CN106290411B - The self-aligning device of solid-liquid phase interfacial chemical reaction in situ - Google Patents
The self-aligning device of solid-liquid phase interfacial chemical reaction in situ Download PDFInfo
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- CN106290411B CN106290411B CN201510313568.3A CN201510313568A CN106290411B CN 106290411 B CN106290411 B CN 106290411B CN 201510313568 A CN201510313568 A CN 201510313568A CN 106290411 B CN106290411 B CN 106290411B
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Abstract
The invention discloses a kind of self-aligning device of solid-liquid phase interfacial chemical reaction in situ, the upper chip (100) and lower chip (200) combined including the corresponding sealing in wall (300), the first insulating film (510), the second insulating film (520) and two sides；Upper chip (100) has the boss (110) towards lower chip (200) protrusion, and lower chip (200) has the groove (210) recessed towards upper chip (100)；Wall (300) is located between first insulating film (510) on boss (110) surface and second insulating film (520) of groove (210) inner wall.The self-aligning device can be applied to conventional TEM sample platform, eliminates the demand of customized sample bar, significantly reduces testing cost；Meanwhile the prepare liquid scale of construction is less, can prevent the first insulating film (510) and/or the second insulating film (520) from rupturing the damage to other component.
Description
Technical field
The invention belongs to transmissioning electric mirror test device arts, in particular, being related to a kind of solid-liquid phase interface in situ
Learn the self-aligning device of reaction.
Background technique
The research of solid-liquid interface is always domestic surgery because of its importance in biology, chemistry and interface science
The hot spot of educational circles's research.Recently as the rise of nanometer material science, more and more results of study show the nanometer of material
Structure has critical influence to its property.Transmission electron microscope (TEM) is used as strong material structure characterization tool,
It can analyze to obtain the information such as material atom grade high resolution picture, electron diffraction diagram, chemical element power spectrum, but common commercialization
TEM cannot be passed through sample, can only carry out the structural research of solid-solid phase or solid-gas phase interface, can not to solid-liquid phase interface into
Row characterization test.
Current TEM solid-liquid phase test method is then to utilize O-shaped rubber using special TEM sample bar and support chip
Chip and special TEM sample bar are closely joined together by circle or epoxy resin, and by special TEM sample bar by testing liquid
Sample is passed through in chip, to realize TEM solid-liquid phase in-situ test in the chips.But existing solid-liquid phase test is special at present
Specimen holder mainly has following two major defect: (1) user need to buy special TEM sample bar, and price is at least in 200,000 people
More than coin, cost is very high；(2) it is injected into special TEM sample bar in real time due to testing liquid by syringe pump, liquid in specimen holder
The scale of construction is more, once the silicon nitride film of chip surface ruptures, the electronics that a large amount of testing liquid is likely to damage TEM occurs
Rifle and corrosion objective pole shoe, it is larger to the threat that instrument is constituted in use.
Summary of the invention
To solve the above-mentioned problems of the prior art, the present invention provides a kind of solid-liquid phase interfacial electrochemistry in situ is anti-
The self-aligning device answered, the self-aligning device can be applied to the sample stage of conventional TEM, without using customized sample bar, thus greatly
Amplitude reduction cost.
In order to achieve the above object of the invention, present invention employs the following technical solutions:
A kind of self-aligning device of original position solid-liquid phase interfacial chemical reaction, comprising: wall, the first insulating film, second are absolutely
The upper chip and lower chip that the corresponding sealing of velum and two sides combines；The upper chip has towards the convex of the lower chip protrusion
Platform has first through hole in the boss, and surface that first insulating film covers the boss and the first through hole are in institute
State the opening on the surface of boss；The lower chip has the groove recessed towards the lower chip, has in the lower chip
Second through-hole, second insulating film cover the groove inner wall and the second through-hole opening on the inner wall of the groove
Mouthful；The boss is set in the groove, and the first through hole is relative to second through-hole, the wall sandwiched
Between first insulating film and second insulating film.
Further, the size of the first through hole is gradually increased along the direction far from second through-hole.
