CN107170794B - Chip applied to TEM for in-situ electrochemical reaction measurement - Google Patents
Chip applied to TEM for in-situ electrochemical reaction measurement Download PDFInfo
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- CN107170794B CN107170794B CN201610130211.6A CN201610130211A CN107170794B CN 107170794 B CN107170794 B CN 107170794B CN 201610130211 A CN201610130211 A CN 201610130211A CN 107170794 B CN107170794 B CN 107170794B
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- 238000003487 electrochemical reaction Methods 0.000 title claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 title abstract description 13
- 238000005259 measurement Methods 0.000 title abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 230000002093 peripheral effect Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000000149 penetrating effect Effects 0.000 abstract description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000010894 electron beam technology Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0603—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by particular constructional design considerations, e.g. for preventing surface leakage, for controlling electric field concentration or for internal isolations regions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0684—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape, relative sizes or dispositions of the semiconductor regions or junctions between the regions
Abstract
The invention discloses a chip applied to TEM (transverse electric and magnetic field) for in-situ electrochemical reaction measurement, which comprises a substrate, a first electrode and a second electrode, wherein the first electrode and the second electrode are arranged on the upper end surface of the substrate, the first electrode is provided with an opening part, one end part of the second electrode is provided with more than one observation window penetrating through the second electrode, at least one end part of the second electrode is arranged in the opening part, and the second electrode and the first electrode are not in direct contact. The chip has simple structure, easy manufacture, accurate control of the distance between the two electrodes, high yield and stable performance, and simultaneously, the observation electrode is provided with a plurality of windows, the edges of the windows are observation points, the observation points are more, and samples can be easily searched.
Description
Technical Field
The invention relates to a liquid chip, in particular to a chip applied to TEM for in-situ electrochemical reaction measurement.
Background
A Transmission Electron Microscope (TEM) uses a focused electron beam as an illumination source, and uses a thin film sample transparent to the electron beam to analyze the microstructure inside the sample in an image formed by a transmission electron beam or a diffraction electron beam transmitted through the sample. TEM is an effective tool for observing and analyzing the morphology, organization and structure of materials, and has been widely used in scientific research and industrial fields. With the development of technology, only obtaining information such as material atomic-level high resolution, sample surface morphology, chemical element energy spectrum and the like cannot meet the needs of people, and research and development personnel hope to see the whole reaction or biological growth process. Therefore, a TEM in-situ test technology is generated, namely, the target to be tested is placed in the original system for TEM detection in real time and on line.
The researchers such as the Cong Youcai designed a TEM in-situ electrochemical chip (see FIG. 1), and studied the reaction mechanism of the chip on a lithium-sulfur battery. However, when the chip is used, a gold wire needs to be manually arranged between two electrodes, the distance between the gold wire and a counter electrode is about 40 micrometers after the gold wire is arranged, the operation is difficult, the yield is low, in addition, observation points are only distributed on the gold wire, the number of sample testing points is relatively small, and an ideal sample is not easy to find for observation.
Disclosure of Invention
The main object of the present invention is to provide a chip for in-situ electrochemical reaction measurement in TEM, by which a battery and a capacitor can be conveniently assembled to work normally, and the shortcomings of the prior art can be overcome.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the embodiment of the invention discloses a chip applied to TEM (transverse electric and magnetic field) for carrying out in-situ electrochemical reaction measurement, which comprises a substrate, a first electrode and a second electrode, wherein the first electrode and the second electrode are arranged on the upper end surface of the substrate, the first electrode is provided with an opening part, one end part of the second electrode is provided with more than one observation window penetrating through the second electrode, at least one end part of the second electrode is arranged in the opening part, and the second electrode is not in direct contact with the first electrode.
In some embodiments, the chip comprises an electrode layer formed on the substrate, the electrode layer comprising the first electrode and the second electrode.
Furthermore, an insulating layer is distributed between the electrode layer and the substrate.
Further, the second electrode has more than two observation windows.
