CN103280527B - A kind of preparation method of the embedded electrode of plane - Google Patents
A kind of preparation method of the embedded electrode of plane Download PDFInfo
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- CN103280527B CN103280527B CN201310218033.9A CN201310218033A CN103280527B CN 103280527 B CN103280527 B CN 103280527B CN 201310218033 A CN201310218033 A CN 201310218033A CN 103280527 B CN103280527 B CN 103280527B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 75
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 75
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 75
- 239000000758 substrate Substances 0.000 claims abstract description 69
- 238000004528 spin coating Methods 0.000 claims abstract description 49
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 47
- 239000002184 metal Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 238000001259 photo etching Methods 0.000 claims abstract description 17
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 238000007711 solidification Methods 0.000 claims abstract description 13
- CXQXSVUQTKDNFP-UHFFFAOYSA-N Simethicone Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- -1 polydimethylsiloxane Polymers 0.000 claims description 88
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 57
- 229910052710 silicon Inorganic materials 0.000 claims description 57
- 239000010703 silicon Substances 0.000 claims description 57
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 229910052757 nitrogen Inorganic materials 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 24
- HEDRZPFGACZZDS-UHFFFAOYSA-N chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 20
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 17
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 17
- 241000252506 Characiformes Species 0.000 claims description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 15
- 239000010931 gold Substances 0.000 claims description 15
- 229910052737 gold Inorganic materials 0.000 claims description 15
- 230000000640 hydroxylating Effects 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N n-methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 11
- KRVSOGSZCMJSLX-UHFFFAOYSA-L Chromic acid Chemical compound O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000002390 adhesive tape Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N iso-propanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N n-heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 5
- 238000011105 stabilization Methods 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 229960002163 hydrogen peroxide Drugs 0.000 claims description 2
- 238000000059 patterning Methods 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 229920002799 BoPET Polymers 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 22
- 230000004048 modification Effects 0.000 abstract description 2
- 238000006011 modification reaction Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- 230000005611 electricity Effects 0.000 description 5
- 230000005669 field effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 description 4
- 101700056996 PMDS Proteins 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000010030 laminating Methods 0.000 description 4
- 230000001105 regulatory Effects 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000004020 conductor Substances 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N Phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 2
- 238000005090 crystal field Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000000609 electron-beam lithography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000813 microcontact printing Methods 0.000 description 2
- 125000003396 thiol group Chemical group [H]S* 0.000 description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N Trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- MYSTXZYFSGSVSD-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethanethiol Chemical compound CCC[Si](OC)(OC)OCS MYSTXZYFSGSVSD-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
Abstract
The invention discloses the preparation method of the embedded electrode of a kind of plane, it is adaptable to electrode preparation field, it is characterised in that completed by following steps: the cleaning of substrate；The modification of substrate；Photoetching electrode pattern on the substrate of modified；Evaporation metal electrode；The surface of metal electrode is modified；The stripping of photoresist；The solidification of spin coating PDMS and PDMS；Electrode is the step such as transfer from substrate.It achieves and at room temperature operates, it is to avoid radiation, solution are to organic semi-conductor damage and pollution；Degree of accuracy is high, can prepare complex pattern；The electrode structure prepared is the embedded electrode of plane.
Description
Technical field
The present invention relates to the preparation method of the embedded electrode of a kind of plane, belong to electrode preparation field.
Background technology
Since organic semiconductor comes out, field-effect transistor based on organic semiconducting materials enjoys people to pay close attention to.
Organic field effect tube is typically by compositions such as source-drain electrode, grid, insulating barrier, organic semiconductors.So imitating at organic field
Answering in the preparation of transistor, the preparation of source-drain electrode is an important ring.And organic semiconductor and the contact quality of source-drain electrode
Threshold voltage to device, mobility have important impact (physica status solidi (a) 2004,201,
1302-1331).The contact quality of organic semiconductor and source-drain electrode except having with the selection of electrode material outside the Pass, also with tool
The technology for preparing electrode of body is relevant with electrode structure.Therefore, the performance improving organic field effect tube is had by the preparation of electrode
Important impact.
