperature gradient is applied in the in-situ transmission electron microscope, which can effectively modulate the domain wall configuration and the domain wall movement of the magnetic material. However, the current method for applying the temperature field depends on a specially designed chip and a sample rod, and only a uniform and stable temperature field can be applied, in addition, the chip needs to process the sample extremely complicated, the experiment failure rate is high, and the research on in-situ temperature gradient experiment is limited. Therefore, a method for applying a temperature gradient field in situ, which is simple to process and wide in heating range, is needed to facilitate the development of subsequent researches.
Patent publication No. CN104815710B discloses a method for establishing a temperature gradient field in a micro-fluidic chip and a micro-channel and application thereof. The heating element with the heating area is formed by directly connecting wires on two long sides of a piece of rectangular ITO coated glass through conductive silver colloid. The ITO coated glass has good light transmittance and thermal uniformity, joule heat is generated by electrifying, various heating devices can be processed and integrated on a microfluidic chip, the optical observation of a chip system is not influenced, a settable temperature gradient field is realized, but the invention only refers to a temperature gradient interval of 23-45 ℃ and has a narrower range.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for applying a temperature gradient field in situ, which has simple processing and wide temperature rising range, so as to synchronously apply the temperature gradient field in situ to a micro-nano scale material, realize the research on temperature-driven magnetic domain walls and observe the continuous change of the material at different temperatures in real time.
The aim of the invention can be achieved by the following technical scheme:
a method of applying an in situ temperature gradient field in a transmission electron microscope, comprising the steps of:
(1) Fixing a test chip loaded with a micro-nano sample to be tested with an in-situ sample rod, and enabling the micro-nano sample to be tested and the sample rod to form a passage;
(2) Inserting an in-situ sample rod into a transmission electron microscope and connecting an external direct current source;
(3) And (3) introducing preset direct current to the U-shaped electrode connected with the sample at one side of the test chip, forming Joule heat at the U-shaped electrode, and conducting the Joule heat to the micro-nano sample to be tested, so as to realize the application of an in-situ temperature gradient field to the micro-nano sample to be tested.
Further, the loading process of the micro-nano sample to be tested on the test chip specifically comprises the following steps:
(a) Selecting a test material, depositing a carbon protective layer on the surface of the test material, etching to obtain a cuboid sample, and transferring and fixing the cuboid sample on a test chip;
(b) Adopting ion beam sprayed tungsten as a wire to form four deposition circuits, namely tungsten electrodes, so as to connect a cuboid sample with four chip electrodes of a test chip;
(c) Etching the surface of the cuboid sample to separate the four tungsten electrodes from each other;
(d) And (3) thinning the cuboid sample, ensuring that the sample can be observed in a transmission electron microscope, namely finishing the loading of the micro-nano sample to be detected on the test chip, and obtaining the sample/chip device.
Further, in the step (a), the carbon protective layer is an amorphous carbon layer having a thickness of 0.8 to 1.2 μm, preferably 1 μm.
Further, in the step (a), in order to ensure that there is enough space for depositing tungsten electrodes on the left and right sides of the sample, the left and right sides of the rectangular parallelepiped sample are left with a width of 3-5 μm, preferably 4 μm.
Further, in the step (b), the cuboid sample is parallel to the connection end of the test chip.
Further, in the step (b), the tungsten electrode has a thickness of 0.6 to 1.0. Mu.m, preferably 0.8. Mu.m.
Further, in the step (b), each tungsten electrode laid is connected to a corresponding chip electrode.
Further, in the step (c), the etching treatment process is as follows:
after depositing the tungsten electrodes, the ion beams are adopted to carry out penetration etching on the areas respectively positioned at the two ends of the cuboid sample, and the tungsten electrodes are separated from each other, so that U-shaped electrodes are respectively formed at the left side and the right side of the sample.
Further, a preferable distance between the two tungsten electrodes is 0.8 μm or more.
Further, in the step (d), the thinning process is as follows: and (3) carrying out etching thinning on the area of the cuboid sample, on which the electrode is not paved, so that the thickness of the area is 80-120nm, and preferably, the thickness is not more than 100nm.
Further, after the in-situ temperature gradient field is applied, the influence of the temperature gradient field on the in-situ test sample can be synchronously observed in the transmission electron microscope.
Compared with the prior art, the invention has the following advantages:
(1) Compared with the traditional complex heating chip, the preparation of the sample has extremely high requirements and can only provide a stable temperature field. The invention provides a micro-nano sample processing method with simple process and rich functions, which can accurately process a sample and can realize flexible application of a sample temperature gradient field.