For example, the second electrode has 1 to 500 observation windows.
In some embodiments, the observation window vertically penetrates through the second electrode, and the observation window has a trapezoidal cross section, and the included angle between the inner wall of the observation window and the horizontal plane is 20-70 degrees.
In some embodiments, within the opening, a distance between an outer peripheral edge portion of the second electrode and an inner peripheral edge portion of the opening is 1 to 3000 μm.
In some embodiments, the second electrode is distributed entirely within the opening.
Wherein the first electrode is a counter electrode and the second electrode is an observation electrode.
In some embodiments, the substrate comprises a P-type, N-type, or intrinsic silicon wafer, but is not so limited.
In some embodiments, the material of the insulating layer includes, but is not limited to, silicon oxide, silicon nitride, or aluminum oxide.
Compared with the prior art, the invention has the advantages that:
(1) the chip applied to the TEM for in-situ electrochemical reaction measurement is simple in structure and easy to manufacture, the distance between the two electrodes can be accurately controlled, the yield is high, the performance is stable, meanwhile, the observation electrode is provided with a plurality of windows, the edges of the windows are observation points, the observation points are more, and a sample is easier to search;
(2) when the chip applied to TEM for in-situ electrochemical reaction measurement works, only the anode and the cathode are respectively placed at the window of the observation electrode and on the counter electrode, and the observation can be carried out after the electrolyte is dripped between the two electrodes, so that the operation is simple.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of an application of a prior TEM in-situ electrochemical chip;
FIG. 2 is a top view of a chip for use in a TEM for in-situ electrochemical reaction measurements, according to an exemplary embodiment of the present invention;
FIG. 3 is a schematic diagram of the electrode structure in the chip shown in FIG. 2;
FIG. 4 is a cross-sectional view of a window in the chip of FIG. 2;
FIG. 5 is a front view of the chip shown in FIG. 2;
description of reference numerals: the chip comprises a chip base body 10, an electrode 20, an electrode 30, a gold wire 40, a substrate 1, an electrode layer 2, a first electrode 21, a second electrode 22, a window 3 and an insulating layer 4.
Detailed Description
For a further understanding of the present invention, reference will now be made in detail to the following examples. It should be noted that those skilled in the art can modify the process parameters appropriately according to the contents of the disclosure. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the invention has been described in terms of preferred embodiments, it will be apparent to those skilled in the art that the techniques of the invention can be implemented and applied by modifying or appropriately combining the applications described herein without departing from the spirit, scope and spirit of the invention.
Referring to fig. 5, the present embodiment discloses a chip for performing in-situ electrochemical reaction measurement by TEM, which includes a substrate 1 and an electrode layer 2 disposed on an upper end surface of the substrate, wherein an insulating layer 4 is further disposed between the electrode layer 2 and the substrate 1.
The substrate 1 may be a silicon wafer, such as a P-type, N-type, intrinsic silicon wafer, or the like.
Wherein, the insulating layer can be silicon oxide, silicon nitride, aluminum oxide and other insulating layers.
The material of the electrode can be one or more of gold, copper, aluminum, alloy and other conductive metals.
The insulating layer may be formed by physical vapor deposition, chemical vapor deposition, or the like, which are known in the art.
Wherein the electrodes may be formed by sputtering, physical/chemical vapor deposition, and the like in a manner known in the art.
Further, the electrode layers include a first electrode 21 (counter electrode) and a second electrode 22 (observation electrode).
The first electrode has an opening, one end of the second electrode has more than one observation window penetrating through the second electrode, at least one end of the second electrode is arranged in the opening, and the second electrode is not in direct contact with the first electrode.
For example, referring to fig. 2-3, the second electrodes 22 are entirely distributed in the openings of the first electrodes 21.
Further, in the opening, a distance between an outer peripheral edge of the second electrode and an inner peripheral edge of the opening is 1 to 3000 μm. For example, referring to FIG. 3, d1 is 1-3000 microns, d2 is 1-3000 microns, and d3 is 1-3000 microns.
