CN213544440U - Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip - Google Patents
Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip Download PDFInfo
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- CN213544440U CN213544440U CN202022337061.0U CN202022337061U CN213544440U CN 213544440 U CN213544440 U CN 213544440U CN 202022337061 U CN202022337061 U CN 202022337061U CN 213544440 U CN213544440 U CN 213544440U
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Abstract
The utility model relates to a transmission electron microscope high resolution in-situ suspended temperature difference pressurizing chip, which comprises a substrate, wherein two sides of the substrate are covered with insulating layers, the middle part of the substrate is provided with a central window, the central window is arranged in a suspended way, and the central window is also covered with a supporting layer; the supporting layer in the central window is provided with two heating wires which are arranged in a bilateral symmetry manner and two pressurizing circuits which are arranged in an up-down symmetry manner, and the two pressurizing circuits are positioned in a gap between the two heating wires; each heating wire is connected with four heating electrodes, and each heating electrode is connected to different positions of the heating wire through a heating circuit; each pressurizing circuit is connected with a pressurizing electrode, each pressurizing electrode is connected with the corresponding pressurizing circuit through a pressurizing circuit, and the chip can simultaneously realize the temperature difference and pressurizing functions.
Description
Technical Field
The utility model relates to an in situ characterization field specifically relates to a transmission electron microscope high-resolution in situ suspension formula difference in temperature pressurization chip.
Background
The in-situ transmission electron microscope technology is widely applied to various scientific fields by the advantages of ultrahigh spatial resolution (atomic scale) and ultrafast time resolution (millisecond scale), and provides a brand new thought and research method for researchers to explore the microstructure of a novel material. The method is mainly characterized in that a visual window is built in an electron microscope, external field effects such as a thermal field, an optical field, an electrochemical field and the like are introduced, and real-time dynamic in-situ test is carried out on a sample. Researchers can capture the dynamic induction of the sample to the environment through an in-situ testing technology, wherein the dynamic induction comprises important information such as size, form, crystal structure, atomic structure, chemical bond, heat energy change and the like. The morphological change of the material at the atomic scale under the action of the external field becomes the root of the research and development of the material. Can be widely used for microstructure analysis, observation of nano material research and the like, and has extremely high application value in the aspects of biology, materials and semiconductor electronic materials.
The existing temperature difference chip also has the defects of low temperature rise and drop rate, insufficient temperature measurement and control accuracy, lower resolution, high sample drift rate, incapability of realizing temperature difference and pressurization functions simultaneously, inconvenience in sample placement and the like, so that the existing temperature difference chip is necessary to be improved.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a transmission electron microscope high resolution normal position suspension type difference in temperature pressurization chip that can realize the difference in temperature and pressurize the function simultaneously.
The specific scheme is as follows:
a transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip comprises a substrate, wherein two sides of the substrate are covered with insulating layers, the middle part of the substrate is provided with a central window, the central window is arranged in a suspended mode, and a supporting layer made of a transparent film is covered on the central window; the supporting layer in the central window is provided with two heating wires which are arranged in a bilateral symmetry manner and two pressurizing circuits which are arranged in an up-down symmetry manner, and the two pressurizing circuits are positioned in a gap between the two heating wires; each heating wire is connected with four heating electrodes, and each heating electrode is connected to different positions of the heating wire through a heating circuit; each pressurizing circuit is connected with a pressurizing electrode, and each pressurizing electrode is connected with the corresponding pressurizing circuit through a pressurizing line.
Preferably, a plurality of heat insulation holes are further arranged in the gap between the two heating wires.
Preferably, the middle part of each pressurizing electrode is provided with a notch part extending along the vertical direction, and the heat insulation holes are uniformly distributed in the notch parts of the two pressurizing electrodes along the vertical direction.
Preferably, the heat insulation hole is a square hole.
Preferably, four heating electrodes of each heating electrode form two groups of equivalent circuits, the two groups of equivalent circuits are respectively controlled by using a single current source meter and a single voltage source meter, one of the two groups of equivalent circuits is responsible for supplying power and heating, and the other group of equivalent circuits is responsible for monitoring the resistance value of the heating wire after heating in real time.
