CN113213419B - Microarray structure patterning process - Google Patents
Microarray structure patterning process Download PDFInfo
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- CN113213419B CN113213419B CN202010682176.5A CN202010682176A CN113213419B CN 113213419 B CN113213419 B CN 113213419B CN 202010682176 A CN202010682176 A CN 202010682176A CN 113213419 B CN113213419 B CN 113213419B
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- 238000002493 microarray Methods 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000000059 patterning Methods 0.000 title claims abstract description 20
- 239000011325 microbead Substances 0.000 claims abstract description 135
- 239000000758 substrate Substances 0.000 claims abstract description 109
- 229920005989 resin Polymers 0.000 claims abstract description 78
- 239000011347 resin Substances 0.000 claims abstract description 78
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims description 58
- 239000007788 liquid Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 230000001276 controlling effect Effects 0.000 claims description 16
- 238000001704 evaporation Methods 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 12
- 229920001187 thermosetting polymer Polymers 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 5
- -1 alkyl mercaptan Chemical compound 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 125000000532 dioxanyl group Chemical group 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000002344 surface layer Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- NJSVDVPGINTNGX-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethanamine Chemical compound CCC[Si](OC)(OC)OCN NJSVDVPGINTNGX-UHFFFAOYSA-N 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims 1
- 239000011324 bead Substances 0.000 description 20
- 238000000016 photochemical curing Methods 0.000 description 18
- 238000009833 condensation Methods 0.000 description 15
- 230000005494 condensation Effects 0.000 description 15
- 239000004065 semiconductor Substances 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 230000003746 surface roughness Effects 0.000 description 6
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 238000005057 refrigeration Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000012806 monitoring device Methods 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005459 micromachining Methods 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- BNCADMBVWNPPIZ-UHFFFAOYSA-N 2-n,2-n,4-n,4-n,6-n,6-n-hexakis(methoxymethyl)-1,3,5-triazine-2,4,6-triamine Chemical compound COCN(COC)C1=NC(N(COC)COC)=NC(N(COC)COC)=N1 BNCADMBVWNPPIZ-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- QJAOYSPHSNGHNC-UHFFFAOYSA-N octadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCS QJAOYSPHSNGHNC-UHFFFAOYSA-N 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00214—Processes for the simultaneaous manufacturing of a network or an array of similar microstructural devices
Abstract
The invention provides a microarray structure patterning process, which comprises the following steps of firstly, obtaining a gaseous medium; step two, introducing a gaseous medium into a condensing environment in which the substrate is placed, controlling the temperature and the pressure of the condensing environment, and controlling the temperature of the substrate to condense the gaseous medium on the surface of the substrate to form microbeads; thirdly, adjusting the pressure, temperature and humidity of the condensing environment so as to control the size of the microbeads, thereby forming microbeads with the required size; step four, cooling and solidifying the condensed microbeads to prepare solid microbeads, and obtaining a microarray of the solid microbeads on a substrate; injecting resin into the surface of the substrate with the microarray to enable the resin to be attached to the surface of the solid-state microbeads, and curing the resin after the resin covers the microarray on the surface of the substrate and is leveled to form a stable structure; and step six, removing the medium on the stable structure to obtain the patterned microarray structure. The invention has the advantages of simple process, low cost and the like.
Description
Technical Field
The invention relates to the technical field of micromachining, in particular to a micromachining process.
Background
To make array patterns, particularly on the micrometer scale, photolithographic methods are generally employed. Although photolithography can produce various array patterns with uniform sizes, it requires a set of special equipment and instruments, which are costly, and the fabrication process of the array patterns using the equipment and instruments is complicated and lengthy, time-consuming and costly; and the photoetching needs to prepare a template, the pattern of the template is usually obtained by repeated process shrinkage, and the process is complex.
Therefore, the method for manufacturing the array pattern of the micrometer scale disclosed in the prior art has the problems of complicated manufacturing process, long time, high cost and the like.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of complex manufacturing procedures, long time and high cost of the process for manufacturing the array pattern at the micron level disclosed in the prior art, thereby providing a process for patterning the microarray structure, which has the advantages of simple procedures, short time and low cost.
A process for patterning a microarray structure, comprising:
step one, obtaining a gaseous medium;
step two, introducing a gaseous medium into a condensing environment in which the substrate is placed, controlling the temperature and the pressure of the condensing environment, and controlling the temperature of the substrate to condense the gaseous medium on the surface of the substrate to form microbeads;
thirdly, adjusting the pressure, temperature and humidity of the condensing environment so as to control the size of the microbeads, thereby forming microbeads with the required size;
step four, cooling and solidifying the condensed microbeads to prepare solid microbeads, and obtaining a microarray of the solid microbeads on a substrate;
injecting resin into the surface of the substrate with the microarray to enable the resin to be attached to the surface of the solid-state microbeads, and curing the resin after the resin covers the microarray on the surface of the substrate and is leveled to form a stable structure;
and step six, removing the medium on the stable structure to obtain the patterned microarray structure.
