CN110514677A - A kind of in-situ liquid chamber chip and preparation method thereof - Google Patents
A kind of in-situ liquid chamber chip and preparation method thereof Download PDFInfo
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- CN110514677A CN110514677A CN201910182781.3A CN201910182781A CN110514677A CN 110514677 A CN110514677 A CN 110514677A CN 201910182781 A CN201910182781 A CN 201910182781A CN 110514677 A CN110514677 A CN 110514677A
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- 239000007788 liquid Substances 0.000 title claims abstract description 66
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 102
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 102
- 239000010703 silicon Substances 0.000 claims abstract description 102
- 239000010410 layer Substances 0.000 claims abstract description 80
- 229910052751 metal Inorganic materials 0.000 claims abstract description 36
- 239000002184 metal Substances 0.000 claims abstract description 36
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 32
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000010894 electron beam technology Methods 0.000 claims abstract description 24
- 239000012790 adhesive layer Substances 0.000 claims abstract description 20
- 238000002347 injection Methods 0.000 claims abstract description 17
- 239000007924 injection Substances 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- 238000003384 imaging method Methods 0.000 claims abstract description 5
- 239000010408 film Substances 0.000 claims description 82
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229920002120 photoresistant polymer Polymers 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000001259 photo etching Methods 0.000 claims description 14
- 238000005530 etching Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 238000001459 lithography Methods 0.000 claims description 9
- 238000001020 plasma etching Methods 0.000 claims description 9
- 238000001039 wet etching Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 229910003978 SiClx Inorganic materials 0.000 claims description 4
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Micromachines (AREA)
Abstract
The present invention discloses a kind of in-situ liquid chamber chip and preparation method thereof, the in-situ liquid chamber chip includes egative film and cover plate, the cover plate is made of two sides with the silicon chip of silicon nitride film layer, and there are two the electron beam forms that symmetrical liquid injection port and one are located at center on the cover plate；The egative film is made of two sides with the silicon chip of silicon nitride film layer, and the egative film includes adhesive layer and observation window, and the adhesive layer is generally metal bonding layer, and the observation window is located at plate center position；The cover plate is be bonded by metal bonding layer adhesive layer with egative film, and the electron beam form vertical alignment of the observation window of the egative film and the cover plate is in the same size.The in-situ liquid chamber chip improves imaging resolution using silicon nitride film layer as support layer, and observable sample liquid layer reaches 50-2000nm, adhesive layer good airproof performance, effective protection Electronic Speculum, integrated manufacture method simplicity.
Description
Technical field
The invention belongs to in-situ characterization fields, and in particular to a kind of in-situ liquid chamber chip and preparation method thereof.
Background technique
In situ TEM technology is with its superelevation spatial resolution (atom level) and Superfast time resolution rate (Millisecond)
Advantage and be widely used in each scientific domain, this provides full the exploration of new material microstructure for researcher
New thinking and research method.Currently, in situ TEM technology has successfully introduced, atmosphere, electric field, thermal field etc. are external to swash
Encourage signal, and the imaging of the transmission electron microscope of in-situ liquid environment due to environment in its high vacuum and there are biggish challenges.With close
The fast development of micro-nano processing technology over year, the in situ TEM liquid cell of different structure and function are developed and complete in succession
Kind, liquid phase reactor liquid cell and graphene liquid cell in situ have been carried out atomic resolution at present, and researcher can
With by realizing analysis of the atomic scale to the pattern, surface and interface component, atomic structure of material in this micro-nano reactor,
Explore the relationship of material microstructure and material property.
Currently used for in-situ liquid chamber chip major design be all upper piece and bottom sheet separate, using unit install additional sample after again
It is packaged, it is inconvenient, and be easy to influence detection quality because the problems such as leakproofness is poor caused by individual operations difference, leakage,
Fluid seepage destroys Electronic Speculum.
Summary of the invention
The present invention provides a kind of in-situ liquid chamber chips and preparation method thereof, and the purpose is to realize in-situ liquid chamber chip
Integrated design, while solve the influences such as above-mentioned in-situ liquid chamber chip spatial resolution low, leakproofness is poor, leakage detection matter
The problem of amount.