(2) In the invention, through the U-shaped electrode at one side of the sample, joule heat is generated at the U-shaped electrode, and heat energy is transferred to one side of the sample through heat conduction, so that the temperature is increased, and finally, a temperature gradient is formed. And the prepared U-shaped electrode is directly connected with the sample, so that the heat transfer efficiency is extremely high.
(3) The invention can provide real-time, real-space high-resolution observation of the magnetic domain/magnetic structure of the material with the temperature field change under the condition of applying the temperature gradient field;
(4) The tungsten electrode adopted in the invention can realize the application of an extremely high upper limit temperature gradient field and cover the working temperature of most ferromagnetic materials;
(5) According to the invention, the magnitude and the direction of the applied temperature gradient field can be adjusted by changing the magnitude and the direction of the current injected into the single-side U-shaped electrode of the sample according to the requirements of a user, so that various experimental scenes are satisfied.
Drawings
FIG. 1 is a schematic diagram of the carbon overcoat process of example 1;
FIG. 2 is a schematic diagram of a sample cuboid for example 1 transferred and fixed to an in situ test chip port;
FIG. 3 is a schematic diagram showing the connection of a cuboid sample and an in-situ test chip according to example 1 via tungsten electrodes;
FIG. 4 is a schematic diagram of a single-sided applied thermal gradient field of example 1;
FIG. 5 is a schematic diagram of the temperature gradient of the micro-nano-scale test sample of example 1.
The figure indicates:
1-carbon protective layer, 2-cuboid sample, 3-tungsten electrode I, 4-tungsten electrode II, 5-tungsten electrode III, 6-tungsten electrode IV, 7-chip electrode I, 8-chip electrode II, 9-chip electrode III, 10-chip electrode IV, 11-etched region I, 12-etched region II, 13-etched region III, 14-separated region I, 15-separated region II, 16-separated region III, 17-separated region IV.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following embodiments or examples, the in-situ test chip is prepared by referring to patent CN209495986U, and the in-situ sample rod is a Gatan company four-electrode low-temperature sample rod, and the Model is Gatan Model 613. The remainder, unless specifically stated, is indicative of a conventional feedstock or conventional processing technique in the art.
In order to synchronously apply an in-situ temperature gradient field to a micro-nano scale material so as to realize the research on a temperature-driven magnetic domain wall and observe the continuous change of the material at different temperatures in real time, the invention provides a method for applying the in-situ temperature gradient field in a transmission electron microscope, which comprises the following steps:
(1) Fixing a test chip loaded with a micro-nano sample to be tested with an in-situ sample rod, and enabling the micro-nano sample to be tested and the sample rod to form a passage;
(2) Inserting an in-situ sample rod into a transmission electron microscope and connecting an external direct current source;
(3) And (3) introducing preset direct current to the U-shaped tungsten electrode connected with the sample at one side of the test chip, forming Joule heat at the U-shaped electrode, and conducting the Joule heat to the micro-nano sample to be tested, so as to realize the application of an in-situ temperature gradient field to the micro-nano sample to be tested.
In some embodiments, referring to fig. 1 to 3, the loading process of the micro-nano sample to be tested on the test chip is specifically:
(a) Selecting a test material, depositing a carbon protective layer on the surface of the test material, etching to obtain a cuboid sample, and transferring and fixing the cuboid sample on a test chip;
(b) Adopting ion beam sprayed tungsten as a wire to form four deposition circuits, namely tungsten electrodes (respectively) so as to connect a cuboid sample with four chip electrodes of a test chip;
(c) Etching the surface of the cuboid sample to separate the four tungsten electrodes from each other;
(d) And (3) thinning the cuboid sample, ensuring that the sample can be observed in a transmission electron microscope, namely finishing the loading of the micro-nano sample to be detected on the test chip, and obtaining the sample/chip device.
In a more specific embodiment, in the step (a), the carbon protection layer is an amorphous carbon layer, and the thickness is 0.8-1.2 μm.
In a more specific embodiment, in the step (a), in order to ensure that the left and right sides of the sample have enough space for depositing tungsten electrodes, the rectangular parallelepiped sample is left with a width of 3-5 μm, preferably 4 μm, along the left and right sides of the long axis.
In a more specific embodiment, in step (b), the cuboid sample is kept parallel to the connection terminals of the test chip.
In a more specific embodiment, in the step (b), the tungsten electrode has a thickness of 0.6 to 1.0 μm.