The temperature of the gaseous medium obtained in the step one is 290K-410K, and the pressure is 100kPa-200kPa; the temperature of the condensing environment in the second step is 280K-370K, the pressure is 90-150kPa, the temperature of the substrate is controlled to be 220K-360K, and the humidity of the condensing environment is 20% -80%.
The medium used in the present invention may be any inert medium which is nonflammable and has good thermal stability, and is preferably a liquid medium having a low boiling point and being easily evaporated, and the medium having good thermal stability is preferably water, silicone oil or dioxane, which does not undergo thermal decomposition within a designed operating temperature range.
The medium is preferably water or dioxane;
when the medium is water, the temperature of the gaseous medium is 290K-400K, the temperature of the condensing environment is 280K-360K, and the temperature of the substrate is 220K-350K;
when the medium is dioxane, the temperature of the gaseous medium is 300K-410K, the temperature of the condensing environment is 290K-370K, and the temperature of the substrate is 230K-360K.
The resin is a photo-curing resin or a thermosetting resin; all types of photo-setting resins or thermosetting resins disclosed in the prior art can be applied to the present invention. For ease of handling, the viscosity of the resin is preferably 5 to 150000mpa.s, as long as no bubbles in the resin are ensured and the microbeads can be leveled and covered when the resin is injected onto the substrate. The resin can be directly added to the surface of the substrate or can be sprayed on the surface of the substrate. For a resin with high viscosity, spraying to the surface of the substrate can be preferably used for achieving the purpose of adhering to the surface structure of the substrate.
When the thermosetting resin is adopted in the invention, the thickness of the thermosetting resin is controlled within 10mm, then one surface is cooled to ensure the solid structure of the microbeads, and the other surface is heated and cured, so that the molding of the microarray structure on the resin can be effectively realized in a short time.
The contact angle of the microbeads on the substrate is preferably set to be 30-150 degrees, and when the contact angle between the microbeads and the substrate is higher than 150 degrees or lower than 30 degrees, the array structure can be obtained, but the shape of the obtained array structure is irregular, so that the contact angle which the microbeads can form on the substrate in the invention is preferably set to be 30-150 degrees, and the acquisition of the contact angle can be controlled by the material of the surface of the substrate. Such as: substrate materials capable of forming contact angles with the medium within a corresponding range are directly adopted, for example: the substrate is preferably made of silicon, silicon dioxide, mica, glass or graphite, and the like, so long as the surface roughness of the substrate prepared from the adopted material is ensured to be smaller than the size of the microsphere, and the surface smoothness of the substrate is ensured, so that the preparation requirement of the microsphere with the corresponding size can be met.
For another example, a contact angle adjusting film capable of promoting the contact angle of the microbeads on the substrate to be in the range of 30-150 degrees can be arranged on the surface of the substrate. The contact angle regulating film can ensure that the contact angle of the microbeads on the substrate is within the range of 30-150 degrees, and the surface property of the substrate is consistent, so that the prepared microarray is even in structure and consistent in size. In addition, the optimal arrangement of the contact angle regulating film can effectively facilitate regulating and controlling the contact angle between the microsphere and the surface of the substrate, and facilitates size control.
And the following steps: the contact angle can be regulated and controlled by adopting a chemical solvent to treat the substrate. The method comprises the following steps: the contact angle adjustment may be achieved by immersing the substrate in a chemical solvent including, but not limited to, hydrogen peroxide, sodium hydroxide, potassium hydroxide, hydrofluoric acid, hydrochloric acid, sulfuric acid, nitric acid.
The invention can better realize consistent substrate surface property and is convenient for regulating contact angle, and the substrate surface property is various in substance types, including but not limited to HMDS (hexamethyldisiloxane), APTMS (3-aminopropyl trimethoxysilane), APTES (3-aminopropyl triethoxysilane), HMMA (hexamethoxymethyl melamine) and other monomolecular films which are modified on the surface layer of the substrate, or gold plating is carried out on the surface of the substrate, such as gold plating is carried out on the surface of a silicon wafer, and then the substrate is modified by monomolecular films such as alkyl mercaptan and the like. Wherein the alkyl mercaptans include, but are not limited to, stearyl mercaptan.
The diameter of the microbeads is 1 μm-3mm.
There are many ways of adjusting the pressure, temperature and humidity of the condensation environment to further adjust and control the size of the microbeads, generally, any one of the pressure, temperature and humidity in the condensation environment is fixed first, and then the other two conditions are matched. For example: the temperature can be fixed firstly, and the regulation and control of the size of the microbeads can be realized through the regulation and control of the pressure and the humidity at a specific temperature; another example is: the humidity can be fixed first, and the regulation and control of the size of the microbeads can be realized through the regulation of temperature and pressure.
