CN113910505A - Processing method of polymer micro-column array - Google Patents
Processing method of polymer micro-column array Download PDFInfo
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- CN113910505A CN113910505A CN202111051357.9A CN202111051357A CN113910505A CN 113910505 A CN113910505 A CN 113910505A CN 202111051357 A CN202111051357 A CN 202111051357A CN 113910505 A CN113910505 A CN 113910505A
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- 229920000642 polymer Polymers 0.000 title claims abstract description 20
- 238000003672 processing method Methods 0.000 title claims abstract description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 43
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 28
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 26
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 26
- 238000005520 cutting process Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 230000001678 irradiating effect Effects 0.000 claims abstract description 5
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 5
- 239000000178 monomer Substances 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 15
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 11
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011521 glass Substances 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 238000003698 laser cutting Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000012125 lateral flow test Methods 0.000 description 4
- BJELTSYBAHKXRW-UHFFFAOYSA-N 2,4,6-triallyloxy-1,3,5-triazine Chemical compound C=CCOC1=NC(OCC=C)=NC(OCC=C)=N1 BJELTSYBAHKXRW-UHFFFAOYSA-N 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OXBLVCZKDOZZOJ-UHFFFAOYSA-N 2,3-Dihydrothiophene Chemical compound C1CC=CS1 OXBLVCZKDOZZOJ-UHFFFAOYSA-N 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/38—Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
- B29C33/3842—Manufacturing moulds, e.g. shaping the mould surface by machining
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Shaping Of Tube Ends By Bending Or Straightening (AREA)
Abstract
The invention relates to the field of micro-nano processing of new materials, in particular to a processing method of a polymer micro-column array, which comprises the following steps: A. designing a mold: designing a surface micro-column array pattern according to needs; B. manufacturing a mould: cutting PMMA according to the surface micro-column array pattern to obtain a PMMA mould with a specific surface pattern; C. and (3) PDMS (polydimethylsiloxane) reverse molding: uniformly pouring the PDMS prepolymer on the surface of the PMMA mould, heating and curing the PDMS prepolymer, and demoulding to obtain a PDMS mould with a specific surface pattern; D. OSTE reverse mold: and uniformly pouring liquid OSTE on the surface of the PDMS mold, and irradiating, curing and demolding by using an ultraviolet lamp to obtain the OSTE sheet with the surface provided with the micro-column array. The invention can effectively solve the problems that the conventional material (silicon-based and glass-based) micro-column array is complex to process and high in cost, so that the material with the micro-column array is difficult to popularize and use on a large scale, and the like.
Description
Technical Field
The invention relates to the field of micro-nano processing of new materials, in particular to a processing method of a polymer micro-column array.
Background
A micropillar array is a structure of a sheet of uniformly arranged micron-sized pillars, which may be circular or square in cross-section, typically several hundred microns in diameter and up to 1000 μm in length, and silicon, glass, polymers (including SU-8 and PDMS), etc. are common fabrication materials. The hydrophilically treated microneedle array can be used as a capillary pump, which is widely used as a base material for lateral flow assays.
However, the conventional material (silicon-based or glass-based) micro-column array is complex to process and high in cost, so that the material with the micro-column array is difficult to popularize and use on a large scale.
Disclosure of Invention
The invention aims to solve the problems that the conventional material (silicon-based and glass-based) micro-column array is complex to process and high in cost, so that the material with the micro-column array is difficult to popularize and use on a large scale, and the like.
In order to solve the technical problems, the invention adopts the following technical scheme:
a processing method of a polymer micro-column array comprises the following steps:
A. designing a mold: designing a surface micro-column array pattern according to needs;
B. manufacturing a mould: cutting PMMA according to the surface micro-column array pattern to obtain a PMMA mould with a specific surface pattern;
C. and (3) PDMS (polydimethylsiloxane) reverse molding: uniformly pouring the PDMS prepolymer on the surface of the PMMA mould, heating and curing the PDMS prepolymer, and demoulding to obtain a PDMS mould with a specific surface pattern;
D. OSTE reverse mold: and uniformly pouring liquid OSTE on the surface of the PDMS mold, and irradiating, curing and demolding by using an ultraviolet lamp to obtain the OSTE sheet with the surface provided with the micro-column array.
The invention provides a processing method of a polymer micro-column array, which uses a novel material OSTE to manufacture the micro-column array through steps of laser cutting, reverse molding and the like. The microstructure was characterized, hydrophilized, used as a capillary pump, and the capillary flow properties of the liquid were tested.
