CN209416966U - Electrochemical in-situ reaction observation chip - Google Patents
Electrochemical in-situ reaction observation chip Download PDFInfo
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- CN209416966U CN209416966U CN201920090064.3U CN201920090064U CN209416966U CN 209416966 U CN209416966 U CN 209416966U CN 201920090064 U CN201920090064 U CN 201920090064U CN 209416966 U CN209416966 U CN 209416966U
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Abstract
The utility model discloses a kind of electrochemical in-situs to react observation chip and its application.Electrochemical in-situ reaction observation chip includes substrate and the first electrode and second electrode for being set to upper surface of substrate, first electrode has opening portion, the one end of at least described second electrode is set in the opening portion, and nothing directly contacts between the second electrode and first electrode, at least in the second electrode being set in first electrode opening portion there is more than one to run through the observation window of the second electrode, the observation window is also continuous through downwards the upper and lower surfaces of the substrate, and the film with micro through hole is covered on the observation window.The utility model covers the observation window of original hollow out using unique low stress nitride silicon thin film, and micron order and/or nanoscale through-hole array have been made on the silicon nitride film above observation window, this improvement is so that chip is provided with bigger advantage in actual use.
Description
Technical field
In particular to a kind of electrochemical in-situ reaction observation chip of the utility model, belongs to Electronic Speculum the field of test technology.
Background technique
With the development of material science, since a nearly century, scientific research personnel is microscopic appearance, the crystal knot of research material
The properties such as structure, chemical composition and Atomic coordinate have developed a variety of characterization techniques.Wherein, transmission electron microscope and synchronous spoke
The technology of penetrating is great representative two ways in a variety of characterization techniques.Transmission electron microscope (TEM) technology is because of its superelevation
Spatial resolution and temporal resolution and powerful built-in analysis means, such as classical electron diffraction technique, and especially look steadily
Mesh.Meanwhile Synchrotron Radiation Technology is also rapidly developing, domestic Synchrotron Radiation has been subjected to three generations's development, in structuring
The fields such as, surface physics and chemistry are widely applied.Original position (in situ) measuring technology developed in recent years, more
The application of transmission electron microscope and synchrotron radiation is further expanded.In-situ testing technique can be in a variety of characterization equipment
Respective physical/the chemical signal for causing object to be measured to generate by outside stimulus (power, heat, light, magnetic, electricity etc.) is captured in real time
Variation.
In-situ testing technique is extended to electrochemical field by scientific research personnel, especially after lithium battery testing field, skill in situ
Art more shows two big unique advantages.It on the one hand, can be real-time using in-situ test (as original position TEM, in-situ synchronization radiate)
The various nonequilibrium state and stable situation for capturing lithium battery chemical reaction process, are conducive to scientific research personnel and study its dynamics
Process, these are difficult to realize in ex situ technology；On the other hand, the electrode material in lithium battery and electrolyte are most
To in air oxygen and water it is more sensitive, ex situ observe when these materials are inevitably contacted with atmosphere, thus
The error of environmental factor is introduced, and in testing in situ, entire electrochemical process is carried out in the cavity of equipment, can be fine
Avoid external environment from causing experimental artifact.In electron microscopic study, refer to that done experiment and measurement are all in quilt in situ
It is carried out in the environment of where the object of measurement is original, also refers to that experimental observation is in real time, can dynamically to observe a biochemistry
Or the process of physical reactions.
A kind of chip carrying out electrochemical in-situ response measurement applied to TEM in the prior art, as shown in Figure 1, chip 1 wraps
It includes substrate and is set to the first electrode 21 and second electrode 22 of substrate upper surface, first electrode 21 has opening portion, described
There is second electrode one end more than one to run through the observation window 3 of the second electrode, at least one end of second electrode 22
Portion is set in the opening portion, and nothing directly contacts between the second electrode and first electrode；It can be directed to lithium-sulfur cell
Reaction mechanism studied.But due to the observation window of this chip structure be full through hollow out window, only
The observation material that patch processing is carried out having a size of grade and convenient for tweezers clamping can be chosen, its partial mulching is enterprising in window
Row observation；Meanwhile the material only vacantly above window can be carried out TEM observation, so that sample to be tested has very greatly in selection
Limitation.In addition, existing technology is only used in TEM, demand associated with a variety of characterization methods is unable to satisfy (such as in TEM
With it is dialectical to the original position of same target in synchrotron radiation X line station).In addition, the electrolyte being added dropwise in electrochemical reaction may also lead to
The trapezoidal side wall that penetrating window penetrates into window is crossed, is directly contacted with exposed silicon base, to the test knot of electrochemical reaction
Fruit impacts.