The second step to the fifth step are all performed in a condensing box, a pressure regulating valve is arranged on the condensing box, and the gaseous medium is led into the condensing box through a connecting pipeline with a connecting valve; in the third step, the process of controlling the size of the microbeads by adjusting the pressure, the temperature and the humidity of the condensing environment is as follows:
when the size of the micro-beads is too large, a connecting valve on a connecting pipeline is closed, a pressure regulating valve on the condensing box is opened, the size of the micro-beads can be gradually reduced, and when the micro-beads are reduced to the required size, the pressure regulating valve is closed;
when the size of the micro-beads is too small, the connecting valve on the connecting pipeline is opened, the pressure regulating valve on the condensing box is closed, the size of the micro-beads is gradually increased at the moment, and when the size of the micro-beads is increased to the required size, the connecting valve on the connecting pipeline is closed.
The second step to the fifth step are all carried out in a condensing box, and the gaseous medium is led into the condensing box through a connecting pipeline with a connecting valve; in the third step, the process of controlling the size of the microbeads by adjusting the pressure, the temperature and the humidity of the condensing environment is as follows:
when the size of the micro-beads is too large, a connecting valve on the connecting pipeline is closed, the temperature and the pressure in the condensing box are increased, at the moment, the size of the micro-beads is gradually reduced, and when the micro-beads are reduced to the required size, the second temperature control component is closed;
when the size of the micro-beads is too small, the connecting valve on the connecting pipeline is closed, the temperature and the pressure in the condensing box are reduced, the size of the micro-beads can be gradually increased, if the size of the micro-beads does not reach the requirement, the connecting valve on the connecting pipeline is closed after the size of the micro-beads is increased to the required size.
The manner of adjusting the size of the beads is not specifically mentioned, but any manner of adjusting the size of the beads by temperature, pressure and humidity is within the scope of the present invention.
The first step is carried out in an evaporation tank, and the specific process is as follows: adding the liquid medium into the evaporation tank, and heating the liquid medium in the evaporation tank to obtain the gaseous medium.
The technical scheme of the invention has the following advantages:
1. according to the microarray structure patterning process provided by the invention, gaseous medium is introduced into a condensation environment, condensation molding of microbeads with specific size on a matrix is realized by controlling the temperature, the pressure and the humidity of the condensation environment, then the condensed liquid microbeads are cooled into solid state by a refrigeration structure, molding of a microbead array pattern is realized, finally resin is injected into a microarray of which the matrix is covered with solid microbeads, a patterned microarray structure can be formed on the resin after the resin is solidified, and the medium on the resin is removed by heating and cleaning; the whole operation flow of the process is simple, the used equipment and raw materials are low in cost, and the time for manufacturing the patterned microarray structure is short; therefore, the invention provides a new process which has lower cost, simpler and more convenient operation and shorter time and can effectively realize the patterning of the microarray structure, the microarray structure prepared by the invention does not need to be arranged manually, and the microarray structure is a natural molding structure obtained after the condensation of the microbeads, and the operation is simpler and more convenient; applications in the biological field have unique advantages.
2. In order to better control the patterning of the micro-bead microarray structure, a contact angle regulating film is additionally arranged on the surface layer of the substrate, wherein the contact angle regulating film is preferably a monomolecular film of HMDS, APTMS, APTES or HMMA, or is plated with gold on the surface of the substrate, and then the monomolecular film of alkyl mercaptan is modified on the surface of the plated gold; the contact angle between the liquid microbeads and the substrate can be effectively regulated and controlled through the contact angle regulating film, so that the formation of a microbead microarray structure is better realized, and the size of the microbeads is better regulated and controlled.
3. The step of regulating and controlling the size of the microbeads is arranged in the condensing box, the size of the microbeads can be controlled more accurately only by mutually coordinating the pressure regulating valve arranged on the condensing box and the connecting pipeline for introducing the gaseous medium, and the method is simple and convenient to operate and has remarkable effect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is a schematic view of an apparatus capable of carrying out the process of the present invention;
FIG. 3 is a schematic view of the internal structure of the condensing box;
reference numerals illustrate:
1-an evaporation tank, 2-a condensation tank and 3-a connecting pipeline;
11-a first cavity, 12-a first temperature control component, 13-a first monitoring component and 14-a liquid injection hole;
21-second chamber, 22-second temperature control means, 23-second monitoring assembly, 24-substrate, 25-resin injection channels, 26-refrigerating structures, 27-transparent observation windows, 28-optical fiber probes and 29-pressure regulating holes.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the processes or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Example 1
A process for patterning a microarray structure, as shown in fig. 1, comprising:
step one, obtaining a gaseous medium;
step two, introducing a gaseous medium into a condensing environment in which the substrate is placed, controlling the temperature and the pressure of the condensing environment, and controlling the temperature of the substrate to condense the gaseous medium on the surface of the substrate to form microbeads;
thirdly, adjusting the pressure, temperature and humidity of the condensing environment so as to control the size of the microbeads, thereby forming microbeads with the required size;
step four, cooling and solidifying the condensed microbeads to prepare solid microbeads, and obtaining a microarray of the solid microbeads on a substrate;
injecting resin into the surface of the substrate with the microarray to enable the resin to be attached to the surface of the solid-state microbeads, and curing the resin after the resin covers the microarray on the surface of the substrate and is leveled to form a stable structure;
and step six, removing the medium on the stable structure to obtain the patterned microarray structure.