The present invention provides a kind of in-situ liquid chamber chip and preparation method thereof, the in-situ liquid chamber chip includes cover plate
And egative film, the cover plate are made of two sides with the silicon chip of silicon nitride film layer, there are two symmetrical fluid injections on the cover plate
Mouth and an electron beam form positioned at center；The egative film is made of two sides with the silicon chip of silicon nitride film layer,
The egative film includes adhesive layer and observation window, and the adhesive layer is generally metal bonding layer, and the observation window is located at egative film
Center；The cover plate is be bonded by metal bonding layer adhesive layer with egative film, the observation window of the egative film and the cover plate
Electron beam form vertical alignment, it is in the same size.
Simultaneously the present invention provides a kind of in-situ liquid chamber chip and preparation method thereof, which includes following step
It is rapid:
Step S1: production egative film；
Step S2: production cover plate；
Step S3: cover plate and egative film are bonded by metal bonding layer, form integrated in-situ liquid chamber chip.
Further, the egative film have first surface and with the opposite facing second surface of first surface, the egative film system
It is as follows to make step S1:
The silicon chip of S101, preparation two sides with silicon nitride film layer, 4 cun of silicon chip size, thickness 50-500um, the nitridation
Silicon layer film thickness 5-200nm；
S102, observation window pattern is transferred to from lithography mask version in ultraviolet photolithographic machine exposure 10-30s using photoetching process
Silicon chip first surface in S101, then develop in developer for positive photoresist 30-60s, takes out silicon chip and is rinsed with deionized water；
S103, the nitridation using reactive ion etching process, on the silicon chip first surface that S102 is produced at watch window
Silicon etching falls, and then silicon chip first surface is put into acetone soak 10-30s upward, is finally rinsed with deionized water, removes light
Photoresist；
S104, the silicon chip second surface produced in S103 is put into mass percent concentration upward for 5% hydrogen tetramethyl hydrogen-oxygen
Change and carry out wet etching in ammonium (TMAH) solution, etching temperature is 90 DEG C, is etched to first surface and leaves behind watch window nitridation
Silicon insulating layer of thin-film takes out silicon chip and is rinsed with ionized water；
S105, using photoetching process, expose 10-30s in ultraviolet photolithographic machine, metal bonding layer pattern shifted from lithography mask version
The silicon chip first surface produced to step S104, then develop in developer for positive photoresist 30-60s, then is rushed with deionized water
It washes；
S106, using thermal evaporation, one layer of metal bonding coating is deposited in the silicon chip first surface that S105 is produced, then by silicon substrate
Piece first surface is put into acetone soak removing 10-30s upward, is finally rinsed with deionized water, removes photoresist, it is viscous to leave metal
Tie layer；
S107, the silicon chip for producing S106 carry out laser scribing, are divided into independent egative film.
Further, the cover plate has third surface and the 4th surface with third surface opposite pair, the cover plate system
Steps are as follows for work:
The silicon chip of S201, preparation two sides with silicon nitride film layer, 4 cun of silicon chip size, thickness 50-500um, the nitridation
Silicon membrane layer thickness 5-200nm；
S202, using photoetching process, the silicon chip in S201 is exposed into 10-30s in ultraviolet photolithographic machine, by liquid injection port pattern from light
It carves mask plate and is transferred to silicon chip third surface, then develop in developer for positive photoresist 30-60s, then cleans table with deionized water
Face；
S203, the silicon nitride using reactive ion etching process, at the 4th surface upper liquid filling mouth of silicon chip that S202 is produced
It etches away, then the 4th surface of silicon chip is put into acetone soak removing 10-30s upward, is finally rinsed with cleaning agent, remove light
Photoresist；
S204, the 4th surface of silicon chip that S203 is produced is put into mass percent concentration upward for 5% hydrogen tetramethyl hydroxide
Carry out wet etching in ammonium (TMAH) solution, etching temperature is 90 DEG C, and being etched to first surface, to leave behind liquid injection port silicon nitride exhausted
Edge layer film takes out silicon chip and is rinsed with ionized water；
S205, using photoetching process, expose 10-30s in ultraviolet photolithographic machine, electron beam form pattern shifted from lithography mask version
The silicon chip third surface produced to S204, then develop in developer for positive photoresist 30-60s；
S206, the nitrogen using reactive ion etching process, on the silicon chip third surface that S205 is produced at electron beam form
SiClx etches away, and then silicon chip third surface is put into acetone soak removing 10-30s upward, is finally rinsed, gone with cleaning agent
Except photoresist；
S207, the 4th surface of silicon chip that S206 is produced is put into mass percent concentration upward for 5% hydrogen tetramethyl hydroxide
Wet etching is carried out in ammonium (TMAH) solution, etching temperature is 90 DEG C, is etched to first surface and leaves behind the nitridation of electron beam form
Silicon insulating layer of thin-film takes out silicon chip and is rinsed with ionized water；
S208, the silicon chip for producing S207 carry out laser scribing, are divided into independent cover plate.
