CN106324000B - Liquid-packing chip - Google Patents
Liquid-packing chip Download PDFInfo
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- CN106324000B CN106324000B CN201610677166.6A CN201610677166A CN106324000B CN 106324000 B CN106324000 B CN 106324000B CN 201610677166 A CN201610677166 A CN 201610677166A CN 106324000 B CN106324000 B CN 106324000B
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- chip
- case chip
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/03—Investigating materials by wave or particle radiation by transmission
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
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Abstract
The invention discloses a kind of liquid-packing chips, including upper layer case chip (1) and lower layer's case chip (2), wherein, the periphery of lower layer's case chip (2) be formed with raise upward circumferentially around wall (24), the upper surface circumferentially around wall (24) forms the first inclined surface, the lower surface of the upper layer case chip (1) forms the second inclined surface, the upper layer case chip (1) is set on lower layer's case chip (2), first inclined surface with second inclined surface is sealed against one another is bonded, Packed liquid storage space is formed between upper layer case chip (1) and lower layer's case chip (2).The upper layer case chip and lower layer's case chip connected by inclined surface sealing structure can be with automatic aligning, with good sealing effect, and it is larger that the liquid storage space formed is surrounded circumferentially around wall, larger amount of fluid sample can be accommodated, it avoids fluid sample very few and dries, cause the liquid-packing chip of assembling that cannot use.
Description
Technical field
The present invention relates to the devices for high vacuum instrument home position observation liquid phase sample, and in particular, to a kind of liquid envelope
Cartridge chip.
Background technique
With the rapid development of nanosecond science and technology, the instruments such as electron microscope, X-ray energy disperse spectroscopy have become analysis nanoscale
The main means of microstructure and ingredient, these instruments be using electron beam, X-ray etc. as light source, by with sample phase interaction
With, obtain the information of sample microstructure and ingredient, and these instruments need high vacuum environment work (usual sample room
Vacuum is higher than 10-4Pa), correspondingly, the sample drying observed by this is required is non-volatile.However, many samples are in liquid phase and solid phase
The structure of (after drying process) is different, for example the molecules such as vesica in the self-assembled structures of liquid phase, biomolecule and chemically reacted
Nonequilibrium state structure in journey etc., therefore, it is necessary to carry out home position observation for liquid phase sample in high vacuum environment.
High vacuum environment observe fluid sample, by using method be by liquid-packing in good seal performance
Container inside, to realize being isolated for sample and sample room high vacuum environment, while forming watch window on device, allow
The structural information that electron beam, X-ray etc. are passed through to obtain sample.Normally, it can be overlapped to form by the silicon wafer with interlayer
Hydraulic seal cabin, and with the silicon nitride (Si to electron beam, X-ray " transparent " on each silicon wafer3N4) film conduct observation
Window, after sealed compartment of the liquid-packing between two silicon wafers, the watch window on two silicon wafers is in alignment with each other to allow electronics
Beam, X-ray etc. pass through.
In order to allow electron beam, X-ray etc. to pass through, the thickness of silicon nitride film is very small, correspondingly, passes through silicon nitride
The window size that film is formed is also very small, to guarantee necessary intensity, silicon nitride film is avoided to make in the pressure of fluid sample
With lower rupture.In the very small size of situation of silicon nitride film window, due to preparation and operating error etc., two nitridations
Silicon thin film window is very easy to be aligned with respect to offset, this see electron beam, X-ray etc. cannot also cross two
Window is examined, so that the device of encapsulation is not available.In addition, the hydraulic seal cabin space very little formed between two silicon wafers, storage
Fluid sample amount it is few, it is easy to production observation sample in volatile dry, can equally packaging system be made not to be available.
Summary of the invention
The object of the present invention is to provide it is a kind of being capable of automatic aligning assembling and with the liquid packaging device of larger capacity.
