CN105974730A - Preparation method of SU8 array micro-reaction pool - Google Patents

Preparation method of SU8 array micro-reaction pool Download PDF

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Publication number
CN105974730A
CN105974730A CN201610432048.9A CN201610432048A CN105974730A CN 105974730 A CN105974730 A CN 105974730A CN 201610432048 A CN201610432048 A CN 201610432048A CN 105974730 A CN105974730 A CN 105974730A
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CN
China
Prior art keywords
film
array
fibre faceplate
preparation
reaction pool
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Pending
Application number
CN201610432048.9A
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Chinese (zh)
Inventor
陈哲
张睿
王者馥
王绪敏
殷金龙
任鲁风
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Beijing Zhongkezixin Technology Co Ltd
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Beijing Zhongkezixin Technology Co Ltd
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Filing date
Publication date
Priority claimed from CN201510521775.8A external-priority patent/CN105045050A/en
Priority claimed from CN201510521819.7A external-priority patent/CN105204290A/en
Application filed by Beijing Zhongkezixin Technology Co Ltd filed Critical Beijing Zhongkezixin Technology Co Ltd
Publication of CN105974730A publication Critical patent/CN105974730A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03FPHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/0035Multiple processes, e.g. applying a further resist layer on an already in a previously step, processed pattern or textured surface

Abstract

The invention relates to a preparation method of an SU8 array micro-reaction pool. The preparation method of the SU8 array micro-reaction pool is characterized by comprising a coating step, a pre-baking step, an exposure step, a post-baking step, a cooling step, a developing step, a film strengthening step and a film coating step, wherein the film coating step is coating the wall of the SU8 array micro-reaction pool with a 30-90nm of reflecting thin film. Compared with the prior art, the preparation method has the advantages that the prepared SU8 micro-reaction pool has good optical crosstalk resistance through adding the film coating step, so that the prepared SU8 micro-reaction pool can be better applied to sequencing-based applications with relatively high requirements on the optical property of the SU8 micro-reaction pool.