Preferably, each of the voltage-applying circuits is provided with a set of equivalent circuits to realize the voltage difference.
Preferably, the substrate is a silicon substrate, the insulating layer is a silicon nitride or silicon oxide insulating layer, the thickness of the silicon nitride or silicon oxide insulating layer is 0.5-5um, and the thickness of the substrate is 50-500 um.
Preferably, the external dimension of the transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip is 2mm by 2mm to 10mm by 10mm or 4mm by 8 mm.
The utility model provides a transmission electron microscope high-resolution normal position suspension type difference in temperature pressurization chip compares with prior art and has following advantage: the transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip provided by the utility model can implement different temperatures at two ends of a carried sample, can also apply different voltages to the sample, and can research solid materials under stimulation of two external fields with different temperatures and voltages; the temperature control device has the advantages of rapid temperature rise and drop, high resolution, accurate temperature measurement and control, realization of temperature difference and pressurization functions, convenience in sample placement and low sample drift rate.
Drawings
FIG. 1 shows a top view of a transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip.
FIG. 2 shows an enlarged view of a central window of a transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip.
FIG. 3 shows a front view of a high-resolution in-situ suspended temperature difference pressurizing chip of a transmission electron microscope.
Detailed Description
To further illustrate the embodiments, the present invention provides the accompanying drawings. The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the embodiments. With these references, one of ordinary skill in the art will appreciate other possible embodiments and advantages of the present invention. Elements in the figures are not drawn to scale and like reference numerals are generally used to indicate like elements.
The present invention will now be further described with reference to the accompanying drawings and detailed description.
Example 1
As shown in fig. 1-3, the present embodiment provides a transmission electron microscope high resolution in-situ suspended type temperature difference pressurizing chip, which includes a substrate 1, and an insulating layer 10 is covered on both the front surface and the back surface of the substrate 1. In this embodiment, the substrate is a silicon substrate, and the insulating layer is a silicon nitride or silicon oxide insulating layer.
The substrate 1 has a central window 11 in the middle, the central window 11 is suspended, and a supporting layer 10 'is covered on the central window 11, the supporting layer 10' is a silicon nitride layer or a silicon oxide layer.
The supporting layer in the central window 11 has two heating wires 12 symmetrically arranged left and right and two pressurizing circuits 13 symmetrically arranged up and down, and the two pressurizing circuits 13 are located in the gap between the two heating wires 12.
Wherein, the heating wire 12 is a spiral annular arc heating wire, and gaps are left between the arc heating wires and are not connected with each other; each heating wire 12 is connected with four heating electrodes 121, the four heating electrodes 121 are distributed on the same side edge of the substrate 1, and the eight heating electrodes 121 of the two heating wires 12 are respectively arranged on the left and right side edges of the substrate 1. Each heating electrode 121 is connected to different positions of the heating wire 12 through a heating circuit 122, and the four heating electrodes enable the heating wire to form two groups of equivalent circuits which are respectively controlled by using a separate current source meter and a separate voltage source meter; one of the two equivalent circuits is responsible for power supply and heating, and the other circuit is responsible for monitoring the resistance value of the heating wire after heating in real time.
Each pressurizing circuit 13 is connected with a pressurizing electrode 131, and the two pressurizing electrodes 131 of the two pressurizing circuits 13 are respectively arranged on the upper and lower edges of the substrate. Each pressurizing electrode 131 is connected to the corresponding pressurizing circuit 13 through a pressurizing line. Preferably, the two voltage-applying circuits are respectively provided with a set of equivalent circuits to realize the voltage difference.
In this embodiment, a plurality of heat insulation holes 14 are further disposed in the gap between the two heating wires 12 to reduce the mutual influence between the temperatures of the two heating wires 12 and improve the accuracy of temperature measurement and control.
Preferably, each of the pressurizing circuits 13 has a notch extending in the vertical direction at the middle thereof, and the heat-insulating holes 14 are uniformly distributed in the notches of the two pressurizing circuits 13 in the vertical direction.