To achieve the goals above, the present invention provides a kind of liquid-packing chip, including upper layer case chip and lower layer's encapsulation
Piece, wherein the periphery of lower layer's case chip be formed with raise upward circumferentially around wall, the upper surface circumferentially around wall
Be formed as the first inclined surface sloped inwardly and downwardly, the lower surface of the upper layer case chip is formed as and first inclined surface
The second inclined surface matched, the upper layer case chip are placed on lower layer's case chip, first inclined surface and described the
The fitting sealed against one another of two inclined surface, and be formed with closed liquid between the upper layer case chip and lower layer's case chip and deposit
Store up space.
Preferably, the first observation window is formed at the top of the upper layer case chip, the bottom of lower layer's case chip is formed
There is the second observation window, first observation window and second observation window are at least partly aligned to allow electron beam to penetrate through institute
State liquid-packing chip.
Preferably, first observation window and second observation window is rectangle and length direction is perpendicular to one another.
Preferably, the upper layer case chip includes first substrate and the first film layer, and the first substrate is formed with perforation
The first observation panel, the first film layer for allowing the electron beam of transmission electron microscope to be transmitted through is set to the first substrate
On lower surface, to form first observation window at first observation panel；And lower layer's case chip includes the second base
Plate and the second film layer, the second substrate are formed with the second observation panel of perforation, allow the electron beam of transmission electron microscope to transmit logical
Second film layer crossed fits on the upper surface of the second substrate, to form described at second observation panel
Two observation windows.
Preferably, the cross section of first observation panel is wide at the top and narrow at the bottom, and the cross section of second observation panel is lower width
It is upper narrow.
Preferably, the first substrate and the second substrate are monocrystalline silicon piece, the first film layer and described second
Film layer is silicon nitride film.
Preferably, the first substrate and the second substrate with a thickness of 200-300 μm, the first substrate and described
The second substrate is the square of side length 2-3mm；The first film layer and second film layer with a thickness of 20-150nm.
Preferably, the length of first observation window and second observation window is 20-1000 μm, and described first sees
The width for examining window and second observation window is 20-40 μm.
Preferably, the lower surface of the upper layer case chip is equipped with the identical interlayer of multiple thickness, and multiple interlayers are located at institute
It states near the first observation window.
Preferably, the interlayer with a thickness of 100-2000nm.
Through the above technical solutions, the upper layer case chip and lower layer's case chip that are connected by inclined surface sealing structure can be certainly
Dynamic alignment has good sealing effect, and it is larger to surround the liquid storage space formed circumferentially around wall, can accommodate compared with
A large amount of fluid sample avoids fluid sample very few and volatilizees cause sample drying in operation, leads to the liquid of assembling
Packaging system is not available.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is a kind of cross-sectional view of the liquid-packing chip of embodiment according to the present invention, at the middle and upper levels case chip and
Lower layer's case chip is separated from each other.
Fig. 2 is a kind of cross-sectional view of the liquid-packing chip of embodiment according to the present invention, at the middle and upper levels case chip and
Lower layer's case chip is engaged with each other.
Fig. 3 is the structural schematic diagram for showing a kind of lower surface of upper layer case chip of embodiment according to the present invention.
Fig. 4 is the structural schematic diagram for showing a kind of upper surface of lower layer's case chip of embodiment according to the present invention.
Fig. 5 is a kind of knot of the liquid-packing chip of embodiment according to the present invention from the top of upper layer case chip
Structure schematic diagram.
Description of symbols
1 upper layer case chip, 2 lower layer's case chip
11 first substrate, 12 the first film layer
13 first observation panel, 14 interlayer
21 the second substrate, 22 second film layer
23 second observation panels 24 are circumferentially around wall
Specific embodiment
Below in conjunction with attached drawing, detailed description of the preferred embodiments.It should be understood that this place is retouched
The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
In the present invention, in the absence of explanation to the contrary, the noun of locality used such as " upper and lower " typically refers to liquid envelope
Relative bearing when cartridge chip is horizontal positioned.