Further, the cover plate and the egative film are bonded by metal bonding layer, and production method step S3 is as follows:
The egative film and cover plate of S301, above-mentioned S107 and S208 production are bonded by metal bonding layer, are assembled integrally formula original position liquid
Body chamber chip.
In above scheme, the silicon chip two sides of the cover plate and egative film is covered with one layer of silicon nitride film layer.Described
Silicon nitride film layer is with a thickness of 5-200nm.Further, the silicon nitride film layer can be used as the cover plate electron beam view
The thin-film material of window；The silicon nitride film layer can be used as the support layer of sample at the egative film observation window, ultra-thin nitrogen
SiClx form film effectively improves imaging resolution, reduces background noise.
In above scheme, the electron beam form of the cover plate and the watch window size of the egative film are 30um*50um,
Vertical alignment.
In above scheme, the adhesive layer is generally metal bonding layer.The metal bonding layer is with a thickness of 50-
Aluminium, copper, titanium, iron, gold, platinum, palladium, indium, tin can be selected in 2000nm, metal used.
In above scheme, in the bonding egative film and cover plate step S3, the observation window of egative film and the electron beam of cover plate are regarded
Window alignment, the second surface of the cover plate and the third surface of the egative film are bonded by metal bonding layer adhesive layer.
The beneficial effect that the present invention generates has following several respects:
A kind of in-situ liquid chamber chip provided by the invention, electron beam form and observation window are to support with silicon nitride film layer
Layer effectively improves imaging resolution, reduces background noise.
A kind of in-situ liquid chamber chip provided by the invention, metal bonding layer thickness is controllable, reaches observation sample liquid layer
50-2000nm, adhesive layer good airproof performance, effective protection Electronic Speculum.
A kind of in-situ liquid chamber chip production method provided by the invention, manufactured cover plate and egative film pass through metal bonding layer
Bonding, realizes integrated design and production, and can sample directly be added by liquid injection port in when use, closes liquid injection port, operates
Simplicity, sealing effect are good.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of in-situ liquid chamber chip of the embodiment of the present invention.
Fig. 2 is a kind of cover plate exploded view of in-situ liquid chamber chip of the embodiment of the present invention.
Fig. 3 is a kind of egative film exploded view of in-situ liquid chamber chip of the embodiment of the present invention.
Fig. 4 is a kind of process flow chart of the production method of in-situ liquid chamber chip of the embodiment of the present invention.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described.Described embodiment is only the present invention
The embodiment of a part, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, should fall within the scope of the present invention.Below
Embodiment is intended to be used to explain the present invention, and is not considered as limiting the invention.The technical side that any equivalence replacement obtains
Case is within the protection scope of the present invention.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.
The embodiment of the invention discloses a kind of in-situ liquid chamber chips, and structure is as shown in Figure 1, Figure 2, Figure 3 shows, the original position liquid
Body chamber chip includes cover plate 1 and egative film 7, and the cover plate 1 is made of two sides with the silicon chip 3 of silicon nitride film layer 2,4, described
There are two the electron beam forms 6 that symmetrical liquid injection port 5 and one are located at center on cover plate 1；The egative film 7 is had by two sides
The silicon chip 10 of silicon nitride film layer 9,11 is made, and the egative film 7 includes adhesive layer 8 and observation window 12, the adhesive layer 8 one
As be metal bonding layer, the observation window 12 is located at 7 center of egative film；The cover plate 1 passes through metal bonding layer with egative film 7
Adhesive layer 8 is bonded, and 6 vertical alignment of electron beam form of the observation window 12 of the egative film 7 and the cover plate 1 is in the same size.