Traditional electrode preparation method has photoetching process, electron beam lithography and vacuum mask deposition etc..But these three electrode
The method of preparation, is individually present the biggest shortcoming.For photoetching process, photoresist, glue and developer solution is gone all some to be had
Machine quasiconductor has certain damage and pollutes (Chemical reviews 2011,111,3358-3406；
ChemicalSociety reviews 2010,39,2643-2666), affect the performance of device；And electron beam lithography
Needing accurate expensive instrument, the scope preparing pattern is little, goes glue and developer solution also to organic as photoetching process simultaneously
Quasiconductor has certain damage and pollution, and high-power electron beam has strong radiation damage to organic semiconductor
(Advanced Materials2006,18,65-68), causes organic semiconductor to lose electric property, causes device
Energy is poor or loses performance；And the method for vacuum mask deposition, on the one hand the electrode size of preparation is relatively big, lines precision
Not, and the shape matching of figure
Limited, it is impossible to the figure that preparation is complicated.On the other hand, in the deposition process of electrode, heat radiation can be to organic half
Conductor causes certain damage (Advanced Materials 2008,20,2947-2951； Advanced Materials
2008,20,1511-1515), thus affect device performance.Therefore, traditional solution in method and radiation are to organic half
Conductor has damage, affects the performance of device.
For the shortcoming overcoming traditional electrode preparation method to be brought, Hu Wenping research group uses " film of gilding "
Method prepares electrode (Advanced Materials 2008,20,1511-1515； Applied Physics
Letters 2008,92,083309；Advanced Materials 2008,20,2947-2951； Applied
Physics Letters 2009,94,203304), the method advantage is to operate at normal temperatures and pressures, it is to avoid have
Machine quasiconductor contacts and radiates with solution to organic semi-conductor damage.But this method is only suitable for making single device,
Being not suitable for doing the circuit of complexity, integrated level is the highest.
Development along with printing technology, it would however also be possible to employ printing technology prepares electrode, such as micro-contact printing and nanometer
Trans-printing prepares electrode (Proceedings of the National Academy of Sciences of the
UnitedStates of America 2002, 99,10252-10256 ；Applied Physics Letters 1993,
63,2002-2004；Applied Physics Letters, 2002,81,562), both approaches is printing process
Separate with deposition process, make organic semiconductor not by other chemically and physically process influence, it is to avoid solution, high energy
The electron beam damage to quasiconductor, can also make the electrode pattern of complexity simultaneously.
Visible, along with the improvement of technology for preparing electrode, people progressively solve during technology for preparing electrode solution and
The problem that radiation etc. are the highest on organic semi-conductor impact and electrode pattern integrated level.But the most traditional electrode preparation side
Method, " film of gilding " method or micro-contact printing and nanometer trans-printing, the electrode structure that they are prepared such as Fig. 1 institute
Show, on the substrates 2 such as electrode 1 directly protrudes at insulating barrier, glass, silicon, therefore present between electrode 1 and insulating barrier
Step-like structure.As shown in Fig. 2, when organic semiconductor is transferred on this structure electrode 1, between two electrodes
Organic semiconductor is not all to form perfect laminating with insulating barrier, and the organic semiconductor near electrode is due to this electrode
Step-like structure and form arch, the organic semiconductor in arch area not and insulating barrier laminating, and is not easy to
Arch area forms defect, also results in the decline of organic semiconductor 3 and electrode 1 contact quality simultaneously.Therefore, You Jiban
Conductor is difficult on this electrode structure realize perfectly contacting and fitting with electrode and insulating barrier simultaneously, and causes this electricity
The device of electrode structure, its performance is affected bigger by contact.And J.J. Lee seminar nano impression has been prepared such as figure
Embedded electrode structure (Microelectronic Engineering 2011,88,1606-1609) shown in 3, this electricity
The height of pole have to be lower than the degree of depth of seal designs, so there is also organic semiconductor 3 and electrode 1 and insulating barrier equally
Perfect contact and the problem of laminating.
Summary of the invention
It is an object of the invention to provide the preparation method of the embedded electrode of a kind of plane, its guarantee at room temperature operates,
Avoid radiation, solution is to organic semi-conductor damage and pollutes；Degree of accuracy is high, can prepare complex pattern；Preparation
The electrode structure gone out is the embedded electrode of plane, i.e. electrode with insulating barrier at same plane, it is ensured that organic semiconductor and electrode and
Insulating barrier perfection contact and laminating.