More preferably, the insulation hole 14 has a square shape.
In this embodiment, the chip external dimension of the transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip is 2mm × 2mm to 10mm × 10 mm; preferably, the chip has a dimension of 4mm by 8 mm.
In this embodiment, the thickness of the silicon nitride or silicon oxide insulating layer is 0.5-5um, and the thickness of the substrate is 50-500 um.
In this embodiment, the central window is a square central window. Preferably, the size of the square central window is 0.5mm by 0.5mm to 1mm by 1 mm; more preferably, the size of the square central window is 0.8mm by 0.8 mm.
In this embodiment, the arc heating wire of the heating layer has an outer diameter of 0.15-0.5mm and a thickness of 50-500 nm. Preferably, the heating wire is made of metal gold, platinum, palladium, rhodium, molybdenum, tungsten, platinum-rhodium alloy or nonmetal molybdenum carbide.
In this embodiment, the pressurizing circuit has a size of 2um x 150um to 5um x 300um and a thickness of 50 to 500 nm. Preferably, the pressurizing circuit is made of metal gold, platinum, palladium, rhodium, molybdenum, tungsten, platinum-rhodium alloy or nonmetal molybdenum carbide.
The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip provided by the embodiment can be prepared by the following method, and comprises the following steps:
s1, preparing a Si (100) wafer A with silicon nitride or silicon oxide layers on two sides, wherein the thickness of the silicon nitride or silicon oxide layer is 0.5-5um, and the thickness of a silicon wafer is 50-500 um;
s2, transferring the central window pattern from the photoetching mask plate to any surface of the wafer A by utilizing a photoetching process, taking the surface as a back surface, and developing in a positive photoresist developing solution to obtain a wafer A-1;
preferably, the photoetching process is exposure in a hard contact mode of an ultraviolet photoetching machine; the photoresist used in the photoetching process is AZ 5214E; the development time was 65 s;
more preferably, the exposure time is 20 s;
s3, etching the silicon nitride layer or the silicon oxide layer at the central window on the silicon nitride layer on the back of the wafer A-1 by using a reactive ion etching process, then placing the wafer with the back facing upwards into acetone for soaking, finally washing with acetone, and removing photoresist to obtain a wafer A-2;
s4, placing the wafer A-2 with the back side facing upwards into a potassium hydroxide solution for wet etching until only a thin film window is left on the front side, taking out the wafer A-2, washing the wafer A-2 with a large amount of deionized water, and then drying the wafer A-3 by blowing to obtain a wafer A-3;
preferably, the mass percentage concentration of the potassium hydroxide solution is 20%; the etching temperature is 70-90 ℃, and the etching time is 1.5-4 h;
more preferably, the etching temperature is 80 ℃; the etching time is 2 h;
s5, transferring patterns of a heating wire, a pressurizing circuit, a heating electrode, a pressurizing electrode, a heating circuit and a pressurizing circuit from a photoetching mask plate to the front side of the wafer A-3 by utilizing a photoetching process, developing in positive photoresist developing solution, and washing and cleaning the surface by using deionized water to obtain a wafer A-4;
preferably, the photoetching process is exposure in a hard contact mode of an ultraviolet photoetching machine, and the photoresist used in the photoetching process is AZ 5214E; the development time was 50 s;
more preferably, the exposure time is 15 s;
preferably, the heating wire is an arc heating wire, the outer diameter of the heating wire is 0.15-0.5mm, and the thickness of the heating wire is 50-500 nm;
s6, evaporating a layer of metal film on the front side of the wafer A-4 by using electron beam evaporation, then putting the wafer A-4 with the front side facing upwards into acetone for soaking and stripping, finally washing with deionized water, removing the photoresist, and leaving the conductive layer corresponding to the pattern in the step S5 to obtain a wafer A-5;
preferably, the material of the conducting layer is metal gold, platinum, palladium, rhodium, molybdenum, tungsten, platinum-rhodium alloy or nonmetal molybdenum carbide; the thickness of the conducting layer is 50-500 nm;
s7, constructing a small hole pattern of a central window on the front surface of the wafer A-5 by utilizing an ultraviolet laser direct writing photoetching process, developing in a positive photoresist developing solution, and washing and cleaning the surface by using deionized water to obtain a wafer A-6;
preferably, the photoresist used in the ultraviolet laser direct writing process is AZ 5214E; the output power is 260W/us;
s8, etching silicon nitride or silicon oxide at the small hole on the back of the wafer A-6 by using a reactive ion etching process, then putting the wafer A-6 with the front side facing upwards into acetone for soaking, finally washing with acetone, and removing photoresist to obtain a wafer A-7;
preferably, the size of the pores is 3um by 30um to 5um by 50 um;
and S9, carrying out laser scribing on the wafer A-7, and dividing the wafer into independent chips.