According to the invention, gaseous medium is introduced into a condensation environment, condensation molding of microbeads with specific size on a matrix is realized by controlling the temperature, the pressure and the humidity of the condensation environment, then the condensed liquid microbeads are cooled into solid state by a refrigeration structure, molding of a microbead array pattern is realized, finally resin is injected into the microarray of the solid microbeads covered on the matrix, a patterned microarray structure is formed on the resin after the resin is solidified, and the medium on the resin is removed by heating and cleaning; the whole operation flow of the process is simple, the used equipment and raw materials are low in cost, and the time for manufacturing the patterned microarray structure is short; therefore, the invention provides a new process which has lower cost, simpler and more convenient operation and shorter time and can effectively realize the patterning of the microarray structure.
The invention also provides a device for realizing the process, and solves the problem of higher equipment and instrument cost for preparing the micron-level array pattern by adopting other methods. An apparatus suitable for the process according to the invention is shown in fig. 2 and 3 and comprises an evaporation tank 1, a condensation tank 2 and a connecting line 3. The evaporation tank 1 includes a first chamber 11 for containing a medium, and a first temperature control member 12 for heating the medium in the first chamber 11 to be in a gaseous state. The condensing tank 2 comprises a second cavity 21, a second temperature control component 22 and a second monitoring assembly 23 which are arranged on the second cavity 21, a base 24 arranged in the second cavity 21, and a resin injection channel 25 extending to the upper side of the base 24 through the second cavity 21 for cooling the condensed liquid microbeads on the base 24 into a solid refrigeration structure 26. The connecting pipeline 3 is communicated with the first cavity 11 and the second cavity 21 and is used for guiding the gaseous medium in the first cavity 11 into the second cavity 21.
In the present invention, the above-mentioned second temperature control component 22 and the first temperature control component 12 are both temperature control bases, which are disposed below the corresponding cavities, that is, the temperature control bases are heating devices disposed below the corresponding cavities for heating the cavities, as shown in fig. 1 and 2.
In order to control the size of the microbeads more accurately, the two cavities can be completely and independently opened through the connecting valve arranged on the connecting pipeline 3, so that the independent control of the temperature, the humidity and the pressure in the second cavity is effectively realized, and the more accurate control of the size of the microbeads can be realized. The specific arrangement is as follows: a connection valve is provided on the connection pipe 3, and a second monitoring assembly 23 including a humidity detecting structure, a temperature detecting structure and a pressure detecting structure is provided on the second chamber 21, and a pressure regulating hole 29 with a valve is provided on the second chamber 21. According to the invention, the medium amount introduced into the second cavity 21 is controlled through the connecting valve arranged on the connecting pipeline 3, so that the humidity in the second cavity 21 can be effectively regulated and controlled; the pressure in the second cavity 21 can be effectively regulated through the pressure regulating hole 29 with the valve arranged on the second cavity 21; the temperature in the second chamber 21 can be adjusted in time by the second temperature control member 22. Therefore, the invention can timely adjust the temperature, humidity and pressure which are introduced into the second temperature control part 22 by connecting the valve, the pressure regulating hole 29 and the second temperature control part 22, thereby realizing the accurate control of the size of the microbeads.
In order to intuitively understand the formation condition of the micro-beads, the invention also provides a transparent observation window 27 and/or a monitoring device mounting hole on the second cavity 21. When the second cavity 21 is provided with a monitoring device mounting hole, a viewing device, such as an optical fiber probe 28, capable of viewing the condition in the second cavity 21 is mounted on the monitoring device mounting hole, so that the molding condition of the microbeads on the substrate 24 can be more intuitively seen.
In order to enable the surface of the substrate to form the microbeads with an ordered microarray structure, the material of the substrate is further limited, and the material of the substrate 24 is preferably silicon, silicon dioxide, mica or graphite; in order to make the formation of the microbeads more uniform, and to better regulate and control the contact angle between the medium and the substrate, a contact angle regulating film is further arranged on the surface layer of the substrate 24, so that the uniformity of the surface of the substrate 24 can be better ensured through the arrangement of the contact angle regulating film, and the regulation and control of the contact angle are facilitated. In the present invention, any material that can be used to control the contact angle between the medium and the substrate can be used for the surface modification of the substrate 24, and further, a contact angle control film, preferably an HMDS monolayer, is formed on the surface of the substrate 24.