For reaching above-mentioned purpose, the technical scheme is that and be achieved in that: the preparation of the embedded electrode of a kind of plane
Method, it is characterised in that: utilize method photoetching electrode pattern on substrate of photoetching, evaporation metal electrode afterwards, obtain
The metal electrode of patterning, then spin coating polydimethylsiloxane on the substrate with electrode, through poly dimethyl
After siloxanes PDMS solidification, electrode is shifted together with polydimethylsiloxane from substrate；Concrete
Step is as follows: the 1) cleaning of silicon substrate: the 5mm*10mm silicon chip cut is put into acetone ultrasonic 15 minutes, takes
Going out and dry up with nitrogen, be then placed in baking 5min in baking oven, temperature is 100 degrees Celsius;Put into chromic acid after drying to wash
Immersion is steeped 20 minutes, and taking-up with deionized water rinsing several times, finally dries up with nitrogen；
2) OTS of silicon substrate modifies: (1) silicon chip surface hydroxylating: preparation Piranha washing liquid, Piranha washing liquid
Configuration be concentrated sulphuric acid and hydrogenperoxide steam generator
Volume ratio is 7:3, and then silicon chip is put into Piranha washing liquid 30min, takes out silicon chip deionized water rinsing
Several times, finally use
Nitrogen dries up；
(2) the silicon chip surface OTS(octadecyl trichlorosilane alkane after hydroxylating) to modify: preparation is molten with normal heptane
The OTS solution of agent, optium concentration is 0.075% 0.1%, then the silicon chip after hydroxylating is put into wherein 14 hours
Rear taking-up；Soak 5 minutes with chloroform, the most ultrasonic 10 minutes, dry up with nitrogen afterwards, put into baking oven baking
5min, temperature is at 70 to 100 degrees Celsius, in order to remove the absorption chloroform at substrate surface, final successfully at silicon
One layer of OTS has been modified on surface, reduces the surface energy of substrate, and the size of this modification rear surface energy is direct and octadecyl
The concentration of trichlorosilane OTS, response time are relevant with ambient temperature, can change above parameter as required to reduce lining
The surface energy at the end, follow-up photoetching electrode pattern and polydimethylsiloxane and electrode turn from silicon substrate
Shifting is got off；
3) photoetching electrode pattern on the substrate of modified:
(1) spin coating photoresist: we select photoresist to be AZ5214E, because the viscosity of AZ5214E photoresist
Bigger, it is possible to be spin-coated under certain condition on the substrate of octadecyl trichlorosilane alkane OTS modified and be easy to stripping
From；Spin coating photoresist condition is 4000 turns/min, and spin-coating time is 40 seconds, first repaiies at octadecyl trichlorosilane alkane OTS
Dripping full photoresist on the substrate adornd, need to wait 90s-180s spin coating again, otherwise photoresist is not gone up in spin coating；
(2) front baking: pre-bake temperature is 100 degrees Celsius, the time is 1 minute；
(3) exposure: time of exposure is 30 seconds；
(4) development: developer solution is AZ400K, dilutes with deionized water, and AZ400K with the volume ratio of deionized water is
1:4,
Developing time is 180s；
(5) fixing: the fixing 30s of deionized water；
4) evaporation metal electrode: with the golden film of coater evaporation 25nm；
5) the surface MPT(mercaptopropyl trimethoxysilane of metal electrode) modify: the sample being deposited with is carried out mercapto
Propyl trimethoxy silicane MPT modifies, in order to has between polydimethylsiloxane with gold and well links, and is beneficial to
Gold electrode shifts from silicon substrate, and optimum condition is to put into 30 μ l-40 μ l mercaptos third under 0.01MPa vacuum condition
Base trimethoxy silane MPT reacts 20 minutes；
6) stripping of photoresist: remove photoresist with N-methyl pyrrolidone, with drying platform heating N-methylpyrrole
Alkanone, temperature is 100 degrees Celsius, is put into by sample in N-methylpyrrolidone solution after temperature stabilization, waits
30 seconds, carry out spraying auxiliary with syringe and remove photoresist, then sample taking-up isopropanol from solution is rinsed, finally use nitrogen
Air-blowing is done；
7) spin coating polydimethylsiloxane and the solidification of polydimethylsiloxane:
(1) spin coating polydimethylsiloxane: polydimethylsiloxane and the volume proportion of firming agent
It is 10: 1, then both is stirred about 10 minutes, stand 1 and a half hours or can also put in vacuum
Row evacuation, it is therefore an objective to removing the bubble in polydimethylsiloxane, spincoating conditions is 2000 turns/min, time
Between be 1 minute, general 200 μm of thickness of polydimethylsiloxane PMDS, thickness can as required by rotating speed and will
Polydimethylsiloxane is diluted regulating；
(2) polydimethylsiloxane solidification: the sample that spin coating is good is put in baking oven and toast 12 hours, temperature
It it is 70 degrees Celsius.