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 detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The utility model provides a transmission electron microscope high resolution normal position suspended type difference in temperature pressurization chip which characterized in that: the device comprises a substrate with two sides covered by insulating layers, wherein the middle part of the substrate is provided with a central window which is arranged in a suspended manner and is covered by a supporting layer made of a transparent film; the supporting layer in the central window is provided with two heating wires which are arranged in a bilateral symmetry manner and two pressurizing circuits which are arranged in an up-down symmetry manner, and the two pressurizing circuits are positioned in a gap between the two heating wires; each heating wire is connected with four heating electrodes, and each heating electrode is connected to different positions of the heating wire through a heating circuit; each pressurizing circuit is connected with a pressurizing electrode, and each pressurizing electrode is connected with the corresponding pressurizing circuit through a pressurizing line.
2. The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip as claimed in claim 1, characterized in that: a plurality of heat insulation holes are also arranged in the gap between the two heating wires.
3. The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip as claimed in claim 2, characterized in that: the middle part of each pressurizing circuit is provided with a notch part which extends along the up-down direction, and the heat insulation holes are uniformly distributed in the notch parts of the two pressurizing circuits along the up-down direction.
4. The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip as claimed in claim 2, characterized in that: the heat insulation holes are square holes.
5. The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip as claimed in claim 1, characterized in that: the four heating electrodes of each heating electrode form two groups of equivalent circuits, the two groups of equivalent circuits are respectively controlled by using a single current source meter and a voltage source meter, one of the two groups of equivalent circuits is responsible for supplying power and heating, and the other group of equivalent circuits is responsible for monitoring the resistance value of the heating wire after heating in real time.
6. The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip as claimed in claim 1, characterized in that: each pressurizing circuit is provided with a group of equivalent circuits respectively so as to realize voltage difference.
7. The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip as claimed in claim 1, characterized in that: the substrate is a silicon substrate, the insulating layer is a silicon nitride or silicon oxide insulating layer, the thickness of the silicon nitride or silicon oxide insulating layer is 0.5-5um, and the thickness of the substrate is 50-500 um.
8. The transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip as claimed in claim 1, characterized in that: the chip external dimension of the transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip is 2mm x 2mm-10mm x 10mm or 4mm x 8 mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202022337061.0U CN213544440U (en) | 2020-10-20 | 2020-10-20 | Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip |
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| CN202022337061.0U CN213544440U (en) | 2020-10-20 | 2020-10-20 | Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112129786A (en) * | 2020-10-20 | 2020-12-25 | 厦门大学 | Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip and preparation method thereof |
| WO2022082989A1 (en) * | 2020-10-20 | 2022-04-28 | 厦门大学 | High-resolution in-situ temperature difference and pressurization chip in transmission electron microscope and preparation method therefor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112129786A (en) * | 2020-10-20 | 2020-12-25 | 厦门大学 | Transmission electron microscope high-resolution in-situ suspended temperature difference pressurizing chip and preparation method thereof |
| WO2022082989A1 (en) * | 2020-10-20 | 2022-04-28 | 厦门大学 | High-resolution in-situ temperature difference and pressurization chip in transmission electron microscope and preparation method therefor |
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