The embodiment of the invention discloses a kind of production methods of in-situ liquid chamber chip simultaneously, as shown in figure 4, the production side
Method the following steps are included:
Step S1: production egative film 7；
Step S2: production cover plate 1；
Step S3: cover plate 1 and egative film 7 are bonded by metal bonding layer adhesive layer 8, form integrated in-situ liquid chamber chip.
Particularly, the egative film 7 have first surface and with the opposite facing second surface of first surface, the egative film 7 makes
It is as follows to make step S1:
S101, prepare the silicon chip that two sides has silicon nitride film layer, 4 cun of silicon chip size, silicon chip thickness 200um is described
Silicon nitride layer film thickness 200nm；
S102, observation window pattern is transferred to from lithography mask version in ultraviolet photolithographic machine exposure 15s using photoetching process
Silicon chip first surface in S101, then develop in developer for positive photoresist 50s；
S103, the nitridation using reactive ion etching process, on the silicon chip first surface that S102 is produced at watch window
Silicon etching falls, and then silicon chip first surface is put into acetone soak 1s upward, is finally rinsed with deionized water, removes photoetching
Glue；
S104, the silicon chip second surface produced in S103 is put into mass percent concentration upward for 5% hydrogen tetramethyl hydrogen-oxygen
Change and carry out wet etching in ammonium (TMAH) solution, etching temperature is 90 DEG C, is etched to first surface and leaves behind watch window nitridation
Silicon insulating layer of thin-film takes out silicon chip and is rinsed with ionized water；
S105, metal bonding layer pattern is transferred to from lithography mask version in ultraviolet photolithographic machine exposure 15s using photoetching process
The silicon chip first surface that step S104 is produced, then develop in developer for positive photoresist 50s；
S106, using thermal evaporation, one layer of metal bonding coating is deposited in the silicon chip first surface that S105 is produced, then by silicon substrate
Piece first surface is put into acetone soak removing 20s upward, is finally rinsed with deionized water, removes photoresist, leaves metal bonding
Layer；
S107, the silicon chip for producing S106 carry out laser scribing, are divided into independent egative film 7, size 3mm*3mm.
Particularly, the cover plate 1 has third surface and the 4th surface with third surface opposite pair, and the cover plate 1 is made
It is as follows to make step S2:
S201, prepare the silicon chip that two sides has silicon nitride film layer, 4 cun of silicon chip size, silicon chip thickness 200um is described
Silicon nitride film layer thickness 200nm；
S202, using photoetching process, the silicon chip in S201 is exposed into 15s in ultraviolet photolithographic machine, by liquid injection port pattern from photoetching
Mask plate is transferred to silicon chip third surface, and then develop in developer for positive photoresist 50s, then with deionized water clean the surface；
S203, the silicon nitride using reactive ion etching process, at the 4th surface upper liquid filling mouth of silicon chip that S202 is produced
It etches away, then the 4th surface of silicon chip is put into acetone soak removing 20s upward, is finally rinsed with deionized water, remove light
Photoresist；
S204, the 4th surface of silicon chip that S203 is produced is put into mass percent concentration upward for 5% hydrogen tetramethyl hydroxide
Carry out wet etching in ammonium (TMAH) solution, etching temperature is 90 DEG C, and being etched to first surface, to leave behind liquid injection port silicon nitride exhausted
Edge layer film takes out silicon chip and is rinsed with ionized water；
S205, electron beam form pattern is transferred to from lithography mask version in ultraviolet photolithographic machine exposure 15s using photoetching process
The silicon chip third surface that S204 is produced, then develop in developer for positive photoresist 50s；
S206, the nitrogen using reactive ion etching process, on the silicon chip third surface that S205 is produced at electron beam form
SiClx etches away, and then silicon chip third surface is put into acetone soak removing 20s upward, is finally rinsed, gone with deionized water
Except photoresist；
S207, the 4th surface of silicon chip that S206 is produced is put into mass percent concentration upward for 5% hydrogen tetramethyl hydroxide
Carry out wet etching in ammonium (TMAH) solution, etching temperature is 90 DEG C, and being etched to first surface, to leave behind liquid injection port silicon nitride exhausted
Edge layer film takes out silicon chip and is rinsed with ionized water；
S208, the silicon chip for producing S207 carry out laser scribing, are divided into independent cover plate 1, size 3mm*3mm.