8) electrode shifts from substrate: with double faced adhesive tape, the sample with electrode is fixed on microscope slide, with the thinnest
Blade the polydimethylsiloxane of sample edge is scratched, then by the PET of 25 μm along one end slowly
Put down, finally utilize PET with the viscosity of polydimethylsiloxane, electrode to be shifted from substrate, finally give electricity
Pole and polydimethylsiloxane are in conplane embedded electrode.
The positive effect of the present invention is that it uses existing lithography technology, convenient and practical；Can with under room temperature operate,
Organic semiconductor not by radiation, developer solution, go glue to be damaged；Its degree of accuracy is high, can make the pattern of complexity
；The electrode structure of final preparation is that electrode is in conplane embedded electrode with insulating barrier.
With the curve of output of the end contact-type CuPc single-crystal field effect transistor prepared by the embedded electrode of this plane and
Transfer curve, the channel width of device is about 4.35 μm, and channel length is about 180 μm, and mobility is about.This migrates
Rate is higher than top contact type CuPc single-crystal field effect transistor (Advanced Materials 2006,18,65-68),
Show that this transistor has excellent performance.
Accompanying drawing explanation
Fig. 1 is traditional electrode structure schematic diagram.
Fig. 2 is that organic semiconductor contacts schematic diagram with traditional electrode.
Fig. 3 is embedded electrode structure schematic diagram prepared by nano impression.
Fig. 4 is the embedded electrode structure schematic diagram that patent system of the present invention is standby.
Wherein in figure, 1 is electrode, and 2 is the substrates such as insulating barrier, glass, silicon, and 3 is organic semiconductor, and 4 are
Gold electrode, 5 is PDMS.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings, and following example are not limited to the present invention,
All within the spirit and principles in the present invention, any amendment made, equivalent and improvement etc., should be included in this
Within bright protection domain.
Embodiment 1
First with method photoetching electrode pattern on substrate 2 of photoetching, gold evaporation electrode 4, obtains pattern afterwards
The gold electrode 4 changed, then spin coating polydimethylsiloxane 5 on the substrate with gold electrode 4, through poly dimethyl
After siloxanes PDMS solidification, gold electrode 4 is shifted together with polydimethylsiloxane from substrate 2；Specifically
Step as follows: 1) cleaning of silicon substrate: silicon chip is cut into 5mm*10mm size, in being then placed in acetone ultrasonic 15
Minute, taking-up nitrogen dries up, and is then placed in baking 5min in baking oven, and temperature is 100 degrees Celsius;Put after drying
Entering chromic acid lotion to soak 20 minutes, taking-up with deionized water rinsing several times, finally dries up with nitrogen；
2) OTS of silicon substrate modifies:
(1) silicon chip surface hydroxylating: preparation Piranha washing liquid, the configuration of Piranha washing liquid is concentrated sulphuric acid and peroxidating
The volume ratio of hydrogen solution is 7:3, and then silicon chip is put into Piranha washing liquid 30min, takes out silicon chip deionized water rinsing
Several times, finally dry up with nitrogen；
(2) the silicon chip surface OTS (octadecyl trichlorosilane alkane) after hydroxylating modifies: preparation is molten with normal heptane
The 0.075%OTS solution of agent, then puts into the silicon chip after hydroxylating and wherein takes out after 14 hours；Use chloroform
Soaking 5 minutes, the most ultrasonic 10 minutes, dry up with nitrogen afterwards, put into baking oven baking 5min, temperature arrives 70
100 degrees Celsius, in order to remove the absorption chloroform at substrate surface, finally successfully modified one layer 18 at silicon face
Alkyltrichlorosilanes OTS, reduces the surface energy of substrate, follow-up polydimethylsiloxane and metal electrode
Shift from silicon substrate；
3) photoetching electrode pattern on the substrate of modified:
(1) spin coating photoresist: we select photoresist to be AZ5214E, because the viscosity of AZ5214E photoresist
Bigger, it is possible to be spin-coated under certain condition on the substrate 2 of octadecyl trichlorosilane alkane OTS modified and be easy to