The present invention provides a kind of liquid-packing chips, including upper layer case chip 1 and lower layer's case chip 2, wherein under described
Layer case chip 2 periphery be formed with raise upward circumferentially around wall 24, the upper surface circumferentially around wall 24 be formed as to
The first inclined surface that is interior and tilting down, the lower surface of the upper layer case chip 1 are formed as matching with first inclined surface
The second inclined surface, the upper layer case chip 1 is set on lower layer's case chip 2, first inclined surface and described second
Inclined surface fitting sealed against one another, and form Packed liquid between the upper layer case chip 1 and lower layer's case chip 2 and deposit
Store up space.
As depicted in figs. 1 and 2, upper layer case chip 1 and lower layer's case chip 2 form the first inclined surface and the in peripheral region respectively
Two inclined surface, along the position being in alignment with each other vertically, first inclined surface is identical with the gradient of second inclined surface, thus
The two can be hermetically bonded.Particularly, due to the presence of inclined surface structure, upper layer case chip 1 can gradually from start with
The higher point of lower layer's case chip contact slides into suitable position, realizes automatic aligning, and upper layer case chip 1 and lower layer is avoided to encapsulate
The problems such as unjustified caused misalignment of watch window up and down of piece 2 and poor sealing；In addition, the sky surrounded circumferentially around wall 24
Between for accommodate fluid sample cavity lateral extent, generally speaking relative to liquid-packing chip, the range of cavity is very big,
More fluid sample can be accommodated, the liquid accommodated during assembling upper layer case chip 1 and lower layer's case chip 2 is avoided to wave
It is dry dry.
In the assembling process of the liquid-packing chip, oxygen plasma can be used respectively to 1 He of upper layer case chip
2 surfaces opposite to each other of lower layer's case chip carry out hydrophilic treated, after placing lower layer's case chip 2, due to depositing circumferentially around wall 24
So that the upper surface of lower layer's case chip 2 forms open container, after injecting fluid sample on lower layer's case chip 2, by upper layer
It after fluid sample is smeared in the lower surface of case chip 1, is placed on lower layer's case chip 2, and is applied in the edge of upper layer case chip 1
Epoxide-resin glue is smeared, realizes the sealed connection of upper layer case chip 1 and lower layer's case chip 2.Wherein, by upper layer case chip 1 gradually
When pushing, the first inclined surface can be made increasingly more tightly to be bonded with the second inclined surface, realize and be tightly connected.
In addition, the top of the upper layer case chip 1 is formed with the first observation window, the bottom of lower layer's case chip 2 is formed
There is the second observation window, first observation window and second observation window are at least partly aligned to allow electron beam transmission through institute
State liquid-packing chip.First observation window and second observation window are spaced each other, wherein accommodating fluid sample, work as electricity
When beamlet is transmitted through the fluid sample between first observation window and second observation window, it can realize that imaging is seen
It examines.Liquid-packing chip of the invention is mainly used for transmission electron microscope observation, and size is relatively small, first observation window and institute
It states to be smaller convenient for electron beam transmitted thickness at the second observation window, and structural strength is relatively low, therefore should not be designed as larger
Size, alignment operation difficulty is relatively large, can easily realize the first observation window and institute using structures described above
State the alignment of the second observation window.
In addition, first observation window and second observation window is rectangle and length direction is perpendicular to one another.Such as Fig. 5
It is shown, respectively laterally, the first observation window for longitudinally extending and the second observation window intersect to form allow transmission electron beam to pass through logical
Road.As described above, the structural strength of upper layer case chip 1 and lower layer's case chip 2 at observation window is smaller, therefore the size of observation window
It is relatively small, the present invention by first observation window and second observation window be designed as the lesser rectangle of width (such as Fig. 3,
Shown in Fig. 4), in the case where the first observation window and the second observation window perpendicularly cross each other, the two, which is easier to be aligned to be formed, to be allowed
The channel that transmission electron beam passes through allows each other the holding part with biggish offset in the longitudinal and transverse direction
Alignment.Specifically, the upper layer case chip 1 includes first substrate 11 and the first film layer 12, and the first substrate 11 is formed with
First observation panel 13 of perforation, the first film layer 12 for allowing the electron beam of transmission electron microscope to be transmitted through are set to described the
On the lower surface of one substrate 11, to form first observation window at first observation panel 13；And lower layer's encapsulation
Piece 2 includes the second substrate 21 and the second film layer 22, and the second substrate 21 is formed with the second observation panel 23 of perforation, is allowed saturating
Second film layer 22 that the electron beam of radio mirror is transmitted through fits on the upper surface of the second substrate 21, in institute
It states and forms second observation window at the second observation panel 23.First substrate 11 and the second substrate 21 are the main of liquid-packing chip
Strength structure, composition accommodate the chamber of fluid sample, therefore, have relatively large thickness, to allow transmission electron beam to pass through,
It is respectively formed the first observation panel 13 and the second observation panel 23；And the first film layer 12 and the second film layer 22 have lesser thickness
Degree allows electron beam to be transmitted through, fluid sample is accommodated between the first film layer 12 and the second film layer 22, to allow electronics
Beam transmission imaging.