In a more specific embodiment, in step (b), each tungsten electrode laid down is connected to a corresponding chip electrode.
In a more specific embodiment, in the step (c), the etching treatment process is as follows:
after depositing the tungsten electrodes, the ion beams are adopted to carry out penetration etching on the areas respectively positioned at the two ends of the cuboid sample, and the tungsten electrodes are separated from each other, so that U-shaped electrodes are respectively formed at the left side and the right side of the sample.
Still more preferably, the preferred distance between the two tungsten electrodes is 0.8 μm or more.
In a more specific embodiment, in the step (d), the thinning process is as follows: and (3) carrying out etching thinning on the area of the cuboid sample, on which the electrode is not paved, so that the thickness of the area is 80-120nm.
In some embodiments, the effect of the temperature gradient field on the in situ test sample can be observed simultaneously in the transmission electron microscope after the application of the in situ temperature gradient field.
The above embodiments may be implemented singly or in any combination of two or more.
The above embodiments are described in more detail below in connection with specific examples.
Example 1
First, as shown in fig. 1, amorphous carbon protective layer 1 is first deposited on the surface of a test material by means of electron beam and ion beam induced deposition, so as to prevent damage to the test material by the ion beam during the subsequent etching process, wherein carbon protective layer 1 is an amorphous carbon layer with a thickness of about 1 μm. The test material is made to face the ion beam, and the ion beam with acceleration voltage of 30kV and beam intensity of 9.3nA is adopted to etch the two sides of the test material, so as to obtain a cuboid sample 2. After etching was completed, the sample stage was tilted ±1° under a view angle against the ion beam, the beam current intensity was switched to 0.79nA, and rough repair was performed on both sides of the exposed sample. After the rough repair operation is finished, the cuboid sample 2 is opposite to the electron beam through the rotary sample table, U-cutting operation (namely, all the left side, the lower side and the right side parts of the sample connected with the matrix are cut off) is carried out on the cuboid sample 2 in an ion beam window, and the U-cutting depth is 4 mu m. At this time, a manipulator and a platinum needle are inserted, the manipulator is moved to align with the position of the cuboid sample 2, and the cuboid sample 2 and the manipulator are connected by ion beam induced deposition of platinum. Then, the sample stage is rotated and moved to enable the in-situ test chip to be parallel to the horizontal plane, then the cuboid sample 2 on the manipulator is transferred to the in-situ test chip, and then the right part of the cuboid sample 2 is etched, so that the horizontal plane of the cuboid sample 2 is parallel to the plane of the in-situ test chip.
And secondly, rotating the sample stage, properly moving the mechanical arm to enable the cuboid sample 2 to be close to and touch the end face of the in-situ test chip, enabling the cuboid sample 2 and the in-situ test chip to face the ion beam window, and connecting the cuboid sample 2 and the in-situ test chip through ion beam induced deposition of tungsten, as shown in fig. 2. And two deposition circuits, namely tungsten electrodes (tungsten electrode one 3, tungsten electrode two 4, tungsten electrode three 5 and tungsten electrode four 6), are respectively deposited on two sides of the sample on the basis, specifically, tungsten sprayed by an ion beam is used as a wire, and the width and the thickness of the sprayed tungsten electrodes are all 0.8 mu m. The tungsten electrode tip is connected to the corresponding preset electrode of the chip (i.e., chip electrode one 7, chip electrode two 8, chip electrode three 9, chip electrode four 10), as shown in fig. 3. The accelerating voltage of the ion beam is adjusted to be 30kV, the intensity is 0.23nA, the rectangle 2 is modified close to the lower end part of the chip, and the etching areas (the first etching area 11, the second etching area 12 and the third etching area 13) between the tungsten electrodes are removed,as shown in the figure 3 of the drawings,therefore, the four tungsten electrodes are all separated, and a thin area with tungsten on the surface is avoided, so that short circuit is formed and the test is influenced.
And thirdly, etching tungsten electrodes on two sides of the cuboid sample 2 through an ion beam (acceleration voltage is 30kV, beam intensity is 80 pA), tilting the cuboid sample 2 for thinning, thinning the sample to 100nm, separating to obtain a separation region (namely, a first separation region 14, a second separation region 15, a third separation region 16 and a fourth separation region 17 shown in fig. 2 and 3 are formed), enabling two tungsten electrodes on two sides to be independent of each other, and completing integral processing to obtain the sample/chip device.
And fourthly, mounting the sample/chip device on a corresponding in-situ test sample rod, and connecting the in-situ test sample/chip device with the sample/chip device through an enameled wire to ensure that the whole device is in a passage state.