Peel off.Spin coating photoresist condition is 4000 turns/min, and spin-coating time is 40 seconds, first repaiies at octadecyl trichlorosilane alkane OTS
Dripping full photoresist on the substrate 2 adornd, need to wait 90s spin coating again, otherwise photoresist is not gone up in spin coating；
(2) front baking: pre-bake temperature is 100 degrees Celsius, the time is 1 minute；
(3) exposure: time of exposure is 30 seconds；
(4) development: developer solution is AZ400K, dilutes with deionized water, AZ400K and the volume ratio of deionized water
It is 180s for 1:4 developing time；
(5) fixing: the fixing 30s of deionized water；
4) evaporation metal electrode: with the golden film of coater evaporation 25nm；
5) the surface mercaptopropyl trimethoxysilane MPT of metal electrode modifies: the sample being deposited with is carried out mercapto third
Base trimethoxy silane MPT modifies, in order to has between polydimethylsiloxane with gold and well links, and is beneficial to gold
Electrode shifts from silicon substrate, and condition is to put into 30 μ l mercapto propyl trimethoxy silicon under 0.01MPa vacuum condition
Alkane MPT reacts 20 minutes；
6) stripping of photoresist: remove photoresist with N-methyl pyrrolidone, with drying platform heating N-methylpyrrole
Alkanone, temperature is 100 degrees Celsius, is put into by sample in N-methylpyrrolidone solution after temperature stabilization, waits
30 seconds, carry out spraying auxiliary with syringe and remove photoresist, then sample taking-up isopropanol from solution is rinsed, finally use nitrogen
Air-blowing is done；7) spin coating polydimethylsiloxane and the solidification of polydimethylsiloxane: (1) spin coating poly-two
Methylsiloxane PDMS: polydimethylsiloxane is 10: 1 with the volume proportion of firming agent, then incite somebody to action both
Stir about 10 minutes, stand 1 and a half hours or can also put into vacuum carries out evacuation, it is therefore an objective to remove poly-
Bubble in dimethyl siloxane PDMS, spincoating conditions is 2000 turns/min, and the time is 1 minute, poly dimethyl
General 200 μm of thickness of siloxanes PMDS, thickness can be as required by rotating speed with by polydimethylsiloxane
It is diluted regulating；
(2) polydimethylsiloxane solidification: the sample that spin coating is good is put in baking oven and toast 12 hours, temperature
It it is 70 degrees Celsius.
8) electrode shifts from substrate: with double faced adhesive tape, the sample with electrode is fixed on microscope slide, with the thinnest
Blade the polydimethylsiloxane of sample edge is scratched, then by the polyethylene terephthalate of 25 μm
PET thin film along one end putting down slowly (note the when of patch, the most down will paste from one end, it is to avoid occur bubble and
Fold), finally utilize the polyethylene terephthalate PET viscosity with polydimethylsiloxane electrode from substrate
Transfer is got off, and finally gives electrode and is in conplane embedded electrode, structural representation with polydimethylsiloxane
Figure is such as Fig. 4.
Embodiment 2
1) cleaning of silicon substrate: the 5mm*10mm silicon chip cut is put into acetone ultrasonic 15 minutes, takes out
Drying up with nitrogen, be then placed in baking 5min in baking oven, temperature is 100 degrees Celsius;Chromic acid lotion is put into after drying
Soaking 20 minutes, taking-up with deionized water rinsing several times, finally dries up with nitrogen.
2) OTS of silicon substrate modifies:
(1) silicon chip surface hydroxylating: preparation Piranha washing liquid, the configuration of Piranha washing liquid is concentrated sulphuric acid and peroxidating
The volume ratio of hydrogen solution is 7:3, and then silicon chip is put into Piranha washing liquid 30min, takes out silicon chip deionized water rinsing
Several times, finally dry up with nitrogen.
(2) the silicon chip surface OTS(octadecyl trichlorosilane alkane after hydroxylating) to modify: preparation is molten with normal heptane
0.0875% OTS solution of agent, then puts into the silicon chip after hydroxylating and wherein takes out after 14 hours；Use chloroform
Soaking 5 minutes, the most ultrasonic 10 minutes, dry up with nitrogen afterwards, put into baking oven baking 5min, temperature is 70
To 100 degrees Celsius, in order to remove the absorption chloroform at substrate surface, finally successfully modified one layer at silicon face
OTS, reduces the surface energy of substrate, and follow-up PDMS and electrode shift from silicon substrate.