Further, the cross section of first observation panel 13 is wide at the top and narrow at the bottom, the cross section of second observation panel 23
It is low wide and up narrow.That is, the first observation panel 13 and the second observation panel 23 are formed as structure wide outside and narrow inside, it is suitable to can permit electron beam
Pass through sharply, the structure around observation panel is avoided to influence the transmission path of electron beam.
Specifically, the first substrate 11 and the second substrate 21 are monocrystalline silicon piece, the first film layer 12 and institute
Stating the second film layer 22 is silicon nitride film.Monocrystalline silicon piece can be preferably used in first substrate 11 and the second substrate 21, or
The materials such as quartz, glass, sapphire or stainless steel can be used to be made.Silicon nitride film intensity with higher, and can
Electron beam is allowed to be transmitted through, it is of course also possible to alternatively use graphene film.In addition, silicon nitride film is only seen first
It examines as the primary structure for bearing fluid sample pressure at mouth 13 and the second observation panel 23, and in other positions, monocrystalline silicon piece is
Main support construction, therefore, silicon nitride film can be more stably supported at the first observation panel 13 and the second observation panel 23
Place, without being easily broken.
Preferably, the first substrate 11 and the second substrate 21 with a thickness of 200-300 μm, the first substrate 11
The square for being side length 2-3mm with the second substrate 21；The thickness of the first film layer 12 and second film layer 22
For 20-150nm.First substrate 11 and the second substrate 21 are the identical square of size, and on the four edges of square, the
The gradient of one inclined surface and the second inclined surface and of same size.
Furthermore it is preferred that the length of first observation window and second observation window is 20-1000 μm, and described
The width of first observation window and second observation window is 20-40 μm.The size of first observation window and the second observation window can be with that
This cooperation is adjusted, wherein the length dimension of the two can determine the offset allowed each other, and the width dimensions of the two are then
Determine the lateral dimension for the transmitted electron beam passage to be formed (shown in Fig. 5).
In addition, as shown in Figure 1, Figure 2, Figure 3 shows, the lower surface of the upper layer case chip 1 is equipped with the identical interlayer of multiple thickness
14, multiple interlayers 14 are located near first observation window.Can be seen that interlayer 14 in conjunction with Fig. 1 and Fig. 3 can be cuboid
Structure.By select different-thickness interlayer 14, the fluid sample space of available different height size, specifically,
In the case that upper layer case chip 1 and lower layer's case chip are tightly connected by the first inclined surface and the second inclined surface, since there are micro-
Small deformation, interlayer 14 can influence upper layer case chip 1 and lower layer's case chip 2 in the distance of observation window.Interlayer 14 can also
To play the role of improving liquid-packing chip compression strength, unexpected fail in compression is avoided；In addition, interlayer 14 is to upper layer case chip
Liquid flowing between 1 and lower layer's case chip 2 has blocking effect, can slow down external sealant to flowing at observation window.Every
Layer 14 can by silicon wafer depositing metal particles formed, such as gold, platinum or copper etc..
Preferably, the interlayer 14 with a thickness of 100-2000nm.