In order to better achieve a more rapid solidification of the liquid microbeads, the cooling structure 26 is preferably a semiconductor cooling fin that is disposed below the substrate 24. More preferably, the refrigerating structure 26 is a peltier semiconductor refrigerating piece, the refrigerating surface of the peltier semiconductor refrigerating piece faces the inside of the condensation box 2, the radiating surface is arranged on the wall of the condensation box, the power supply line is connected from the condensation box, the substrate is arranged on the refrigerating surface, the power of the peltier semiconductor refrigerating piece is selected according to the size of the substrate, and the substrate can be rapidly refrigerated after being electrified.
The medium in the present invention may be any inert medium which is nonflammable and has good thermal stability, and the medium having good thermal stability means a medium which does not undergo thermal decomposition within a designed operating temperature range, and in the present invention, water, silicone oil or dioxane is preferable.
In order to facilitate timely regulation and control of the medium condition in the evaporation tank 1, the first cavity 11 is provided with a liquid injection hole 14 with a valve, and when the medium content in the first cavity 11 is insufficient, the medium can be effectively supplemented for the cavity through the liquid injection hole 14. The invention is also provided with a first monitoring component 13 on the first cavity 11; the first monitoring assembly 13 includes a temperature detecting structure and a pressure detecting structure. The temperature and pressure in the evaporation tank 1 are monitored in time by the temperature detection structure and the pressure detection structure.
The specific process for realizing the process of the invention by adopting the structure comprises the following steps:
firstly, medium, in this embodiment, water, silicone oil or dioxane is supplemented into the first cavity 11 of the evaporation tank 1, and the medium is heated by the first temperature control component 12 to be converted into a gas state, so that the temperature in the first cavity 11 reaches 290K-400K and the pressure reaches 100kPa-200kPa.
Secondly, introducing gaseous water into the condensing box 2 through the connecting pipeline 3, controlling the humidity in the condensing box 2 to be 20% -80%, regulating the temperature in the second cavity 21 to be 280K-360K, regulating the pressure to be 90-150kPa, enabling a medium to start condensing on the surface of the substrate 24, observing the size of the microbeads, regulating the temperature of the substrate to be 220K-350K, enabling the size of the microbeads to reach a specific size, and at the moment, gradually balancing the system in the second cavity 21 to form a microbead array with the specific size.
The refrigeration mechanism 26 is then activated to cause the condensed beads to transiently cool and solidify to obtain solid state beads, i.e., a microarray of solid state beads formed on the substrate 24.
Finally, resin is slowly injected or sprayed through the resin injection channel 25 to be attached to the surface of the solid-state microbeads, and the solid-state microbeads are maintained for a certain time to be leveled so as to ensure that the microarray formed by condensation is completely covered on the surface of the substrate, and then the resin is solidified to form a stable structure. The resin is a thermally curable or photo-curable resin.
The stable structure is subjected to medium separation and cleaning to obtain a patterned microarray structure.
In this embodiment, taking water as an example, the substrate is made of silicon dioxide, a layer of HMDS monomolecular film is disposed on the surface, the surface roughness is 0.1 μm, the contact angle of the microbeads on the surface of the substrate is 65 degrees, and the process of generating the microarray structure of microbeads with the size of 1 μm by adopting the above-mentioned process and device is as follows:
controlling the temperature in the first cavity 11 to be 350K, the pressure to be 100kPa, opening a connecting valve of the first cavity 11 and the second cavity 21, and also opening a pressure regulating valve of the second cavity 21, namely a valve on a pressure regulating hole 29, so that water vapor slowly enters the second cavity 21, controlling the temperature in the second cavity 21 to be 320K, the pressure to be 100kPa, the substrate temperature to be 290K-320K, condensing the water vapor on the surface of the substrate, and when the system slowly reaches dynamic balance, observing the size of the micro beads at the moment, if the size of the micro beads is oversized, closing the connecting valve communicated with the first cavity 11, opening the pressure regulating valve on the second cavity 21, and gradually reducing the size of the micro beads to 1 mu m; if the size of the beads is too small, a connection valve communicating with the first chamber 11 is opened, and a pressure regulating valve on the second chamber 21 is closed, and at this time, the size of the beads is gradually increased so that the size of the beads is increased to 1 μm. When the size of the micro-beads reaches 1 μm, the connection valve on the connection pipeline 3 and the pressure regulating valve on the second cavity 21 are closed, and at the moment, the peltier semiconductor refrigerating plate is started to cool the substrate at a high speed, so that the liquid micro-beads are solidified. And slowly injecting the photo-curing resin with proper temperature and viscosity, wherein the photo-curing resin with the viscosity of 600 Pa.s is adopted in the embodiment, the temperature is 300K, the photo-curing resin is attached to the surface of the solid-state microbeads, the time is maintained for 15 minutes, and ultraviolet light can be started after the surface of the photo-curing resin is leveled, so that the resin is cured, and a stable structure is formed. Finally, the system is allowed to return to normal temperature, the second cavity 21 is opened, and the photo-cured stable structure is taken out, and at this time, the resin layer in the stable structure is separated from the medium, and the separation surface has a circular hole array structure with a size of about 1 μm.