3) photoetching electrode pattern on the substrate of modified:
(1) spin coating photoresist: we select photoresist to be AZ5214E, because the viscosity of AZ5214E photoresist
Bigger, it is possible to be spin-coated under certain condition on the substrate of OTS modified and be easy to peel off.Spin coating photoresist condition
Being 4000 turns/min, spin-coating time is 40 seconds, first drips full photoresist on the substrate of OTS modified, needs to wait
120s spin coating again, otherwise photoresist is not gone up in spin coating.
(2) front baking: pre-bake temperature is 100 degrees Celsius, the time is 1 minute.
(3) exposure: time of exposure is 30 seconds.
(4) development: developer solution is AZ400K, dilutes with deionized water, AZ400K and the volume ratio of deionized water
It is 180s for 1:4 developing time.
(5) fixing: the fixing 30s of deionized water.
4) evaporation metal electrode: with the golden film of coater evaporation 25nm.
5) the surface MPT(mercaptopropyl trimethoxysilane of metal electrode) modify: the sample being deposited with is carried out
MPT modifies, in order to having between polydimethylsiloxane with gold and well link, beneficially gold electrode is from silicon substrate
Transfer is got off, and condition is to put into 35 μ l MPT under 0.01MPa vacuum condition to react 20 minutes.
6) stripping of photoresist: remove photoresist with N-methyl pyrrolidone, with drying platform heating N-methylpyrrole
Alkanone, temperature is 100 degrees Celsius, is put into by sample in N-methylpyrrolidone solution after temperature stabilization, waits 30
Second, carry out spraying auxiliary with syringe and remove photoresist, then sample taking-up isopropanol from solution is rinsed, finally use nitrogen
Dry up.
7) spin coating polydimethylsiloxane and the solidification of polydimethylsiloxane:
(1) spin coating polydimethylsiloxane: polydimethylsiloxane and the volume proportion of firming agent
It is 10: 1, then both is stirred about 10 minutes, stand 1 and a half hours or can also put in vacuum
Row evacuation, it is therefore an objective to removing the bubble in polydimethylsiloxane, spincoating conditions is 2000 turns/min, time
Between be 1 minute, general 200 μm of thickness of polydimethylsiloxane PMDS, thickness can as required by rotating speed and will
Polydimethylsiloxane is diluted regulating；
(2) polydimethylsiloxane solidification: the sample that spin coating is good is put in baking oven and toast 12 hours, temperature
It it is 70 degrees Celsius.
8) electrode shifts from substrate: with double faced adhesive tape, the sample with electrode is fixed on microscope slide, with the thinnest
Blade the polydimethylsiloxane of sample edge is scratched, then by the polyethylene terephthalate of 25 μm
PET thin film along one end putting down slowly (note the when of patch, the most down will paste from one end, it is to avoid occur bubble and
Fold), finally utilize the polyethylene terephthalate PET viscosity with polydimethylsiloxane electrode from substrate
Transfer is got off, and finally gives electrode and is in conplane embedded electricity, structural representation with polydimethylsiloxane
Such as Fig. 4.
Embodiment 3
1) cleaning of silicon substrate: the 5mm*10mm silicon chip cut is put into acetone ultrasonic 15 minutes, takes out
Dry up with nitrogen, be then placed in baking 5min in baking oven;Put into chromic acid lotion after drying to soak 20 minutes, take out and use
Deionized water rinsing several times, finally dries up with nitrogen.
2) OTS of silicon substrate modifies:
(1) silicon chip surface hydroxylating: preparation Piranha washing liquid, the configuration of Piranha washing liquid is concentrated sulphuric acid and peroxidating
Hydrogen solution
Volume ratio be 7:3, then silicon chip is put into Piranha washing liquid 30min, takes out silicon chip deionized water and rush
Wash several times, finally dry up with nitrogen.
(2) the silicon chip surface OTS(octadecyl trichlorosilane alkane after hydroxylating) to modify: preparation is molten with normal heptane
0.1% OTS solution of agent, then puts into the silicon chip after hydroxylating and wherein takes out after 14 hours；Soak with chloroform
5 minutes, the most ultrasonic 10 minutes, drying up with nitrogen afterwards, put into baking oven baking 5min, temperature is 70 to 100
Degree Celsius, in order to remove the absorption chloroform at substrate surface, finally successfully modify one layer of OTS at silicon face,
Reducing the surface energy of substrate, follow-up PDMS and electrode shift from silicon substrate.