Further, the size of second through-hole is gradually increased along the direction far from the first through hole.
Further, the self-aligning device further include: third insulating film and the 4th insulating film；The third insulating film covers
The outer surface of the upper chip is covered, the 4th insulating film covers the outer surface of the lower chip.
Further, first insulating film and/or second insulating film and/or the third insulating film and/or institute
The 4th insulating film is stated to be formed by silicon nitride.
Further, the upper chip and the two sides of the lower chip respectively by adhesive seal bond together with.
Further, the adhesive is the adhesive formed by epoxy resin.
Further, the thickness of the wall is not less than 100nm.
Further, any one of the material of the wall in gold, platinum, chromium, silica.
Further, second insulating film cover the lower chip on the surface of the groove two sides, wherein
The thickness for being covered on the second insulating film on the surface of the groove two sides of the lower chip is described recessed greater than being covered on
The thickness of the second insulating film on slot inner wall.
The present invention is by the preparation upper chip and lower chip that mutually agree with, and respectively in the boss of upper chip and lower chip
Wall is prepared between groove, sample to be tested can be sealed in the enclosure space formed by upper chip, lower chip and wall.
The self-aligning device can be applied to the sample stage of conventional TEM, to eliminate the demand of customized sample bar, considerably reduce into
This (ten thousand yuan of Cong Ershi or more are down to several hundred members)；At the same time, the prepare liquid scale of construction stored in above-mentioned enclosure space is less
(0.1 μ L or so) can effectively prevent the first insulating film and/or the second insulating film to rupture and make to the electron gun and objective pole shoe of TEM
At damage；Therefore cost is being greatly lowered in the self-aligning device of solid-liquid phase interfacial electrochemistry reaction in situ according to the present invention
While, and can avoid the damage to instrument other component.
Detailed description of the invention
What is carried out in conjunction with the accompanying drawings is described below, above and other aspect, features and advantages of the embodiment of the present invention
It will become clearer, in attached drawing:
Fig. 1 is the sectional view of the self-aligning device of the solid-liquid phase interfacial chemical reaction in situ of embodiment according to the present invention.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to detailed description of the present invention embodiment.However, it is possible to come in many different forms real
The present invention is applied, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, providing these implementations
Example is in order to explain the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.In the accompanying drawings, for the sake of clarity, element can be exaggerated
Shape and size, and identical label will be used to indicate the same or similar element always.
Term " first ", " second " etc. herein can be used to describe various elements although will be appreciated that, these
Element should not be limited by these terms, and these terms are only used to distinguish an element with another element.
Fig. 1 is the section of the self-aligning device of the solid-liquid phase interfacial electrochemistry in situ reaction of embodiment according to the present invention
Figure.
Referring to Fig.1, the self-aligning device of the solid-liquid phase interfacial electrochemistry in situ reaction of embodiment according to the present invention includes
Upper chip 100, lower chip 200, wall 300, adhesive 400, the first insulating film 510, the second insulating film 520, third insulation
Film 530 and the 4th insulating film 540；Wherein, upper chip 100 and lower chip 200 are oppositely arranged and mutually agree with, upper chip 100
It is combined with the two sides of lower chip 200 by the corresponding sealing of adhesive 400, wall 300 is folded in the first insulating film 510 and second
Between insulating film 520.
In the present embodiment, the sectional dimension of upper chip 100 and lower chip 200 is 5mm × 5mm, with a thickness of 200 μm, material
Material is Si piece, and the material of adhesive 400 is epoxy resin.The thickness of upper chip 100 and lower chip 200 does not make particular requirement, root
It is determined according to the thickness of specifically selected Si piece；The distance between upper chip 100 and lower chip 200 are generally according to the interval between it
The thickness of layer 300 determines that in the present embodiment, the material of wall 300 is crome metal, with a thickness of 100nm or so.But this
Invention is not restricted to this, and the thickness of general wall 300 can meet requirement of the invention not less than 100nm, meanwhile, interval
The material of layer 300 can also be metal platinum, gold or silica etc..