Further, the second electrode has more than one observation window, preferably 1-500 observation windows.
Further, the observation window may have a square shape, a circular shape, an irregular shape, or the like.
Referring to fig. 4, the observation window vertically penetrates through the second electrode, and the observation window has a trapezoidal cross section, and an included angle between an inner wall of the observation window and a horizontal plane is 33 °.
The first electrode and the second electrode may be made of conductive metal such as gold, copper, aluminum, and alloy.
In the chip of the embodiment, the distance between the observation electrode and the counter electrode is fixed, and the performance is stable. And because there are a plurality of windows on observing the electrode, the window edge all is the observation point, and the observation point is more, seeks the sample more easily.
Meanwhile, the chip of the embodiment is simple to manufacture, only two electrodes are required to be directly manufactured, an observation window is reserved, a user does not need to manually overlap gold wires, the distance between the two electrodes can be accurately controlled, and the yield is improved.
When the chip works, the anode and the cathode are respectively placed at the observation window of the observation electrode and on the counter electrode, and the electrolyte is dripped between the two electrodes to observe, so that the operation is simple.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Claims (8)
1. The utility model provides a be applied to TEM and carry out normal position electrochemical reaction measuring chip, its characterized in that includes the basement and sets up in the first electrode and the second electrode of basement up end, first electrode has the opening, second electrode global distribution in the opening, just no direct contact between second electrode and the first electrode, a second electrode tip has more than one and runs through perpendicularly the observation window of second electrode, observation window has trapezoidal cross-section, and the contained angle of its inner wall and horizontal plane is 20 ~ 70.
2. The chip of claim 1, comprising an electrode layer formed on the substrate, the electrode layer comprising the first and second electrodes.
3. The chip of claim 2, wherein: and an insulating layer is also distributed between the electrode layer and the substrate.
4. The chip of claim 1, wherein: the second electrode has 1-500 observation windows.
5. The chip of claim 4, wherein: the second electrode has more than two observation windows.
6. The chip of claim 1, wherein: in the opening, the distance between the outer peripheral edge of the second electrode and the inner peripheral edge of the opening is 1 to 3000 μm.
7. The chip of claim 1, wherein: the substrate comprises a P-type, N-type or intrinsic silicon wafer.
8. The chip of claim 3, wherein: the material of the insulating layer comprises silicon oxide, silicon nitride or aluminum oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610130211.6A CN107170794B (en) | 2016-03-08 | 2016-03-08 | Chip applied to TEM for in-situ electrochemical reaction measurement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610130211.6A CN107170794B (en) | 2016-03-08 | 2016-03-08 | Chip applied to TEM for in-situ electrochemical reaction measurement |
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| Publication Number | Publication Date |
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| CN107170794A CN107170794A (en) | 2017-09-15 |
| CN107170794B true CN107170794B (en) | 2020-02-04 |
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| CN109682711B (en) * | 2019-01-24 | 2021-03-23 | 中国科学院上海微系统与信息技术研究所 | Chip for direct in-situ characterization of TEM structure-effect correlation and manufacturing method thereof |
| CN111948231A (en) * | 2020-07-22 | 2020-11-17 | 中国科学院物理研究所 | In situ monitoring of AlF3Method for discharge process as positive electrode of lithium primary battery |
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| JP4283880B2 (en) * | 2007-07-20 | 2009-06-24 | パナソニック株式会社 | Electrode measurement electrode plate, electrochemical measurement apparatus having the electrode plate, and method for quantifying a target substance using the electrode plate |
| WO2013156075A1 (en) * | 2012-04-20 | 2013-10-24 | Topsøe Fuel Cell A/S | Metallic element useful as spacer or interconnect for a high temperature fuel cell |
| CN104502428A (en) * | 2015-01-12 | 2015-04-08 | 清华大学 | Miniature electrochemical sensor based on direct forming mesoporous carbon technology and manufacturing method |
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