Description

A kind of preparation method of SU8 array micro reaction pool
Technical field
The present invention relates to microelectronic processing technique field, particularly relate to the preparation side of a kind of SU8 array micro reaction pool Method.
Background technology
Fibre faceplate surface makes array micro reaction pool three kinds of alternate ways: one be fibre faceplate superficial growth without Machine thin-film material, and use semiconductor microactuator processing technique to produce array micro reaction pool;Two is to have array to decline anti-making Pond thin-film material is answered to be bonded with fibre faceplate;Three is to use thick resist lithography technique to make polymer array formula on fibre faceplate surface Micro reaction pool.Thick resist lithography is simple for process and cost of manufacture is low, becomes the first-selected approach that array micro reaction pool makes.
Photoresist also known as photoresist, by photosensitive resin, sensitizer and three kinds of main components of solvent form to photosensitive The mixing liquid of sense.The technical sophistication of photoresist, kind is more.According to its chemical reaction mechanism and development principle, negativity can be divided Glue and positive photoresist two class.Form insoluble material after illumination is negative photoresist;Otherwise, it is insoluble to some solvent, through light Become soluble substance after according to is positive photoresist.Utilize this performance, by photoresist making coatings, just can etch institute at silicon chip surface The circuitous pattern needed.
Photoresist should have smaller surface tension, makes photoresist have good mobility and covering.SU8 material It is the negative epoxy photoresist developed by IBM Corporation nineteen ninety-five, there is the highest ultraviolet light sensitive characteristic, making plasticity machine The MEMS aspects such as tool structure, microfluidic device, MCA obtain a wide range of applications, and are a kind of more conventional thick glue. SU8 is the organic polymer colloid being dissolved in gamma-butyrolacton by bisphenol A type epoxy resin and being formed, because containing in an average molecule 8 epoxy resin are had to gain the name.Jiao's SU8 phosphorus process is broadly divided into two steps: the light trigger in (1) SU8 absorbs photon, and chemistry occurs Reaction generates acidic catalyst;(2) acidic catalyst epoxy reaction, formation cause between catalytic molecular under the assosting effect of heat energy Close cross-linked network.Relative to other thick glue, SU8 processing technique is simple, and reproducible, bio-compatibility is good, easily silicon, glass, Potteries etc. form array structure on substrate, and SU8 includes the epoxy radicals enriched, and the active response type of chemical property is strong, can be in temperature React with multiple group generation nucleophilic ring opening with under price modification, can under conditions of not affecting biological activity with various biomolecules altogether Valency combines, it is possible to effective increase functional group efficiency.Traditional chip material exposition uniformity is poor, and the exposition uniformity of SU8 is good, High aspect ratio structure can be made, it is possible to form super hydrophobic surface by chemical modification, reduce the frictional force during using, increase Its abrasion durability strong, has good mechanical performance, relatively low Young's modulus and preferable metal level adhesiveness.These character SU8 is made to become the splendid selection making micro reaction pool in many photoresists being applied to thick resist lithography technique.
But SU8 is up to 90% in visible light wave range absorbance, SU8 array micro reaction pool is caused to be optically isolated poor performance, The adjacent mutual crosstalk of the optical signalling between micro reaction pool, reduces the noise when accuracy of optical detection.Additionally, SU8 The problems such as the glue limit of manufacturing process and stress greatly have impact on its process repeatability and yield rate.
Summary of the invention
In order to solve optical signal crosstalk that existing SU8 micro reaction pool preparation method is prevented effectively between adjacent micro reaction pool Problem, it is an object of the invention to provide the preparation method of a kind of SU8 array micro reaction pool, it is characterised in that include following step Rapid:
(1) spin coating: SU8 drops to fibre faceplate center, spin fiber panel is until SU8 forms thick layer on fibre faceplate Spend uniform coating;
(2) front baking: the fibre faceplate that fine jade scribbles SU8 coating is placed in the environment of dry heat, makes SU8 layer film forming;
(3) exposure: employing ultraviolet light will be covered with the SU8 film exposure of the mask of array pattern;
(4) after bake: after bake in the environment of the fibre faceplate dry heat of SU8 film after overlying is exposed;
(5) cooling: the fibre faceplate of the SU8 film processed by overlying after bake is put into and made SU8 film and fibre faceplate fall in helium cabinet To room temperature;
(6) development: use developing agent to make the SU8 film development on fibre faceplate, form array reaction tank;
(7) hard mould: the SU8 array reaction tank formed and fibre faceplate are put into and carries out hard mould, oven temperature in baking oven It is 80 DEG C, continues 1-1.5h;
(8) plated film: SU8 array reaction tank pool wall is plated the reflective film of 30-90nm.