Utility model content
The main purpose of the utility model is to provide a kind of electrochemical in-situs to react observation chip, to overcome the prior art
Deficiency.
For the aforementioned purpose of utility model of realization, the technical solution adopted in the utility model includes:
The utility model embodiment provides a kind of electrochemical in-situ reaction observation chip, including substrate and is set to base
The first electrode and second electrode of bottom upper surface, the first electrode have opening portion, the one end of at least described second electrode
At least first electrode is being set to without directly contacting in the opening portion, and between the second electrode and first electrode
There is second electrode in opening portion more than one to run through the observation window of the second electrode, and the observation window also connects downwards
The continuous upper and lower surfaces through the substrate, and, the film with micro through hole is covered on the observation window.
Further, the material of the film include low stress SiNx, boron nitride, in graphene any one or two
Kind or more combination, but not limited to this.
Further, the film with a thickness of 1nm-5 μm.
Further, the second electrode has a plurality of observation windows, the film covered on any two observation window
Quantity, shape and the spread pattern of micro through hole can be identical or different.
Further, the film, which has, arranges the micro through hole array formed by a plurality of micro through holes.
Preferably, the shape of the micro through hole includes circle.
Preferably, the aperture of the micro through hole is 1nm-100 μm.
In some more specific embodiments, the electrochemical in-situ reaction observation chip includes being sequentially formed at
The upper the first film layer and electrode layer of the upper surface of substrate, the electrode layer include the first electrode and second electrode,
The film with micro through hole is formed by the first film layer for being located at observation window region.
In some more specific embodiments, the electrochemical in-situ reaction observation chip further include: be formed in
Second film layer of the substrate lower surface, the observation window run through second film layer.
Preferably, the material of the first film and the second film layer is identical.
Further, the substrate includes p-type, N-type or intrinsic silicon wafer, but not limited to this.
In some more specific embodiments, in the opening portion, the lateral edge portion of second electrode is opened with described
The distance between Inner peripheral portions of oral area are much larger than between the nose lip of second electrode and the Inner peripheral portions of the opening portion
Distance.
Preferably, the distance between Inner peripheral portions of the lateral edge portion of second electrode and the opening portion are more than or equal to 500 μ
m。
Preferably, the distance between the nose lip of second electrode and the Inner peripheral portions of the opening portion are 1 μm -100 μm.
In some more specific embodiments, the observation window extends vertically through the second electrode, and the sight
Surveying window has trapezoid cross section.
In some more specific embodiments, the second electrode overall distribution is in the opening portion.
The utility model embodiment additionally provides the electrochemical in-situ reaction observation chip and tests neck in Electronic Speculum in situ
The purposes in domain.
Preferably, the Electronic Speculum test includes in situ TEM test, in-situ synchronization radiation test.
Compared with prior art, a kind of electrochemical in-situ reaction observation chip provided by the embodiment of the utility model, structure
It is more reasonable, with better function, it can be applied not only to the TEM field of electrochemical test of lithium battery, to micron order and/or can also receive
The electrode material of meter level carries out electro-chemical test, can also on the film of observation window by way of vapor deposition evaporated film material
Material carries out electro-chemical test；And a kind of electrochemical in-situ reaction observation chip provided by the embodiment of the utility model can be with
In analysis for a variety of characterization methods such as synchrotron radiation X-ray, grenz ray, demand associated with TEM and synchrotron radiation is realized.
Detailed description of the invention
Fig. 1 be in the prior art it is a kind of applied to TEM carry out electrochemical in-situ response measurement chip structural schematic diagram；
Fig. 2 is a kind of planar structure schematic diagram of electrochemical in-situ reaction observation chip in the utility model embodiment 1；
Fig. 2 a is a kind of enlarged drawing of the partial structurtes of electrochemical in-situ reaction observation chip in Fig. 2；
Fig. 3 is single observation window on a kind of electrochemical in-situ reaction observation chip in one exemplary embodiments of the utility model
The structural schematic diagram of mouth；
Fig. 4 is that a kind of cross section structure of electrochemical in-situ reaction observation chip in one exemplary embodiments of the utility model shows
It is intended to；
Fig. 5 is a kind of structural schematic diagram of electrochemical in-situ reaction observation chip in the utility model embodiment 2.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose that this is practical new
The technical solution of type.The technical solution, its implementation process and principle etc. will be further explained as follows.