Step S3: group reload 7 with cover plate 1.The observation window 12 of egative film 7 and the electron beam form 6 of cover plate 1 are vertical right
Together, the third surface of the second surface of the cover plate 1 and the egative film 7 is bonded by metal bonding layer adhesive layer 8, forms one
Change in-situ liquid chamber chip.
Optionally, when making egative film 7,12 size of watch window is 30um*50um.
Optionally, when making cover plate 1,5 pattern of liquid injection port is rectangle or square, 5 ruler of the present embodiment liquid injection port
Very little is 300um*400um.
Optionally, when making egative film 7, the adhesive layer 8 is generally metal bonding layer, with a thickness of 1000nm, metal used
Aluminium, copper, titanium, iron, gold, platinum, palladium, indium, tin can be selected.
During the work time, user of service can be loaded by sample preparation storehouse in liquid injection port, after closing liquid injection port, by leak detection
After be put into electron microscope and observe.
Finally it should be noted that the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, to the greatest extent
Invention is explained in detail referring to above-described embodiment for pipe, it should be understood by a person of ordinary skill in the art that technology
Personnel read present specification after still can with modifications or equivalent substitutions are made to specific embodiments of the invention, but this
A little modifications are changed within all without departing from the present patent application accompanying claims protection scope.
Claims (10)
1. a kind of in-situ liquid chamber chip and preparation method thereof, it is characterised in that: the in-situ liquid chamber chip include egative film and
Cover plate, the cover plate are made of two sides with the silicon chip of silicon nitride film layer, and there are two symmetrical liquid injection ports on the cover plate
It is located at the electron beam form of center with one；The egative film is made of two sides with the silicon chip of silicon nitride film layer, institute
Stating egative film includes adhesive layer and observation window, and the adhesive layer is generally metal bonding layer, and the observation window is located in egative film
Heart position；The cover plate is be bonded by metal bonding layer adhesive layer with egative film, the observation window of the egative film and the cover plate
Electron beam form vertical alignment, it is in the same size.
2. a kind of in-situ liquid chamber chip and preparation method thereof, it is characterised in that: the production method the following steps are included:
Step S1: production egative film；
Step S2: production cover plate；
Step S3: cover plate and egative film are bonded by metal bonding layer, form integrated in-situ liquid chamber chip.
3. a kind of in-situ liquid chamber chip according to claim 2 and preparation method thereof, it is characterised in that: the egative film tool
Have first surface and with the opposite facing second surface of first surface, the negative film making step S1 is as follows:
The silicon chip of S101, preparation two sides with silicon nitride film layer, 4 cun of silicon chip size, thickness 50-500um, the nitridation
Silicon layer film thickness 5-200nm；
S102, observation window pattern is transferred to from lithography mask version in ultraviolet photolithographic machine exposure 10-30s using photoetching process
Silicon chip first surface in S101, then develop in developer for positive photoresist 30-60s, takes out silicon chip and is rinsed with deionized water；
S103, the nitridation using reactive ion etching process, on the silicon chip first surface that S102 is produced at watch window
Silicon etching falls, and then silicon chip first surface is put into acetone soak 10-30s upward, is finally rinsed with deionized water, removes light
Photoresist；
S104, the silicon chip second surface produced in S103 is put into mass percent concentration upward for 5% hydrogen tetramethyl hydrogen-oxygen
Change and carry out wet etching in ammonium (TMAH) solution, etching temperature is 90 DEG C, is etched to first surface and leaves behind watch window nitridation
Silicon insulating layer of thin-film takes out silicon chip and is rinsed with ionized water；
S105, using photoetching process, expose 10-30s in ultraviolet photolithographic machine, metal bonding layer pattern shifted from lithography mask version
The silicon chip first surface produced to step S104, then develop in developer for positive photoresist 30-60s, then is rushed with deionized water
It washes；
S106, using thermal evaporation, one layer of metal bonding coating is deposited in the silicon chip first surface that S105 is produced, then by silicon substrate
Piece first surface is put into acetone soak removing 10-30s upward, is finally rinsed with deionized water, removes photoresist, it is viscous to leave metal
Tie layer；
S107, the silicon chip for producing S106 carry out laser scribing, are divided into independent egative film.