And fifthly, connecting an in-situ test sample rod with an external direct current source, injecting current with preset intensity and action time (the action time of the current is preferably not more than 80ns, the current intensity can be set by a user according to the bearable temperature region of a specific sample) through a tungsten electrode I3 and a chip electrode I7, outputting the current through a tungsten electrode II 4 and a chip electrode II 8, starting an electron beam to observe the position of a chip device after generating a heat-induced temperature gradient field on one side of the sample, and obtaining data related to the temperature gradient of the single-side applied temperature gradient field and the micro-nano scale test sample.
Fig. 4 is a schematic diagram showing a simulation of the generation of a sample temperature gradient field due to the temperature rise caused by joule heat and the heat conduction after the current is injected into the left side U-shaped tungsten electrode of the sample. In the figure, electrodes on two sides of a sample are simple tungsten substances, and the sample is pure iron. The left side is a high temperature region, the highest temperature is 135K, the right side is a low temperature region, the temperature gradient of the temperature gradient is in a descending trend from the hot end, and the lowest temperature is the ambient temperature set in the transmission electron microscope and is about 100K.
Fig. 5 shows the effect of different current application times, voltage (current) intensities, tungsten electrode thicknesses and sample thicknesses on the application of a temperature gradient field, respectively, were designed on the basis of example 1. As a result, it was found that the current application time and voltage are the main influencing factors of the temperature gradient field size, and that the longer the current application time, the larger the voltage field, the larger the temperature gradient field, while the overall influence is smaller for the tungsten electrode thickness as well as the sample thickness, and the temperature gradient gradually decreases as the sample thickness increases.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. A method of applying an in situ temperature gradient field in a transmission electron microscope, comprising the steps of:
(1) Fixing a test chip loaded with a micro-nano sample to be tested with an in-situ sample rod, and enabling the micro-nano sample to be tested and the sample rod to form a passage;
(2) Inserting an in-situ sample rod into a transmission electron microscope and connecting an external direct current source;
(3) And (3) introducing a preset direct current into the test chip to form Joule heat and conducting the Joule heat to the micro-nano sample to be tested, so as to realize the application of an in-situ temperature gradient field to the micro-nano sample to be tested.
2. The method for applying an in-situ temperature gradient field in a transmission electron microscope according to claim 1, wherein the loading process of the micro-nano sample to be tested on the test chip is specifically as follows:
(a) Selecting a test material, depositing a carbon protective layer on the surface of the test material, etching to obtain a cuboid sample, and transferring and fixing the cuboid sample on a test chip;
(b) Adopting ion beam sprayed tungsten as a wire to form four deposition circuits, namely tungsten electrodes, so as to connect a cuboid sample with four chip electrodes of a test chip;
(c) Etching the surface of the cuboid sample to separate the four tungsten electrodes from each other;
(d) And (3) thinning the cuboid sample, ensuring that the sample can be observed in a transmission electron microscope, namely finishing the loading of the micro-nano sample to be detected on the test chip, and obtaining the sample/chip device.
3. The method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 2, wherein in step (a), the carbon protective layer is an amorphous carbon layer having a thickness of 0.8 to 1.2 μm.
4. A method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 2, wherein in step (a), the rectangular parallelepiped sample is left with a width of 3 to 5 μm on both sides in the long axis direction.
5. A method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 2, wherein in step (b), the cuboid sample is held parallel to the connection ends of the test chip.
6. A method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 2, wherein in step (b), the tungsten electrode has a thickness of 0.6 to 1.0 μm.
7. A method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 2 wherein in step (b), each tungsten electrode laid down is connected to a corresponding chip electrode.
8. A method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 2, wherein in step (c), the etching process is:
after depositing the tungsten electrodes, carrying out penetration etching on the regions respectively positioned at the two ends of the cuboid sample by adopting ion beams, and separating the tungsten electrodes from each other, thereby forming U-shaped electrodes on the left side and the right side of the micro-nano sample to be detected.
9. The method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 8, wherein a distance between two tungsten electrodes is 0.8 μm and above.
10. A method of applying an in situ temperature gradient field in a transmission electron microscope as set forth in claim 2, wherein in step (d), the thinning process is: and (3) carrying out etching thinning on the area of the cuboid sample, on which the electrode is not paved, so that the thickness of the area is 80-120nm.
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| CN202311252525.XA CN117030755A (en) | 2023-09-26 | 2023-09-26 | Method for applying temperature gradient field in transmission electron microscope |
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