Example 2
A process for patterning a microarray structure using the apparatus disclosed in example 1 in combination with the process of the present invention to produce a microarray structure of 3 mm-sized microbeads, the process is as follows:
in this embodiment, the medium is water, the substrate is made of silicon, the surface roughness is 10 μm, the contact angle of the microbeads on the surface of the substrate is 90 degrees, the temperature 380K in the first cavity 11 and the pressure 120kPa are controlled, the connection valve between the first cavity 11 and the second cavity 21 is opened, the pressure regulating valve of the second cavity 21, namely the valve on the pressure regulating hole 29 is also opened, so that the water vapor slowly enters the second cavity 21, the temperature 300K in the second cavity 21 and the pressure 110kPa are controlled, the substrate temperature is 280K-300K, the water vapor starts to condense on the surface of the substrate, when the system slowly reaches dynamic balance, the microbead size is observed at this time, if the microbead size is too large, the connection valve communicated with the first cavity 11 is closed, the pressure regulating valve on the second cavity 21 is opened, and the microbead size is gradually reduced to 3mm; if the size of the beads is too small, a connection valve communicating with the first chamber 11 is opened, and a pressure regulating valve on the second chamber 21 is closed, and at this time, the size of the beads is gradually increased, so that the size of the beads is increased to 3mm. When the size of the microbeads reaches 3mm, the connecting valve on the connecting pipeline 3 and the pressure regulating valve on the second cavity 21 are closed, and at the moment, the peltier semiconductor refrigerating plate is started to cool the substrate at a high speed, so that the liquid microbeads are solidified. And slowly injecting the photo-curing resin with proper temperature and viscosity, wherein the photo-curing resin with the viscosity of 150Pa.s is adopted in the embodiment, the temperature is 300K, the photo-curing resin is attached to the surface of the solid-state microbeads, the time is maintained for 40 minutes, and ultraviolet light can be started after the surface of the photo-curing resin is leveled, so that the resin is cured, and a stable structure is formed. Finally, the system is allowed to return to normal temperature, the second cavity 21 is opened, and the photo-cured stable structure is taken out, and at this time, the resin layer in the stable structure is separated from the medium, and the separation surface has a circular hole array structure with a size of about 3mm.
Example 3
A process for patterning a microarray structure using the apparatus disclosed in example 1 in combination with the process of the present invention to produce a microarray structure of 1 mm-sized microbeads, the process is as follows:
in this embodiment, the medium is water, the substrate is made of silicon, the surface roughness is 1 μm, the contact angle of the microbeads on the surface of the substrate is 80 degrees, the temperature 320K in the first cavity 11 and the pressure 100kPa are controlled, the connection valve between the first cavity 11 and the second cavity 21 is opened, the pressure regulating valve of the second cavity 21, namely the valve on the pressure regulating hole 29, is also opened, so that the water vapor slowly enters the second cavity 21, the temperature 280K in the second cavity 21 and the pressure 100kPa are controlled, the substrate temperature is 240K-260K, the water vapor starts to condense on the surface of the substrate, when the system slowly reaches dynamic balance, the microbead size is observed at this time, if the microbead size is too large, the connection valve communicated with the first cavity 11 is closed, the pressure regulating valve on the second cavity 21 is opened, and the microbead size is gradually reduced to 1mm; if the size of the beads is too small, a connection valve communicating with the first chamber 11 is opened, and a pressure regulating valve on the second chamber 21 is closed, and at this time, the size of the beads is gradually increased so that the size of the beads is increased to 1mm. When the size of the micro-beads reaches 1mm, the connecting valve on the connecting pipeline 3 and the pressure regulating valve on the second cavity 21 are closed, and at the moment, the Peltier semiconductor refrigerating plate is started to cool the substrate at a high speed, so that the liquid micro-beads are solidified. And slowly injecting the photo-curing resin with proper temperature and viscosity, wherein the photo-curing resin with the viscosity of 800 Pa.s is adopted in the embodiment, the photo-curing resin is attached to the surface of the solid microbeads, the time is maintained for 20 minutes, and ultraviolet light can be started after the surface of the photo-curing resin is leveled, so that the resin is cured, and a stable structure is formed. Finally, the system is allowed to return to normal temperature, the second cavity 21 is opened, and the photo-cured stable structure is taken out, and at this time, the resin layer in the stable structure is separated from the medium, and the separation surface has a circular hole array structure with a size of about 1mm.