The utility model embodiment provides a kind of electrochemical in-situ reaction observation chip, including substrate and is set to base
The first electrode and second electrode of bottom upper surface, the first electrode have opening portion, the one end of at least described second electrode
At least first electrode is being set to without directly contacting in the opening portion, and between the second electrode and first electrode
There is second electrode in opening portion more than one to run through the observation window of the second electrode, and the observation window also connects downwards
The continuous upper and lower surfaces through the substrate, and, the film with micro through hole is covered on the observation window.
Further, the material of the film includes appointing in the thin-film materials such as low stress SiNx, boron nitride, graphene
Meaning a combination of one or more, but not limited to this.
Further, the film with a thickness of 1nm-5 μm.
Further, the second electrode has a plurality of observation windows；The shape of observation window can be rectangular, round
Deng quantity, shape and the spread pattern of the micro through hole of the film covered on any two observation window can be identical or different.
Further, the film, which has, arranges the micro through hole array formed by a plurality of micro through holes, such as can be 6*6
Array of circular holes.
Preferably, the shape of the micro through hole includes circle, but not limited to this.
Preferably, the aperture of the micro through hole is 1nm-100 μm, such as can be 2 μm.
In some more specific embodiments, the electrochemical in-situ reaction observation chip includes being sequentially formed at
The upper the first film layer and electrode layer of the upper surface of substrate, the electrode layer include the first electrode and second electrode,
The film with micro through hole is formed by the first film layer for being located at observation window region.
Preferably, the material of the first electrode and second electrode includes conductive metal and conductive non-metals, conductive metal
Alloy including the formation of one or more of gold, silver, copper, platinum, chromium, molybdenum etc. metal, but not limited to this；Conductive non-metals
Including conductivity ceramics etc., but not limited to this.
In some more specific embodiments, the electrochemical in-situ reaction observation chip further include: be formed in
Second film layer of the substrate lower surface, the observation window run through second film layer.
Preferably, the material of the first film and the second film layer is identical.
Further, the substrate includes p-type, N-type or intrinsic silicon wafer, but not limited to this.
In some more specific embodiments, in the opening portion, the lateral edge portion of second electrode is opened with described
The distance between Inner peripheral portions of oral area are much larger than between the nose lip of second electrode and the Inner peripheral portions of the opening portion
Distance.
Preferably, the distance between Inner peripheral portions of the lateral edge portion of second electrode and the opening portion are more than or equal to 500 μ
m。
Preferably, the distance between the nose lip of second electrode and the Inner peripheral portions of the opening portion are 1 μm -100 μm.
In some more specific embodiments, the observation window extends vertically through the second electrode, and the sight
Surveying window has trapezoid cross section.
In some more specific embodiments, the second electrode overall distribution is in the opening portion.
The utility model embodiment additionally provides the electrochemical in-situ reaction observation chip and tests neck in Electronic Speculum in situ
The purposes in domain.
Preferably, the Electronic Speculum test includes in situ TEM test, in-situ synchronization radiation test.
The technical solution, its implementation process and principle etc. are further explained below in conjunction with the accompanying drawings and embodiments
It is bright.
Embodiment 1
Please refer to Fig. 2, Fig. 3 and Fig. 4, a kind of electrochemical in-situ reaction observation chip, including substrate 10, be formed in substrate
The first film layer 20 on surface, the second film layer 30 for being formed in substrate lower surface, the electricity for being formed in the first film layer upper surface
Pole layer 40, electrode layer 40 include first electrode 410 and second electrode 420, and first electrode 410 has opening portion, second electrode 420
It is integrally dispersed in the opening portion, and nothing directly contacts between second electrode 420 and first electrode 410, and in second electrode
420 one end has nine observation windows 50 for running through the second electrode 420, and observation window is also continuous through downwards substrate
10 and second film layer 30, the corresponding the first film layer 20 of observation window 50 forms the film 60 of covering observation window, in film
A plurality of micro through holes 610 are provided on 60, a plurality of micro through holes 610 are according to setting form (such as square array form of 6*6)
Arrangement forms micro through hole array, (quantity, spread pattern, the shape of the micro through hole on each film can be identical or different)；?
In the opening portion, the distance between Inner peripheral portions of the lateral edge portion of second electrode 420 and opening portion d1 is much larger than the second electricity
The distance between the Inner peripheral portions of the nose lip of pole and opening portion d2, wherein d1 >=500 μm；Specifically, the material of film
Matter includes low stress SiNx, boron nitride, any one or two or more combinations in graphene, but not limited to this；Film
With a thickness of 1nm-5 μm, the penetration of electrons rate of film is 97% or more.