OSTE is known collectively as off-stoichiometrically thio-enes, and is based on the chemical structure of UV curable thiol-ene, using non-stoichiometric ratios to control its mechanical strength and surface chemical groups. The material has good mechanical properties, can realize illumination rapid molding by click chemistry, and has the potential of large-scale commercial production. Compared with the traditional silicon-based or glass-based micro-column array, the OSTE has better deformation performance, simpler processing and lower cost. By integrating the performance of OSTE, the method has the potential of Roll-to-Roll production, and can solve the defects of time and labor waste, high labor intensity, low production rate, low dimensional stability and the like in sheet technology production.
Preferably, the PDMS comprises the following components and proportions: SYLGARD 184silicon monomer and curing agent were mixed in a mass ratio of 10: 1.
Preferably, the amount of mercapto groups of the OSTE groups in the OSTE solution is more than 40% of the amount of vinyl groups.
Preferably, the OSTE solution comprises the following components: thiol group monomer, vinyl monomer and curing agent.
Preferably, the thiol group monomer comprises pentaerythritol tetramercaptoacetate and the vinyl monomer comprises triallyl cyanurate.
Thiol group monomers, vinyl monomers, these agents only serve to provide a thiol group and a vinyl group, in a ratio that is specific to the group, not a specific chemical agent. The invention selects OSTE (40%), and the percentage directly represents the excess degree of sulfydryl. The amount of surface active groups, i.e., mercapto groups on the surface of the material, is higher and the activity is higher than that of OSTE (30% or less). If OSTE (50% or more) is used, however, the elastoplasticity is reduced, which is extremely disadvantageous in the case of preparing OSTE sheets and, ultimately, in the case of obtaining lateral flow test strip products. Studies have shown that when the number of mercapto groups of the OSTE group is 40% greater than the number of vinyl groups, i.e. mercapto: vinyl 1.4:1, rapid prototyping is possible at ambient temperature and UV, and the OSTE properties obtained are optimal.
Preferably, the curing agent is a photoinitiator Igr 819.
Preferably, in step a, the surface micropillar array pattern is designed using SOLIDWORKS software.
The present invention uses a simple method to fabricate the microneedle array of OSTE. The manufacturing process comprises the steps of designing a drawing by using SOLIDWORKS software, cutting an acrylic plate by laser, inverting a PDMS mold and inverting an OSTE mold. Wherein PDMS is prepared by mixing SYLGARD 184silicon monomer and curing agent in a ratio of 10:1, and is baked and cured at 70 ℃ by an oven; the OSTE (40%) was formulated using three reagents, thiol monomer (pentaerythritol tetramercaptoacetate), vinyl monomer (triallyl cyanurate) and photoinitiator Igr 819, and cured by UV irradiation. The whole process is simple to operate and short in time consumption, the whole process does not exceed 2 hours, and the space between the micro-columns can be freely adjusted (obvious micro-columns exist when the space is 350 mu m or more).
Preferably, in step B, a laser cutting machine is used to cut PMMA, specifically: the inner X-direction grains are cut firstly, then the Y-direction grains are cut, and finally the edge of the die is cut to separate the die.
The inner lines are cut in the X direction and the Y direction, so that the micro-column array can be cut simply, conveniently and quickly, and finally the edge of the die is cut to enable the die to be separated from the acrylic plate.
Preferably, the specific operation of step C is: pouring the prepared PDMS prepolymer on the surface of the PMMA mould uniformly, pumping out bubbles, heating and curing at 70 ℃ for 1 hour, and then stripping off the PMMA mould to obtain the PDMS mould with a specific surface pattern.
Preferably, the PDMS prepolymer is heat cured by evacuating air bubbles using a vacuum pump and using an electrothermal blowing dry box.
Preferably, the specific operation of step D is: and uniformly pouring the prepared liquid OSTE on the surface of the PDMS mold, irradiating and curing for 3 minutes by using an ultraviolet lamp, and then stripping and removing the PDMS mold to obtain the OSTE sheet with the surface provided with the micro-column array.
The ultraviolet lamp is irradiated for curing for 2-3 minutes. If the curing time is too short, the material is difficult to form; however, if the curing time is too long, it may result in the material being difficult to separate from the template.
Preferably, the method further comprises the following steps:
E. the OSTE sheet was further processed to obtain lateral flow strips.
Preferably, the flow characteristics of the lateral flow chromatography test strip conform to the walsh equation.
Through testing, the flow characteristics of the lateral chromatography test strip obtained by the method conform to the Walsh equation and are consistent with the flow characteristics on the traditional lateral chromatography detection substrate. Compared with the traditional lateral chromatography detection substrate, the lateral chromatography test strip obtained by the invention is a transparent substrate, has the characteristics of stable flow rate and stable surface property, and has good application prospect.
An OSTE sheet having an array of micropillars on its surface is obtained by the method of processing a polymer micropillar array as described above.