Further, the one during the material of reflectance coating described in plating steps is gold, silver, aluminum, copper.Passed by photon energy Pass relation, under conditions of conservative control optical absorption, the transmission of light can be reduced by increasing the reflectance on surface.Reflectance coating Can be effectively increased surface reflectivity, and application conditions mature and reliable, conventional reflectance coating has metallic reflective coating and full electrolyte anti- Penetrate film two class.Full electrolyte reflectance coating generally has high reflectance and absorbance relatively low at specific wavelength, but be difficult to whole can High reflectance is kept in seeing optical range.The operating wavelength range width of metallic reflective coating, and preparation technology is the simplest.Wherein, Gold, silver, aluminum, copper these four metal have good reflectance, and their plating conditions is also looser than other metals.
Further, the material of reflectance coating described in plating steps is aluminum.Compared to other metals above-mentioned, aluminum is near ultraviolet Light, visible ray and near infrared light will be good reflecting rate, aluminum also can thickness less than 100nm time also keep preferably reflecting Rate.
Further, described reflectance coating thickness is 40-55nm.Irradiate the pass of the penetration depth of light and the fundamental property of material It is as follows: δ=[λ/(π c μ σ)] ^ (1/2), wherein δ is the penetration depth of light, and λ is the wavelength of light, and c is the light velocity, and μ is leading of material Magnetic coefficient, σ is quiet electrical conductivity.Being understood by this formula, the wavelength of light is the longest more penetrates readily through irradiated material;And The electrical conductivity of material is the highest, and the penetration depth irradiating light is the most shallow, thus the reflectance that materials control penetrates light is the highest.Skill of the present invention Art personnel combine this formula and substantial amounts of test draws, reflectance coating thickness not only can reach the biggest when 40-55nm Reflectance, also the structure of micro reaction pool and performance will not be produced significantly impact.
Further, the plated film mode of described reflective film is evaporation.Plated film typically has three kinds of modes: evaporation (evaporation), sputter (sputtering) and ion coating (ion plating).Owing to the present invention program is intended to instead Penetrate film plating be only plated on reaction tank pool wall, plating steps the most of the present invention should select one can to the plated film scope control of target relatively Good plated film mode.In evaporation mode, technical staff can by adjust the factor such as orientation substrate, evaporation rate can be preferable Ground controls the plated film scope of target.Meanwhile, the metal that other modes of luminance factor making genus reflectance coating that evaporation is formed are formed is anti- The reflectance penetrating film wants height.It addition, the cost of metal evaporation is cheaper than other two ways, beneficially the present invention program exists Application in actual industrial production.
Further, described evaporation is 10-6-10-8The vacuum of Pa completes.Under this condition, the metal formed The density of reflectance coating is relatively big, thus its reflectance is the highest.
Further, in plating steps, the temperature of SU8 array reaction tank and fibre faceplate is 60-70 DEG C.This Condition advantageously forms the metallic reflective coating that density is bigger, so that the reflectance of the reflectance coating formed is bigger.
Compared with prior art, it is an advantage of the invention that the step by adding plated film, make the SU8 micro reaction pool prepared There is good anti-optical crosstalk ability, it is thus possible to be preferably applied for based on order-checking etc., SU8 micro reaction pool optical property being wanted Ask in higher application.
Detailed description of the invention
Embodiments of the invention are described below in detail, are only used for explaining the present invention, and limitation of the present invention can not be considered as.
For reducing the variable of test, the degree of depth of following SU8 reaction tank, the SU8 film that preparation method the most of the present invention is initially formed Thickness, be 30 μm, the pool wall thickness between reaction tank is 6 μm, reaction tank cross section be 30 μ m 30 μm square, reaction tank battle array It is classified as 10 × 10 quadrate arrays.
But, those skilled in the art, it is known that reaction tank array can be arranged by more reasonably geometry, make anti- Answering pond to arrange tightr, the size and dimension of reaction tank itself can also do other and adjust according to concrete applied environment.
Embodiment 1
(1) spin coating: SU8 drops to fibre faceplate center, spin fiber panel is until SU8 forms thick layer on fibre faceplate Spend uniform coating;
(2) front baking: the fibre faceplate that fine jade scribbles SU8 coating is placed in the environment of dry heat, makes SU8 layer film forming;
(3) exposure: employing ultraviolet light will be covered with the SU8 film exposure of the mask of array pattern;
(4) after bake: after bake in the environment of the fibre faceplate dry heat of SU8 film after overlying is exposed;
(5) cooling: the fibre faceplate of the SU8 film processed by overlying after bake is put into and made SU8 film and fibre faceplate fall in helium cabinet To room temperature;
(6) development: use developing agent to make the SU8 film development on fibre faceplate, form array reaction tank;
(7) hard mould: the SU8 array reaction tank formed and fibre faceplate are put into and carries out hard mould, oven temperature in baking oven It is 80 DEG C, continues 1-1.5h;
(8) plated film: the method that SU8 array reaction tank pool wall is deposited with is plated the aluminum reflective film of 40 nm, is wherein deposited with gas Pressure is 6.7*10-7The temperature of Pa, SU8 array reaction tank and fibre faceplate is 60 DEG C.
Embodiment 2
(1) spin coating: SU8 drops to fibre faceplate center, spin fiber panel is until SU8 forms thick layer on fibre faceplate Spend uniform coating;