3) photoetching electrode pattern on the substrate of modified:
(1) spin coating photoresist: we select photoresist to be AZ5214E, because the viscosity of AZ5214E photoresist
Bigger, it is possible to be spin-coated under certain condition on the substrate of OTS modified and be easy to peel off.Spin coating photoresist condition
Being 4000 turns/min, spin-coating time is 40 seconds, first drips full photoresist on the substrate of OTS modified, needs
Treating more than 180s spin coating again, otherwise photoresist is not gone up in spin coating.
(2) front baking: pre-bake temperature is 100 degrees Celsius, the time is 1 minute.
(3) exposure: time of exposure is 30 seconds.
4) development: developer solution is AZ400K, dilutes with deionized water, AZ400K and the volume ratio of deionized water
For 1:4, developing time is 180s.
5) fixing: the fixing 30s of deionized water.
4) evaporation metal electrode: with the golden film of coater evaporation 25nm.
5) the surface MPT(mercaptopropyl trimethoxysilane of metal electrode) modify: the sample being deposited with is carried out
MPT modify, in order to have between polydimethylsiloxane with gold and well link, beneficially gold electrode from
Shifting on silicon substrate, condition is to put into 40 μ l MPT under 0.01MPa vacuum condition to react 20 minutes.
6) stripping of photoresist: remove photoresist with N-methyl pyrrolidone, with drying platform heating N-methylpyrrole
Alkanone, temperature is 100 degrees Celsius, is put into by sample in N-methylpyrrolidone solution after temperature stabilization, waits 30
Second, carry out spraying auxiliary with syringe and remove photoresist, then sample taking-up isopropanol from solution is rinsed, finally use nitrogen
Dry up.
7) spin coating polydimethylsiloxane and the solidification of polydimethylsiloxane:
(1) spin coating polydimethylsiloxane: polydimethylsiloxane and the volume proportion of firming agent
It is 10: 1, then both is stirred about 10 minutes, stand 1 and a half hours or can also put in vacuum
Row evacuation, it is therefore an objective to removing the bubble in polydimethylsiloxane, spincoating conditions is 2000 turns/min, time
Between be 1 minute, general 200 μm of thickness of polydimethylsiloxane PMDS, thickness can as required by rotating speed and will
Polydimethylsiloxane is diluted regulating；
(2) polydimethylsiloxane solidification: the sample that spin coating is good is put in baking oven and toast 12 hours, temperature
It it is 70 degrees Celsius.
8) electrode shifts from substrate: with double faced adhesive tape, the sample with electrode is fixed on microscope slide, with the thinnest
Blade the polydimethylsiloxane of sample edge is scratched, then by the polyethylene terephthalate of 25 μm
PET thin film along one end putting down slowly (note the when of patch, the most down will paste from one end, it is to avoid occur bubble and
Fold), finally utilize the polyethylene terephthalate PET viscosity with polydimethylsiloxane electrode from substrate
Transfer is got off, and finally gives electrode and is in conplane embedded electricity, structural representation with polydimethylsiloxane
Such as Fig. 4.
Claims (1)
1. the preparation method of the embedded electrode of plane, it is characterised in that: utilize method photoetching electrode figure on substrate of photoetching
Case, afterwards evaporation metal electrode, obtain the metal electrode of patterning, then spin coating poly dimethyl silicon on the substrate with electrode
Oxygen alkane PDMS, through polydimethylsiloxane solidify after, by electrode together with polydimethylsiloxane from substrate
Transfer is got off；Concrete step is as follows:
1) cleaning of silicon substrate: the 5mm*10mm silicon chip cut is put into acetone ultrasonic 15 minutes, and taking-up nitrogen dries up, so
After put into baking oven baking 5min, temperature is 100 degrees Celsius;Putting into chromic acid lotion after drying to soak 20 minutes, taking-up spends
Ionized water rinses several times, finally dries up with nitrogen；
2) OTS of silicon substrate modifies:
(1) silicon chip surface hydroxylating: preparation Piranha washing liquid, the configuration of Piranha washing liquid is concentrated sulphuric acid and hydrogenperoxide steam generator
Volume ratio is 7:3, and then silicon chip is put into Piranha washing liquid 30min, takes out silicon chip with deionized water rinsing several times, finally uses nitrogen
Air-blowing is done；
(2) the silicon chip surface octadecyl trichlorosilane alkane OTS after hydroxylating modifies: the preparation OTS solution with normal heptane as solvent,