Example 4
A process for patterning a microarray structure using the apparatus disclosed in example 1 in combination with the process of the present invention to produce a microarray structure of 1 mm-sized microbeads, the process is as follows:
in this embodiment, the medium is dioxane, the substrate is made of silicon, the surface roughness is 5 μm, the contact angle of the microbeads on the surface of the substrate is 100 degrees, the temperature 400K in the first cavity 11 and the pressure 125kPa are controlled, the connection valve of the first cavity 11 and the second cavity 21 is opened, the pressure regulating valve of the second cavity 21, namely the valve on the pressure regulating hole 29 is also opened, the gaseous medium slowly enters the second cavity 21, the temperature 350K in the second cavity 21 and the pressure 110kPa are controlled, the substrate temperature is 290K-310K, the gaseous medium starts to condense on the surface of the substrate to form microbeads, when the system slowly reaches dynamic balance, the size of the microbeads is observed at this time, if the size of the microbeads is too large, the connection valve communicated with the first cavity 11 is closed, the pressure regulating valve on the second cavity 21 is opened, the size of the microbeads is gradually reduced, and the size of the microbeads is reduced to 1mm; if the size of the beads is too small, a connection valve communicating with the first chamber 11 is opened, and a pressure regulating valve on the second chamber 21 is closed, and at this time, the size of the beads is gradually increased so that the size of the beads is increased to 1mm. When the size of the micro-beads reaches 1mm, the connecting valve on the connecting pipeline 3 and the pressure regulating valve on the second cavity 21 are closed, and at the moment, the Peltier semiconductor refrigerating plate is started to cool the substrate at a high speed, so that the liquid micro-beads are solidified. And slowly injecting the photo-curing resin with proper temperature and viscosity, wherein the photo-curing resin with the viscosity of 5 Pa.s is adopted in the embodiment, the photo-curing resin is attached to the surface of the solid microbeads, the time is maintained for 1 minute, and ultraviolet light can be started after the surface of the photo-curing resin is leveled, so that the resin is cured, and a stable structure is formed. Finally, the system is allowed to return to normal temperature, the second cavity 21 is opened, and the photo-cured stable structure is taken out, and at this time, the resin layer in the stable structure is separated from the medium, and the separation surface has a circular hole array structure with a size of about 1mm.
Example 5
A process for patterning a microarray structure using the apparatus disclosed in example 1 in combination with the process of the present invention to produce a microarray structure of 1 mm-sized microbeads, the process is as follows:
in this embodiment, the medium is dioxane, the substrate is made of silicon, the surface roughness is 5 μm, the substrate is soaked with a chemical reagent ammonia solution, the mass concentration of the ammonia solution is 1%, the soaking time is 2min, the contact angle of the microbeads on the surface of the substrate is 80 degrees, the temperature 330K in the first cavity 11 and the pressure 110kPa are controlled, the connecting valve of the first cavity 11 and the second cavity 21 is opened, the pressure regulating valve of the second cavity 21, namely the valve on the pressure regulating hole 29 is also opened, so that the gaseous medium slowly enters the second cavity 21, the temperature 310K in the second cavity 21 and the pressure 105kPa are controlled, the substrate temperature is 240K-260K, the gaseous medium starts to condense on the surface of the substrate to form microbeads, when the system slowly reaches dynamic balance, the microbead size is observed at this moment, if the microbead size is too large, the connecting valve communicated with the first cavity 11 is closed, the pressure regulating valve on the second cavity 21 is opened, the microbead size is gradually reduced to 1mm; if the size of the beads is too small, a connection valve communicating with the first chamber 11 is opened, and a pressure regulating valve on the second chamber 21 is closed, and at this time, the size of the beads is gradually increased so that the size of the beads is increased to 1mm. When the size of the micro-beads reaches 1mm, the connecting valve on the connecting pipeline 3 and the pressure regulating valve on the second cavity 21 are closed, and at the moment, the Peltier semiconductor refrigerating plate is started to cool the substrate at a high speed, so that the liquid micro-beads are solidified. And slowly injecting a photo-curing resin with proper temperature and viscosity, wherein the thermosetting resin with the viscosity of 40mPa.s is adopted in the embodiment, the thermosetting resin is adhered to the surface of the solid-state microbeads, and is maintained for 1 minute, after the surface of the thermosetting resin is leveled, the temperature of one side of the thermosetting resin, which is close to the peltier semiconductor refrigerating sheet, is controlled to be minus 40 ℃, the temperature of one side of the thermosetting resin, which is far from the peltier semiconductor refrigerating sheet, is controlled to be 150 ℃, and a stable structure is formed after 30 seconds of curing. Finally, the system is allowed to return to normal temperature, the second cavity 21 is opened, and the thermally cured stable structure is taken out, and at this time, the resin layer in the stable structure is separated from the medium, and the separation surface has a circular hole array structure with a size of about 1mm.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (6)