(2) front baking: the fibre faceplate that fine jade scribbles SU8 coating is placed in the environment of dry heat, makes SU8 layer film forming;
(3) exposure: employing ultraviolet light will be covered with the SU8 film exposure of the mask of array pattern;
(4) after bake: after bake in the environment of the fibre faceplate dry heat of SU8 film after overlying is exposed;
(5) cooling: the fibre faceplate of the SU8 film processed by overlying after bake is put into and made SU8 film and fibre faceplate fall in helium cabinet To room temperature;
(6) development: use developing agent to make the SU8 film development on fibre faceplate, form array reaction tank;
(7) hard mould: the SU8 array reaction tank formed and fibre faceplate are put into and carries out hard mould, oven temperature in baking oven It is 80 DEG C, continues 1-1.5h;
(8) plated film: the method that SU8 array reaction tank pool wall is deposited with is plated the golden reflective film of 30nm, is wherein deposited with gas Pressure is 9*10-7The temperature of Pa, SU8 array reaction tank and fibre faceplate is 65 DEG C.
Embodiment 3
(1) spin coating: SU8 drops to fibre faceplate center, spin fiber panel is until SU8 forms thick layer on fibre faceplate Spend uniform coating;
(2) front baking: the fibre faceplate that fine jade scribbles SU8 coating is placed in the environment of dry heat, makes SU8 layer film forming;
(3) exposure: employing ultraviolet light will be covered with the SU8 film exposure of the mask of array pattern;
(4) after bake: after bake in the environment of the fibre faceplate dry heat of SU8 film after overlying is exposed;
(5) cooling: the fibre faceplate of the SU8 film processed by overlying after bake is put into and made SU8 film and fibre faceplate fall in helium cabinet To room temperature;
(6) development: use developing agent to make the SU8 film development on fibre faceplate, form array reaction tank;
(7) hard mould: the SU8 array reaction tank formed and fibre faceplate are put into and carries out hard mould, oven temperature in baking oven It is 80 DEG C, continues 1-1.5h;
(8) plated film: the method that SU8 array reaction tank pool wall is deposited with is plated the aluminum reflective film of 55nm, is wherein deposited with gas Pressure is 5*10-6The temperature of Pa, SU8 array reaction tank and fibre faceplate is 70 DEG C.
Embodiment 4
(1) spin coating: SU8 drops to fibre faceplate center, spin fiber panel is until SU8 forms thick layer on fibre faceplate Spend uniform coating;
(2) front baking: the fibre faceplate that fine jade scribbles SU8 coating is placed in the environment of dry heat, makes SU8 layer film forming;
(3) exposure: employing ultraviolet light will be covered with the SU8 film exposure of the mask of array pattern;
(4) after bake: after bake in the environment of the fibre faceplate dry heat of SU8 film after overlying is exposed;
(5) cooling: the fibre faceplate of the SU8 film processed by overlying after bake is put into and made SU8 film and fibre faceplate fall in helium cabinet To room temperature;
(6) development: use developing agent to make the SU8 film development on fibre faceplate, form array reaction tank;
(7) hard mould: the SU8 array reaction tank formed and fibre faceplate are put into and carries out hard mould, oven temperature in baking oven It is 80 DEG C, continues 1-1.5h;
(8) plated film: the method that SU8 array reaction tank pool wall is deposited with is plated the silver-colored reflective film of 85nm, is wherein deposited with gas Pressure is 3.5*10-6The temperature of Pa, SU8 array reaction tank and fibre faceplate is 70 DEG C.
Comparative example 1
(1) spin coating: SU8 drops to fibre faceplate center, spin fiber panel is until SU8 forms thick layer on fibre faceplate Spend uniform coating;
(2) front baking: the fibre faceplate that fine jade scribbles SU8 coating is placed in the environment of dry heat, makes SU8 layer film forming;
(3) exposure: employing ultraviolet light will be covered with the SU8 film exposure of the mask of array pattern;
(4) after bake: after bake in the environment of the fibre faceplate dry heat of SU8 film after overlying is exposed;
(5) cooling: the fibre faceplate of the SU8 film processed by overlying after bake is put into and made SU8 film and fibre faceplate fall in helium cabinet To room temperature;
(6) development: use developing agent to make the SU8 film development on fibre faceplate, form array reaction tank;
(7) hard mould: the SU8 array reaction tank formed and fibre faceplate are put into and carries out hard mould, oven temperature in baking oven It is 80 DEG C, continues 1-1.5h.
Coated for Cy3 fluorescent marker polystyrene microsphere is filled into by the various embodiments described above by centrifugal action and The SU8 array micro reaction pool that comparative example scheme is prepared, detects fluorescence signal from its back side.Wherein, according to above-mentioned each enforcement Example and comparative example scheme prepare 9 array reaction tanks respectively, and each array reaction tank repeats at least 30 fluorescence letters Number detection, average reflecting rate and the average optical crosstalk rate of these array reaction tanks are listed in the following table.
Can be apparent from from upper table, the SU8 micro reaction pool with metallic reflection has good anti-optical crosstalk energy Power, the reflecting rate of metallic reflective coating has an impact by Coating Materials, coating film thickness and plating conditions, thus further to micro-reaction The optical crosstalk rate in pond has an impact.
Above-mentioned detailed description is illustrating for one of them possible embodiments of the present invention, and this embodiment is also not used to Limiting the scope of the claims of the present invention, all equivalences done without departing from the present invention are implemented or change, are intended to be limited solely by the technology of the present invention In the range of scheme.