In this way, form closed cavity by upper chip 100, lower chip 200 and wall 300, the closed cavity can into
It is used as when row in situ measurement solid-liquid phase interfacial electrochemistry reacts and holds testing liquid 610.
Specifically, upper chip 100 includes the boss 110 convexed to form towards lower chip 200, and is arranged in boss 110
In first through hole 120；First through hole 120 in the present embodiment is through to the table of boss 110 by the top surface of upper chip 100
Face, and the size of the first through hole 120 is gradually increased with far from the direction of lower chip 200；That is, in upper chip 100
First through hole 120 be a tetragonous groove, and its section be an inverted trapezoidal.Chip 100 in 110 reason of boss in the present embodiment
Downward 200 direction of chip of inner surface under convex into, therefore the boss 110 its actually inverted boss.
In the present embodiment, first through hole 120 covers in the opening on 110 surface of boss and the surface of the boss 110
There is the first insulating film 510, that is to say, that be covered on first through hole 120 towards the first insulating film in the opening of lower chip 200
510 extend to two sides and the surface of boss 110 are completely covered.In this way, first through hole 120 and being covered on the first of its opening
Insulating film 510 is to form a window for observation when measuring in situ.
In the present embodiment, the top surface of upper chip 100 is covered with third insulating film 530；But the present invention is not restricted to
This, can cover third insulating film 530 on other outer surfaces of upper chip 100.
Lower chip 200 includes towards the groove 210 of the recessed formation of upper chip 200 to match with boss 110, and setting
Second through-hole 220 opposite with the first through hole 120 in 210 bottom end of groove.It is similar with the structure of first through hole 120
It is that the second through-hole 220 in the present embodiment is through to the bottom end of groove 210, and second through-hole by the bottom surface of lower chip 200
220 size is gradually increased with the direction far from first through hole 120；That is, the second through-hole 220 in lower chip 200
It is inverted tetragonous groove for one, and its section is one trapezoidal.
In the present embodiment, the opening of the inner wall of groove 210 and the second through-hole 220 on 210 inner wall of groove is covered with
Two insulating films 520, meanwhile, lower chip 200 is again covered with the second insulating film 520 on the surface of 210 two sides of groove, and under
The thickness of the second insulating film 520 on the surface of 210 two sides of groove of chip 200 will be thicker than on 210 inner wall of groove
The thickness of two insulating films 520；That is, being covered on the second insulation of the opening that the second through-hole 220 is located on 210 inner wall of groove
Film 520 extends to two sides, always all covers on the surface positioned at 210 two sides of groove of lower chip 200.
In the present embodiment, the bottom surface of lower chip 200 is covered with the 4th insulating film 540；Certainly, lower chip 200 other
The 4th insulating film 540 can also be covered on outer surface.
In this way, solid 620 to be measured is that can be placed on the second insulating film 520 of covering the second through-hole 220 opening, work as simultaneously
Upper chip 100 and lower chip 200 encapsulation after the completion of, solid 620 to be measured can be immersed in testing liquid 610 and therewith occur consolidate-
Reaction between liquid phase, and the reaction can carry out home position observation by the window in upper chip 100.
In the present embodiment, the boss 110 in upper chip 100 is in tetragonous boss-shaped, corresponding, lower chip 200
In groove 210 be in tetragonous groove-like, in this way, the boss 110 of 100 bottom end of upper chip can agree with the groove in lower chip 200
In 210；Certainly, the shape of above-mentioned first through hole 120, the second through-hole 220, boss 110 and groove 210 is not to immobilize
, other shapes with identity function as boss 110 and groove 210 can also be other irregular shapes, but are wanted
Ask the shape between boss 110 and groove 210 to match so that wall 300 can sandwiched therebetween, thus formed storage it is to be measured
The closed cavity of liquid 610.