1. A process for patterning a microarray structure, comprising:
step one, obtaining a gaseous medium;
step two, introducing a gaseous medium into a condensing environment in which the substrate is placed, controlling the temperature and the pressure of the condensing environment, and controlling the temperature of the substrate to condense the gaseous medium on the surface of the substrate to form microbeads;
thirdly, adjusting the pressure, temperature and humidity of the condensing environment so as to control the size of the microbeads, thereby forming microbeads with the required size;
step four, cooling and solidifying the condensed microbeads to prepare solid microbeads, and obtaining a microarray of the solid microbeads on a substrate;
injecting resin into the surface of the substrate with the microarray to enable the resin to be attached to the surface of the solid-state microbeads, and curing the resin after the resin covers the microarray on the surface of the substrate and is leveled to form a stable structure;
step six, removing the medium on the stable structure to obtain a patterned microarray structure;
the temperature of the gaseous medium obtained in the step one is 290K-410K, and the pressure is 100kPa-200kPa; the temperature of the condensing environment in the second step is 280K-370K, the pressure is 90-150kPa, the temperature of the substrate is controlled to be 220K-360K, and the humidity of the condensing environment is 20% -80%;
the medium is water or dioxane;
when the medium is water, the temperature of the gaseous medium is 290K-400K, the temperature of the condensing environment is 280K-360K, and the temperature of the substrate is 220K-350K;
when the medium is dioxane, the temperature of the gaseous medium is 300K-410K, the temperature of the condensing environment is 290K-370K, and the temperature of the substrate is 230K-360K;
the substrate is made of silicon, silicon dioxide, mica, glass or graphite; or the surface of the substrate is provided with a contact angle regulating film; or adopting chemical solvent to treat the substrate to realize the regulation and control of the contact angle;
the contact angle regulating film is a monomolecular film of HMDS, APTMS, APTES or HMMA modified on the surface layer of the substrate; or gold plating is carried out on the surface of the substrate, and then a monomolecular film of alkyl mercaptan is modified on the gold plating surface;
the second step to the fifth step are all performed in a condensing box, a pressure regulating valve is arranged on the condensing box, and the gaseous medium is led into the condensing box through a connecting pipeline provided with a connecting valve; in the third step, the process of controlling the size of the microbeads by adjusting the pressure, the temperature and the humidity of the condensing environment is as follows:
when the size of the micro-beads is too large, the connecting valve is closed, the pressure regulating valve on the condensing box is opened, the size of the micro-beads is gradually reduced, and when the micro-beads are reduced to the required size, the pressure regulating valve is closed;
when the size of the micro-beads is too small, the connecting valve is opened, the pressure regulating valve on the condensing box is closed, the size of the micro-beads is gradually increased, and after the size of the micro-beads is increased to the required size, the connecting pipeline is closed.
2. The process for patterning a microarray structure of claim 1 wherein the resin is a photo-curable resin or a thermosetting resin.
3. The process for patterning a microarray structure according to claim 1 or 2, wherein the contact angle of the microbeads on the substrate is 30 ° -150 °.
4. The process for patterning a microarray structure according to claim 1 or 2, wherein,
the chemical solvents include, but are not limited to, hydrogen peroxide, sodium hydroxide, potassium hydroxide, hydrofluoric acid, hydrochloric acid, sulfuric acid, nitric acid.
5. The process for patterning a microarray structure according to claim 1 or 2, wherein the microbeads have a diameter of 1 μm to 3mm.
6. The process for patterning a microarray structure according to claim 1 or 2, wherein the first step is performed in an evaporation tank, and comprises the following steps: adding the liquid medium into the evaporation tank, and heating the liquid medium in the evaporation tank to obtain the gaseous medium.
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| CN101910829A (en) * | 2007-11-14 | 2010-12-08 | 3M创新有限公司 | Make the method for microarray |
| CN103180735A (en) * | 2011-03-28 | 2013-06-26 | 株式会社Ntt都科摩 | Method for fabricating microarrays of soft materials |
| JP2013149884A (en) * | 2012-01-23 | 2013-08-01 | Dainippon Printing Co Ltd | Method for manufacturing pattern structure, nanoimprint lithography method, and imprint device |
| EP3205394A1 (en) * | 2016-02-10 | 2017-08-16 | Karlsruher Institut für Technologie | Patterned substrate having hydrophilic and hydrophobic areas and method for producing the same |
| CN108472647A (en) * | 2015-10-16 | 2018-08-31 | 牛津大学科技创新有限公司 | Microfluid is arranged |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101910829A (en) * | 2007-11-14 | 2010-12-08 | 3M创新有限公司 | Make the method for microarray |
| CN103180735A (en) * | 2011-03-28 | 2013-06-26 | 株式会社Ntt都科摩 | Method for fabricating microarrays of soft materials |
| JP2013149884A (en) * | 2012-01-23 | 2013-08-01 | Dainippon Printing Co Ltd | Method for manufacturing pattern structure, nanoimprint lithography method, and imprint device |
| CN108472647A (en) * | 2015-10-16 | 2018-08-31 | 牛津大学科技创新有限公司 | Microfluid is arranged |
| EP3205394A1 (en) * | 2016-02-10 | 2017-08-16 | Karlsruher Institut für Technologie | Patterned substrate having hydrophilic and hydrophobic areas and method for producing the same |
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