It is described the prefered embodiments of the present invention in detail above in conjunction with attached drawing, still, the present invention is not limited to above-mentioned realities
The detail in mode is applied, within the scope of the technical concept of the present invention, a variety of letters can be carried out to technical solution of the present invention
Monotropic type, these simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (9)
1. a kind of liquid-packing chip, including upper layer case chip (1) and lower layer's case chip (2), which is characterized in that lower layer's envelope
The periphery of load (2) be formed with raise upward circumferentially around wall (24), the upper surface circumferentially around wall (24) is formed as
The first inclined surface sloped inwardly and downwardly, the lower surface of the upper layer case chip (1) are formed as and first inclined surface phase
Second inclined surface of cooperation, the upper layer case chip (1) are placed on lower layer's case chip (2), first inclined surface and institute
The fitting sealed against one another of the second inclined surface is stated, and is formed between the upper layer case chip (1) and lower layer's case chip (2) close
The liquid storage space closed is formed with the first observation window at the top of the upper layer case chip (1), lower layer's case chip (2)
Bottom is formed with the second observation window, and first observation window and second observation window are at least partly aligned to allow electron beam saturating
It penetrates through the liquid-packing chip.
2. liquid-packing chip according to claim 1, which is characterized in that first observation window and second observation
Window is rectangle and length direction is perpendicular to one another.
3. liquid-packing chip according to claim 2, which is characterized in that the upper layer case chip (1) includes the first base
Plate (11) and the first film layer (12), the first substrate (11) are formed with the first observation panel (13) of perforation, allow to transmit electricity
The first film layer (12) that the electron beam of mirror is transmitted through is set on the lower surface of the first substrate (11), in institute
It states and forms first observation window at the first observation panel (13)；And
Lower layer's case chip (2) includes the second substrate (21) and the second film layer (22), and the second substrate (21) is formed with
The second observation panel (23) of perforation, second film layer (22) for allowing the electron beam of transmission electron microscope to be transmitted through fit in institute
On the upper surface for stating the second substrate (21), to form second observation window at second observation panel (23).
4. liquid-packing chip according to claim 3, which is characterized in that the cross section of first observation panel (13) is
Wide at the top and narrow at the bottom, the cross section of second observation panel (23) is low wide and up narrow.
5. liquid-packing chip according to claim 3, which is characterized in that the first substrate (11) and second base
Plate (21) is monocrystalline silicon plate, and the first film layer (12) and second film layer (22) are silicon nitride film.
6. liquid-packing chip according to claim 5, which is characterized in that the first substrate (11) and second base
Plate (21) with a thickness of 200 μm -300 μm, the first substrate (11) and the second substrate (21) be side length 2mm-3mm just
It is rectangular；The first film layer (12) and second film layer (22) with a thickness of 20nm-150nm.
7. liquid-packing chip according to claim 1, which is characterized in that first observation window and second observation
The length of window is 20 μm -1000 μm, and the width of first observation window and second observation window is 20 μm -40 μm.
8. liquid-packing chip according to claim 1, which is characterized in that the lower surface of the upper layer case chip (1) is set
There is the identical interlayer of multiple thickness (14), which is located near first observation window.
9. liquid-packing chip according to claim 8, which is characterized in that the interlayer (14) with a thickness of 100nm-
2000nm。
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| CN201610677166.6A CN106324000B (en) | 2016-08-16 | 2016-08-16 | Liquid-packing chip |
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| CN201610677166.6A CN106324000B (en) | 2016-08-16 | 2016-08-16 | Liquid-packing chip |
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| CN106324000B true CN106324000B (en) | 2018-11-16 |
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| US20220102107A1 (en) * | 2019-02-05 | 2022-03-31 | Germán Sciaini | Nanofluidic carrier |
| CA3129209A1 (en) * | 2019-02-05 | 2020-08-13 | German SCIAINI | Nanofluidic cell and loading platform |
| CN110736760B (en) * | 2019-10-28 | 2021-11-09 | 厦门超新芯科技有限公司 | Transmission electron microscope in-situ electrochemical detection chip and manufacturing method thereof |
| WO2023175749A1 (en) * | 2022-03-15 | 2023-09-21 | 株式会社日立製作所 | Sample holding tool, electron ray device, and manufacturing method for sample holding tool |
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