Preferably, above-mentioned first insulating film 510, the second insulating film 520, third insulating film 530 and the 4th insulating film 540
Material be low stress SiNx, the stress of the low stress nitride silicon fiml is about 800MPa.In the present embodiment, it is located at upper core
The first insulating film 510 and third insulating film 530 of piece 100, positioned at lower chip 200 the 4th insulating film 540 and be located at groove
The thickness of second insulating film 520 of 210 inner walls is 100nm, and covers the surface positioned at 210 two sides of groove of lower chip 200
On the second insulating film 520 there are secondary depositions in preparation process, therefore it is substantially two layers of silicon carbide film, with a thickness of
200nm；Certainly, the present invention is not restricted to this, as the first insulating film 510, the second insulating film 520,530 and of third insulating film
The Stress Control of the low stress nitride silicon fiml of 4th insulating film, 540 material is covered on core in 800MPa~1000MPa
It first insulating film 510 of piece 100, third insulating film 530 and is covered on the 4th insulating film 540 of lower chip 200 and is covered on
The thickness of the second insulating film 520 on 210 inner wall of groove controls in the range of 100nm~400nm, and is covered on down
The thickness of the second insulating film 520 on the surface of 210 two sides of groove of chip 200 then controls the model in 200nm~800nm
In enclosing.
In the present embodiment, adhesive 400 is circumferentially positioned at the top surface of chip 100 and the top surface of lower chip 200
Between, and the two sides of upper chip 100 and lower chip 200 correspondence is glued together.
Further, adhesive 400 is the adhesive formed by epoxy resin.Certainly, other can be realized upper chip 100
The adhesive that sealing corresponding with the two sides of lower chip 200 combines, the technology are those skilled in the art's customary means, herein
No longer repeat one by one.
The following institute of preparation process for the self-aligning device that the above-mentioned solid-liquid phase interfacial electrochemistry in situ suitable for TEM reacts
It states.
It is the preparation of upper chip 100 first, specifically uses following methods.
(1) a piece of Si piece with a thickness of 200 μm is selected as the raw material for preparing upper chip 100, using chemical vapor deposition
Silicon nitride film of the method in the opposite two sides growth 100nm thickness of Si piece (stress of the silicon nitride film is about 800MPa).
(2) region that 50 μ m, 400 μm of sizes are chosen at the middle part of wherein side silicon nitride film is logical as preparation first
The initial position in hole 120 (is denoted as 1#Corrosion region), and 50 μ ms are chosen at the both ends of other side silicon nitride film on the other side
The region of 400 μm of sizes (is denoted as 2 as the initial position for preparing boss 110#Corrosion region).
(3) 1 selected using semiconductor potassium hydroxide wet corrosion technique by two sides in Si piece#Corrosion region and 2#Corrosion region
Start to be corroded, until by 1#Corrosion region starts the silicon nitride film that the other side is exposed in corrosion, forms first through hole 120, together
When, in the other side by 2#Corrosion region starts corrosion and forms boss 110, in this way, the remaining nitrogen being still covered on Si piece surface
SiClx film i.e. the first insulating film 510 and third insulating film 530.
It is worth noting that the first through hole 120 of formation is a tetragonous groove during above-mentioned corrosion Si piece, and
The boss 110 of formation is a tetragonous boss；That is, the cross sectional shape of the first through hole 120 and boss 110 be it is trapezoidal,
The first through hole 120 forms two openings of different sizes on the top surface of upper chip 100 and the surface of boss 110；
Wherein, it is covered on 120 smaller opening of first through hole (being located at the opening on 110 surface of boss) and prolongs to the opening two sides
Silicon nitride film i.e. the first insulating film 510 on the surface for the boss 110 stretched, and be covered on this on another surface of chip 100
Silicon nitride film, that is, third insulating film 530.And it is subsequent by upper chip 100 with lower 200 assembly of chip during, by first
Insulating film 510 is towards the direction of lower chip 200, that is to say, that its essence is the tables for being covered on boss 110 for the first insulating film 510
The opening of face and first through hole 120 on 110 surface of boss, and third insulating film 530 is then covered on the top table of chip 100 on this
Face.