More specifically, please refer to Fig. 2 and Fig. 2 a, second electrode 420 can from a short side of chip extend
To the middle position of chip, and the observation window 50 of nine rectangles is distributed in the second electrode region in middle position, observation
Electrode is not covered on window 50, first electrode 410 surrounds second electrode 420 simultaneously from two longitudinal directions of chip and middle position
Keep apart with second electrode, it can be understood as, defining second electrode 420 to enter the direction of opening portion is incision direction, positioned at cutting
The one end for entering the extending direction in direction is the front end of second electrode, is the side of second electrode positioned at incision direction two sides,
Then, the outer peripheral edge of the front end of second electrode 420 (is directed to this implementation for d1 at a distance from the inner peripheral of first electrode opening portion
Example, it is understood that the outer peripheral edge for being first electrode opening portion inner peripheral and second electrode along the distance of short side direction is d1), the
The outer peripheral edge of the side of two electrodes 420 (is directed to the present embodiment, can also manage at a distance from the inner peripheral of first electrode opening portion for d2
Solution is that distance of the outer peripheral edge of first electrode opening portion inner peripheral and second electrode in the longitudinal direction of chip is d2), d2's
Size can be adjusted according to experiment condition, but d1 is much larger than d2.
Preferably, the material of the first film layer, thickness can be identical with the material of film.
Preferably, the material of the first film layer and the second film layer is identical, and thickness is identical.
More preferably, the first film layer and the second film layer are wholely set.
Preferably, the material of first electrode and second electrode includes conductive metal and conductive non-metals, and conductive metal includes
The alloy that one or more of gold, silver, copper, platinum, chromium, molybdenum etc. metal is formed, but not limited to this；Conductive non-metals include
Conductivity ceramics etc., but not limited to this.
Preferably, the substrate includes p-type, N-type or intrinsic silicon wafer, but not limited to this.
Preferably, observation window extends vertically through the second electrode 420, and observation window has trapezoid cross section, inner wall
Angle with horizontal plane is 20-90 °
Embodiment 2
Referring to Fig. 5, a kind of electrochemical in-situ reaction observation chip, structure and the electrochemical in-situ in embodiment 1 are anti-
The structure that chip should be observed is almost the same, the difference is that, only the opening portion of first electrode is arranged in one end to second electrode
It is interior.
It should be noted that the other structures about electrochemical in-situ reaction observation chip a kind of in the utility model are special
Sign etc., which is seen, carries out spy disclosed in the chip of electrochemical in-situ response measurement applied to TEM as CN107170794A is a kind of
The concrete shape and form of sign and first electrode and second electrode can also be there are many forms, and details are not described herein.
A kind of electrochemical in-situ reaction observation chip provided by the embodiment of the utility model uses unique low stress
Silicon nitride film covers the observation window of original hollow out, and has made micron order on the silicon nitride film above observation window
And/or nanoscale through-hole array, this improvement is so that chip is provided with bigger advantage, specific manifestation in actual use
Are as follows:
1) observation window covers low stress nitride silicon thin film, the silicon nitride film to the electronics in electron microscope almost
It is transparent (penetration of electrons rate >=97%), sample to be tested can be placed on the silicon nitride film of observation window and be observed,
So that observable sample is increased, linear one-dimensional material and micron-sized dusty material can not only be seen
It surveys, some special evaporation materials can also be observed by the method in area of observation coverage evaporation material；
2) observation window material can be further reduced by micro-via structures being prepared on the silicon nitride film of observation window mouth region
The accurate analysis of the high-resolution imaging and electronic diffraction of sample is realized in influence to observed result；
3) thickness of silicon nitride film and hole size, period and shape on film can be required according to observation and
The viscosity of electrolyte is modified and additions and deletions, not only can be used as the scale and reference point of observation, more can effectively prevent
Only contact of the electrolyte with base silicon；
4) electrochemical in-situ reaction observation chip provided by the embodiment of the utility model can be applied not only to TEM and carry out original
The observation of position electrochemical reaction, simultaneously because silicon nitride film can realize the maximum transmission rate of grenz ray, therefore, this money chip
It can be also used in other reflection, transmission imaging and the analyses such as synchrotron radiation.
It should be appreciated that above-described embodiment is only to illustrate the technical ideas and features of the present invention, it is ripe its object is to allow
The personage for knowing technique can understand the content of the utility model and implement accordingly, can not limit the utility model with this
Protection scope.All equivalent change or modifications according to made by the spirit of the present invention essence, should all cover in the utility model
Within protection scope.