Optium concentration is 0.075% 0.1%, is then put into by the silicon chip after hydroxylating and wherein takes out after 14 hours；Use chloroform
Soaking 5 minutes, the most ultrasonic 10 minutes, dry up with nitrogen afterwards, put into baking oven baking 5min, temperature is Celsius 70 to 100
Degree, in order to remove the absorption chloroform at substrate surface, finally successfully modified one layer of OTS at silicon face, reduced lining
The surface at the end can, and this modify rear surface can size directly and the concentration of octadecyl trichlorosilane alkane OTS, the response time and
Ambient temperature is relevant, and follow-up photoetching electrode pattern and polydimethylsiloxane and electrode shift from silicon substrate
Get off；
3) photoetching electrode pattern on the substrate of modified:
(1) spin coating photoresist: we select photoresist to be AZ5214E, because the ratio of viscosities of AZ5214E photoresist is bigger, it is possible to
It is spin-coated under certain condition on the substrate of octadecyl trichlorosilane alkane OTS modified and is easy to peel off；Spin coating photoresist
Condition is 4000 turns/min, and spin-coating time is 40 seconds, first drips full light on the substrate of octadecyl trichlorosilane alkane OTS modified
Photoresist, needs to wait 90s-180s spin coating again, otherwise photoresist is not gone up in spin coating；
(2) front baking: pre-bake temperature is 100 degrees Celsius, the time is 1 minute；
(3) exposure: time of exposure is 30 seconds；
(4) development: developer solution is AZ400K, dilutes with deionized water, and AZ400K is 1:4 with the volume ratio of deionized water, development
Time is 180s；
(5) fixing: the fixing 30s of deionized water；
4) evaporation metal electrode: with the golden film of coater evaporation 25nm；
5) the surface mercaptopropyl trimethoxysilane MPT of metal electrode modifies: the sample being deposited with is carried out mercapto propyl group trimethoxy
Base silane MPT modifies, in order to having between polydimethylsiloxane with gold and well link, beneficially gold electrode is from silicon substrate
Transfer is got off, and optimum condition is to put into 30 μ l-40 μ l mercaptopropyl trimethoxysilane MPT reactions under 0.01MPa vacuum condition
20 minutes；
6) stripping of photoresist: remove photoresist with N-Methyl pyrrolidone, with drying platform heating N-Methyl pyrrolidone, temperature is
100 degrees Celsius, sample is put in N-Methyl pyrrolidone solution after temperature stabilization, wait 30 seconds, spray with syringe
Penetrate auxiliary to remove photoresist, then sample taking-up isopropanol from solution is rinsed, finally dry up with nitrogen；
7) spin coating polydimethylsiloxane and the solidification of polydimethylsiloxane:
(1) spin coating polydimethylsiloxane: polydimethylsiloxane is 10:1 with the volume proportion of firming agent, then
Both are stirred about 10 minutes, stand 1 and a half hours or put into vacuum carries out evacuation, it is therefore an objective to remove poly dimethyl
Bubble in siloxanes PDMS, spincoating conditions is 2000 turns/min, and the time is 1 minute, the thickness of polydimethylsiloxane
It is 200 μm；
(2) polydimethylsiloxane solidification: put into by the sample that spin coating is good in baking oven and toast 12 hours, temperature is 70 Celsius
Degree；
8) electrode shifts from substrate: with double faced adhesive tape, the sample with electrode is fixed on microscope slide, will with the thinnest blade
The polydimethylsiloxane of sample edge is scratched, then by the polyethylene terephthalate PET film of 25 μm along one
End putting down slowly, finally utilize the viscosity of polyethylene terephthalate PET and polydimethylsiloxane electrode from
Shift on substrate, finally give electrode and be in conplane embedded electrode with polydimethylsiloxane.
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| CN101449405A (en) * | 2006-05-18 | 2009-06-03 | 巴斯夫欧洲公司 | Patterning nanowires on surfaces for fabricating nanoscale electronic devices |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101449405A (en) * | 2006-05-18 | 2009-06-03 | 巴斯夫欧洲公司 | Patterning nanowires on surfaces for fabricating nanoscale electronic devices |
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| Title |
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| 《Metal Electrodes in Plastinc Microfluidic Systems》;Walter Scott, et al.;《Microelectronic Engineering》;20090118;第86卷;1340-1342 * |
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