(4) metal of 100nm thickness is deposited on the first insulating film 510 on 110 surface of boss using means of electron beam deposition
Chromium forms wall 300, which does not stop the opening of first through hole 120, in this way, wall 300 be covered on it is convex
On 110 surface of platform and the first insulating film 510 of the opening of first through hole 120 forms an accommodation groove, after which can be used for
Testing liquid 610 is held before continuous encapsulation self-aligning device.
Followed by the preparation of lower chip 200, specifically use following methods.
(5) another is selected with a thickness of 200 μm of Si piece as the raw material for preparing lower chip 200, using chemical vapor deposition
Area method is in the silicon nitride film that its opposite two sides growth thickness is 100nm.
(6) corroded using semiconductor potassium hydroxide wet corrosion technique in the wherein side of Si piece, until opening
Mouth size is groove 210 of the tetragonous groove of 2mm × 2mm as lower chip 200, wherein corrosion depth control is 100 μm, i.e.,
The depth of the groove 210 is 100 μm.
(7) 210 two sides of groove are located in the inner wall of the groove 210 and lower chip 200 again using chemical vapour deposition technique
Surface on silicon nitride film on growth thickness be 100nm silicon nitride film, so lower chip 200 be located at groove
The second insulating film 520 is formd on the surface of 210 two sides and on the inner wall of groove 210；Wherein, because being located at for lower chip 200 is recessed
The deposition of silicon nitride film twice is carried out on the surface of 210 two sides of slot, therefore its thickness is than the second insulation on 210 inner wall of groove
The thickness of film 520 is thicker, is 200nm.
(8) the Si on piece using semiconductor potassium hydroxide wet corrosion technique in the side opposite with the groove 210 is rotten
Erosion forms the second through-hole 220, second through-hole 220 and first through hole until exposing the second insulating film 520 of 210 bottom end of groove
120 are oppositely arranged；And still it is covered on silicon nitride film i.e. the 4th insulating film 540 of lower 200 bottom surface of chip.
It is worth noting that corrosion makes first through hole 120 and boss 110, in lower chip 200 on upper chip 100
During upper corrosion makes the second through-hole 220 and groove 210, by calculating first through hole 120 and the second through-hole in advance
The size of the corrosion opening of the size and boss 110 and groove 210 in 220 initial corrosion region, further according to upper 100 He of chip
Si piece thickness used in lower chip 200 can be automatically performed corrosion, formed the first through hole 120 of predefined size, the second through-hole 220,
Boss 110 and groove 210；That is, the size difference of first through hole 120, the second through-hole 220, boss 110 and groove 210
It is related to initial corrosion area size and corrosion opening size；At the same time, what is be made of silicon nitride film is covered on first
Thickness, the stress etc. of the first insulating film 510 and the second insulating film 520 for being covered on the second through-hole 220 opening that through-hole 120 is open
Factor also has an impact to the design of first through hole 120 and the second through-hole 220.
Finally solid 620 to be measured is adhered on the second insulating film 520 of 210 bottom end of groove, and guarantees solid 620 to be measured
At the second through-hole of face 220, that is to say, that be adhered to opening of the second through-hole 220 of covering on 210 inner wall of groove second is exhausted
On velum 520；Testing liquid 610 is placed in the accommodation groove formed by the first insulating film 510 and wall 300, and uses ring
Oxygen resin bonds the opposite two sides of upper chip 100 and lower chip 200 as adhesive, adhesive 400 is formed, in this way, will
Solid 620 to be measured is packaged in the closed cavity formed by upper chip 100, lower chip 200 and wall 300 with testing liquid 610
Interior, the TEM in situ that the reaction of solid-liquid phase interfacial electrochemistry can be then carried out by conventional TEM is measured.
The sectional dimension of the above-mentioned upper chip 100 being prepared and lower chip 200 is 5mm × 5mm.