Claims (16)
1. a kind of electrochemical in-situ reaction observation chip, including substrate and it is set to the first electrode and second of upper surface of substrate
Electrode, the first electrode have opening portion, and the one end of at least described second electrode is set in the opening portion, and described the
Nothing directly contacts between two electrodes and first electrode, it is characterised in that: at least in second be set in first electrode opening portion
There is electrode more than one to run through the observation window of the second electrode, and the observation window is also continuous through downwards the substrate
Upper and lower surfaces, and, the film with micro through hole is covered on the observation window.
2. electrochemical in-situ according to claim 1 reaction observation chip, it is characterised in that: the material of the film includes
Low stress SiNx, boron nitride, any one or two or more combinations in graphene.
3. electrochemical in-situ reaction observation chip according to claim 1 or 2, it is characterised in that: the thickness of the film
It is 1nm-5 μm.
4. electrochemical in-situ reaction observation chip according to claim 1, it is characterised in that: the second electrode has multiple
Several observation windows.
5. electrochemical in-situ reaction observation chip according to claim 1, it is characterised in that: the film has by plural number
A micro through hole arranges the micro through hole array to be formed.
6. electrochemical in-situ reaction observation chip according to claim 5, it is characterised in that: the shape packet of the micro through hole
Include circle.
7. electrochemical in-situ reaction observation chip according to claim 5 or 6, it is characterised in that: the hole of the micro through hole
Diameter is 1nm-100 μm.
8. electrochemical in-situ reaction observation chip according to claim 1, it is characterised in that described including being sequentially formed at
The upper the first film layer and electrode layer of upper surface of substrate, the electrode layer include the first electrode and second electrode, described
Film with micro through hole is formed by the first film layer for being located at observation window region.
9. electrochemical in-situ reaction observation chip according to claim 8, it is characterised in that further include: it is formed in the base
Second film layer of bottom surface, the observation window run through second film layer.
10. electrochemical in-situ according to claim 9 reaction observation chip, it is characterised in that: the first film and the
The material of two film layers is identical.
11. electrochemical in-situ reaction observation chip according to claim 1, it is characterised in that: the substrate includes p-type, N
Type or intrinsic silicon wafer.
12. electrochemical in-situ reaction observation chip according to claim 1, it is characterised in that: in the opening portion, the
Nose lip of the distance between the Inner peripheral portions of the lateral edge portion of two electrodes and the opening portion much larger than second electrode and institute
State the distance between the Inner peripheral portions of opening portion.
13. electrochemical in-situ reaction observation chip according to claim 12, it is characterised in that: the side edge of second electrode
The distance between the Inner peripheral portions in portion and the opening portion are more than or equal to 500 μm.
14. electrochemical in-situ reaction observation chip according to claim 13, it is characterised in that: the front-end edge of second electrode
The distance between the Inner peripheral portions in portion and the opening portion are 1 μm -100 μm.
15. electrochemical in-situ reaction observation chip according to claim 1, it is characterised in that: the observation window is vertical
Through the second electrode, and the observation window has trapezoid cross section.
16. electrochemical in-situ reaction observation chip according to claim 1, it is characterised in that: the second electrode is whole
It is distributed in the opening portion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920090064.3U CN209416966U (en) | 2019-01-18 | 2019-01-18 | Electrochemical in-situ reaction observation chip |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920090064.3U CN209416966U (en) | 2019-01-18 | 2019-01-18 | Electrochemical in-situ reaction observation chip |
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| CN209416966U true CN209416966U (en) | 2019-09-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111627981A (en) * | 2020-05-08 | 2020-09-04 | 北京大学 | In-situ TEM electrical chip easy to expand and process and manufacturing method thereof |
| CN114993232A (en) * | 2022-07-18 | 2022-09-02 | 苏州宇量电池有限公司 | Method for detecting morphology of electrode material |
-
2019
- 2019-01-18 CN CN201920090064.3U patent/CN209416966U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111627981A (en) * | 2020-05-08 | 2020-09-04 | 北京大学 | In-situ TEM electrical chip easy to expand and process and manufacturing method thereof |
| CN114993232A (en) * | 2022-07-18 | 2022-09-02 | 苏州宇量电池有限公司 | Method for detecting morphology of electrode material |
| CN114993232B (en) * | 2022-07-18 | 2022-10-18 | 苏州宇量电池有限公司 | Method for detecting morphology of electrode material |
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Address after: No. 398 Ruoshui Road, Suzhou Industrial Park, Jiangsu Province Patentee after: Suzhou Mengwei Chip Technology Co., Ltd Address before: Chongchuan District 226000 Century Avenue in Jiangsu province Nantong City 369 Building No. 8 Room 803, room 804 Patentee before: NANTONG MENGWEI CHIP TECHNOLOGY Co.,Ltd. |