Claims (7)

1. the preparation method of a SU8 array micro reaction pool, it is characterised in that comprise the following steps:
(1) spin coating: SU8 drops to fibre faceplate center, spin fiber panel is until SU8 forms thick layer on fibre faceplate Spend uniform coating;
(2) front baking: the fibre faceplate that fine jade scribbles SU8 coating is placed in the environment of dry heat, makes SU8 layer film forming;
(3) exposure: employing ultraviolet light will be covered with the SU8 film exposure of the mask of array pattern;
(4) after bake: after bake in the environment of the fibre faceplate dry heat of SU8 film after overlying is exposed;
(5) cooling: the fibre faceplate of the SU8 film processed by overlying after bake is put into and made SU8 film and fibre faceplate fall in helium cabinet To room temperature;
(6) development: use developing agent to make the SU8 film development on fibre faceplate, form array reaction tank;
(7) hard mould: the SU8 array reaction tank formed and fibre faceplate are put into and carries out hard mould, oven temperature in baking oven It is 80 DEG C, continues 1-1.5h;
(8) plated film: SU8 array reaction tank pool wall is plated the reflective film of 30-90nm.
2. the preparation method of SU8 array micro reaction pool as claimed in claim 1, it is characterised in that anti-described in plating steps The material penetrating film is the one in gold, silver, aluminum, copper.
3. the preparation method of SU8 array micro reaction pool as claimed in claim 2, it is characterised in that anti-described in plating steps The material penetrating film is aluminum.
4. the preparation method of the SU8 array micro reaction pool as described in any one of claim 3, it is characterised in that described reflection Film thickness is 40-55nm.
5. the preparation method of the SU8 array micro reaction pool as described in any one of claim 1-4, it is characterised in that described The plated film mode of reflective film is evaporation.
6. the preparation method of SU8 array micro reaction pool as claimed in claim 5, it is characterised in that described evaporation is 10-6-10-8The vacuum of Pa completes.
7. the preparation method of the SU8 array micro reaction pool as described in any one of claim 1-5, it is characterised in that in plating In film step, the temperature of SU8 array reaction tank and fibre faceplate is 60-70 DEG C.
CN201610432048.9A 2015-08-24 2016-06-17 Preparation method of SU8 array micro-reaction pool Pending CN105974730A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN2015105218197 2015-08-24
CN201510521775.8A CN105045050A (en) 2015-08-24 2015-08-24 Fabrication process for photoresist die
CN201510521819.7A CN105204290A (en) 2015-08-24 2015-08-24 Preparation method of SU8 array type micro-reaction cell
CN2015105217758 2015-08-24

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110218628A (en) * 2019-06-19 2019-09-10 中国科学院半导体研究所 A kind of digital pcr chip and preparation method thereof

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CN101398377A (en) * 2007-09-25 2009-04-01 北京大学 Polymer SPR chip and method for making same
CN102129971A (en) * 2010-12-24 2011-07-20 长治虹源科技晶体有限公司 Method and system for etching graphical sapphire substrate
CN102192988A (en) * 2010-03-05 2011-09-21 北京同方光盘股份有限公司 Substrate mould for microfluidic chip and manufacturing method thereof
CN105045050A (en) * 2015-08-24 2015-11-11 北京中科紫鑫科技有限责任公司 Fabrication process for photoresist die
CN105204290A (en) * 2015-08-24 2015-12-30 北京中科紫鑫科技有限责任公司 Preparation method of SU8 array type micro-reaction cell

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6473237B2 (en) * 2000-11-14 2002-10-29 Ball Semiconductor, Inc. Point array maskless lithography
CN101025460A (en) * 2006-02-22 2007-08-29 中国科学院长春光学精密机械与物理研究所 Micro optical component positioning structure and micro channel module preparation using micro channel array
CN101398377A (en) * 2007-09-25 2009-04-01 北京大学 Polymer SPR chip and method for making same
CN102192988A (en) * 2010-03-05 2011-09-21 北京同方光盘股份有限公司 Substrate mould for microfluidic chip and manufacturing method thereof
CN102129971A (en) * 2010-12-24 2011-07-20 长治虹源科技晶体有限公司 Method and system for etching graphical sapphire substrate
CN105045050A (en) * 2015-08-24 2015-11-11 北京中科紫鑫科技有限责任公司 Fabrication process for photoresist die
CN105204290A (en) * 2015-08-24 2015-12-30 北京中科紫鑫科技有限责任公司 Preparation method of SU8 array type micro-reaction cell

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110218628A (en) * 2019-06-19 2019-09-10 中国科学院半导体研究所 A kind of digital pcr chip and preparation method thereof

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Application publication date: 20160928