The solid-liquid phase interfacial electrochemistry in situ reaction that can be applied to conventional TEM being prepared using above-mentioned preparation method
Self-aligning device, when carrying out original position TEM measurement, without using the customized sample bar of valuableness, testing cost is greatly reduced；Together
When, it is packaged in 610 dosage of testing liquid in the closed cavity formed by upper chip 100, lower chip 200 and wall 300 very
Few (about 0.1 μ L or so), even if the first insulating film 510 and/or 520 break accident of the second insulating film occurs, excessive is few
Testing liquid 610 can also be taken away by vacuum system rapidly, thus prevent testing liquid 610 damage TEM equipment on electron gun
And objective pole shoe.
Although the present invention has shown and described referring to specific embodiment, it should be appreciated by those skilled in the art that:
In the case where not departing from the spirit and scope of the present invention being defined by the claims and their equivalents, can carry out herein form and
Various change in details.
Claims (10)
1. a kind of self-aligning device of original position solid-liquid phase interfacial chemical reaction characterized by comprising wall (300), the
The upper chip (100) and lower chip (200) that the corresponding sealing in one insulating film (510), the second insulating film (520) and two sides combines；
The upper chip (100) has the boss (110) towards lower chip (200) protrusion, has in the boss (110)
First through hole (120), first insulating film (510) covers the surface of the boss (110) and the first through hole (120) exists
Opening on the surface of the boss (110)；
The lower chip (200) has the groove (210) recessed towards the upper chip (100), tool in the lower chip (200)
Have the second through-hole (220), second insulating film (520) covers the inner wall and second through-hole (220) of the groove (210)
Opening on the inner wall of the groove (210)；
The boss (110) is set in the groove (210), and the first through hole (120) is logical relative to described second
Hole (220), the wall (300) are folded between first insulating film (510) and second insulating film (520)；
Wherein, closed cavity, the closing are formed by the upper chip (100), lower chip (200) and the wall (300)
Cavity is used to hold testing liquid when carrying out the reaction of in situ measurement solid-liquid phase interfacial electrochemistry；Cover second through-hole
(220) for placing solid to be measured on second insulating film (520) being open.
2. self-aligning device according to claim 1, which is characterized in that the size of the first through hole (120) is along remote
Direction from second through-hole (220) is gradually increased.
3. self-aligning device according to claim 1 or 2, which is characterized in that the size of second through-hole (220) along
Direction far from the first through hole (120) is gradually increased.
4. self-aligning device according to claim 1, which is characterized in that the self-aligning device further include: third insulation
Film (530) and the 4th insulating film (540)；
The third insulating film (530) covers the outer surface of the upper chip (100), and the 4th insulating film (540) covers institute
State the outer surface of lower chip (200).
5. self-aligning device according to claim 4, which is characterized in that first insulating film (510) and/or described
Two insulating films (520) and/or the third insulating film (530) and/or the 4th insulating film (540) are formed by silicon nitride.
6. self-aligning device according to claim 4, which is characterized in that the upper chip (100) and the lower chip
(200) two sides respectively by adhesive (400) seal bond together.
7. self-aligning device according to claim 6, which is characterized in that the adhesive (400) is by epoxy resin shape
At adhesive.
8. self-aligning device according to claim 1, which is characterized in that the thickness of the wall (300) is not less than
100nm。
9. self-aligning device according to claim 8, which is characterized in that the material of the wall (300) be selected from gold,
Platinum, chromium, any one in silica.
10. self-aligning device according to claim 1, which is characterized in that under the second insulating film (520) covering is described
Chip (200) on the surface of the groove (210) two sides, wherein it is described to be covered on being located at for the lower chip (200)
The thickness of the second insulating film (520) on the surface of groove (210) two sides is greater than the be covered on the groove (210) inner wall
The thickness of two insulating films (520).
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| CN107525816A (en) * | 2017-09-30 | 2017-12-29 | 南通盟维芯片科技有限公司 | TEM liquid testings chip and its preparation method with ultra-thin silicon nitride watch window |
| JP6881206B2 (en) * | 2017-10-05 | 2021-06-02 | トヨタ自動車株式会社 | Electrochemical measurement cell |
| CN111829822B (en) * | 2019-04-18 | 2023-10-20 | 中国科学院微电子研究所 | Liquid chip sampling device of electron microscope |
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