4. a kind of in-situ liquid chamber chip according to claim 2 and preparation method thereof, it is characterised in that: the cover plate tool
There are third surface and the 4th surface with third surface opposite pair, the cover plate making step S2 is as follows:
The silicon chip of S201, preparation two sides with silicon nitride film layer, 4 cun of silicon chip size, thickness 50-500um, the nitridation
Silicon membrane layer thickness 5-200nm；
S202, using photoetching process, the silicon chip in S201 is exposed into 10-30s in ultraviolet photolithographic machine, by liquid injection port pattern from light
It carves mask plate and is transferred to silicon chip third surface, then develop in developer for positive photoresist 30-60s, then cleans table with deionized water
Face；
S203, the silicon nitride using reactive ion etching process, at the 4th surface upper liquid filling mouth of silicon chip that S202 is produced
It etches away, then the 4th surface of silicon chip is put into acetone soak removing 10-30s upward, is finally rinsed with cleaning agent, remove light
Photoresist；
S204, the 4th surface of silicon chip that S203 is produced is put into mass percent concentration upward for 5% hydrogen tetramethyl hydroxide
Carry out wet etching in ammonium (TMAH) solution, etching temperature is 90 DEG C, and being etched to first surface, to leave behind liquid injection port silicon nitride exhausted
Edge layer film takes out silicon chip and is rinsed with ionized water；
S205, using photoetching process, expose 10-30s in ultraviolet photolithographic machine, electron beam form pattern shifted from lithography mask version
The silicon chip third surface produced to S204, then develop in developer for positive photoresist 30-60s；
S206, the nitrogen using reactive ion etching process, on the silicon chip third surface that S205 is produced at electron beam form
SiClx etches away, and then silicon chip third surface is put into acetone soak removing 10-30s upward, is finally rinsed, gone with cleaning agent
Except photoresist；
S207, the 4th surface of silicon chip that S206 is produced is put into mass percent concentration upward for 5% hydrogen tetramethyl hydroxide
Wet etching is carried out in ammonium (TMAH) solution, etching temperature is 90 DEG C, is etched to first surface and leaves behind the nitridation of electron beam form
Silicon insulating layer of thin-film takes out silicon chip and is rinsed with ionized water；
S208, the silicon chip for producing S207 carry out laser scribing, are divided into independent cover plate.
5. a kind of in-situ liquid chamber chip according to claim 2 and preparation method thereof, it is characterised in that: the cover plate and
The egative film is bonded by metal bonding layer, and production method step S3 is as follows:
The egative film and cover plate of S301, above-mentioned S107 and S208 production are bonded by metal bonding layer, are assembled integrally formula original position liquid
Body chamber chip.
6. a kind of in-situ liquid chamber chip according to claim 1 and preparation method thereof, it is characterised in that: the cover plate
It is covered with one layer of silicon nitride film layer with the silicon chip two sides of egative film, the silicon nitride film layer is with a thickness of 5-200nm.
7. a kind of in-situ liquid chamber chip according to claim 6 and preparation method thereof, it is characterised in that: the nitridation
Silicon membrane layer can be used as the thin-film material of the cover plate electron beam form；The silicon nitride film layer can be used as the bottom
The support layer of sample at piece observation window effectively improves imaging resolution, reduces background noise.
8. a kind of in-situ liquid chamber chip according to claim 1 and preparation method thereof, it is characterised in that: the cover plate
The watch window size of electron beam form and the egative film is 30um*50um, vertical alignment.
9. a kind of in-situ liquid chamber chip according to claim 1 and preparation method thereof, it is characterised in that: the metal
For bonded layer with a thickness of 50-2000nm, aluminium, copper, titanium, iron, gold, platinum, palladium, indium, tin is can be selected in metal used.
10. a kind of in-situ liquid chamber chip according to claim 2 and preparation method thereof, it is characterised in that: the bonding
In egative film and cover plate step S3, the observation window of egative film and the electron beam align to view of cover plate, the second surface of the cover plate with
The third surface of the egative film is bonded by metal bonding layer adhesive layer, forms integrated in-situ liquid chamber chip.
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| CN201910182781.3A CN110514677A (en) | 2019-03-12 | 2019-03-12 | A kind of in-situ liquid chamber chip and preparation method thereof |
| PCT/CN2020/078968 WO2020182184A1 (en) | 2019-03-12 | 2020-03-12 | In-situ electrochemical detection chip, in-situ liquid cell chip, and in-situ heating chip for transmission electron microscope, and manufacturing method therefor |
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