Compared with the prior art, the implementation of the invention has the following beneficial effects:
1. the processing method of the invention has low cost and high efficiency, and can be used for industrial mass production.
2. The invention adopts PMMA laser cutting to manufacture the mould with uniform texture, so that the OSTE substrate obtained after twice die reversing also has uniform micro-column array.
3. The invention leads the texture size of PMMA to be controllable by guiding the laser cutting mode through CAD drawing, and leads the size of the microcolumn array of OSTE finally obtained by twice back molding to be controllable.
4. The invention uses UV lamp to irradiate the liquid OSTE material on PDMS for 3 minutes, so that OSTE is rapidly molded to form a micro-column array with uniform surface.
5. The materials used in the method have good mutual stripping performance, the dies can be removed by adopting a physical stripping mode in both twice die inversions on the premise of keeping the micro-column array structure, and compared with the dies removed by a traditional erosion method, the method is more convenient and rapid, environment-friendly and practical, and has good popularization prospect.
Drawings
FIG. 1 is a schematic flow chart of a method for processing a polymer microcolumn array according to the present invention; wherein 1-acrylic (PMMA), 2-Polydimethylsiloxane (PDMS), 3-non-stoichiometric mercaptan (OSTE);
FIG. 2 is a schematic diagram of the cutting pattern of PMMA in processing step (1) (2); wherein p represents the grain spacing, X represents the first cutting direction, and Y represents the second cutting direction;
FIG. 3 is an image of an OSTE micro-column array obtained by a body microscope after the processing flow of the present invention is completed;
FIG. 4 is a schematic view of the shape of a lateral flow test strip prepared after the process flow of the present invention is completed;
FIG. 5 is a graph of volumetric capacity results for lateral flow test strips prepared after the completion of a process flow of the present invention;
FIG. 6 is a graph of flow rate versus time for a lateral flow test strip prepared after completion of a process sequence of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The following description of the embodiments of the present invention with reference to the drawings shows a method for processing a polymer micro-column array, comprising the following steps:
1. preparing a PMMA mold: selecting PMMA as a mold, and designing a cutting pattern of the PMMA by using SOLIDWORKS software, wherein the size of one PMMA mold is 11cm multiplied by 11cm as shown in figure 2;
2. laser cutting of PMMA: using a laser cutter, as shown in fig. 2, the internal texture cutting parameters are set as: the surface cutting mode is that the material thickness is 1mm, the blowing-free mode is adopted, the cutting speed is 100mm/s, the power is 25%, the corner power is 70%, the laser frequency is 20kHz, and the sealing length is 0 mm; the external disconnection parameter is set as: cutting off a cutting mode, wherein the thickness of the material is 1mm, the cutting speed is 10mm/s, the power is 90%, the corner power is 70%, the laser frequency is 20kHz, and the length of a seal is 0 mm; the cutting sequence is that the inner X-direction grains are cut firstly, then the Y-direction grains are cut, and finally the edge of the die is cut to separate the die;
3. and (3) PDMS (polydimethylsiloxane) reverse molding: uniformly pouring the prepared PDMS (a SYLGARD 184silicon monomer and a photoinitiator Igr 819 mixed according to the mass ratio of 10: 1) on the surface of a PMMA mould, pumping out bubbles in the PDMS through a vacuum pump, heating and curing the PDMS for 1 hour at 70 ℃ by using an electrothermal blowing drying box, and taking off the PDMS from the PMMA;
4. OSTE reverse mold: OSTE (40%) is prepared by using three reagents of thiol monomer (pentaerythritol tetramercaptoacetate), vinyl monomer (triallyl cyanurate) and photoinitiator Igr 819, the prepared OSTE is uniformly poured on the surface of a PDMS mold, the OSTE is irradiated and cured for 3 minutes by using an ultraviolet lamp, and the OSTE is taken off from the PDMS to obtain (5) an OSTE micro-column array, as shown in FIG. 3.
Since the intensity distribution of the laser beam from the core to the periphery is gaussian (ALDA,2011), the groove profiles on PMMA and ostee are similar to gaussian curves as shown in fig. 1 (this schematic does not reflect true scale).
The structural dimensions of the OSTE micropillar array with a grain pitch of 350 μm and 500 μm prepared by the above processing method were obtained by using a scanning electron microscope, ImageJ software and a step profiler, as shown in table 1;
after the OSTE micro-column array is obtained by the above processing method, the OSTE micro-column array is cut into the shape of a lateral chromatography test strip by using a laser cutting machine, as shown in fig. 4, the cutting parameters are set as follows: the surface cutting mode is that the material thickness is 1mm, the blowing-free mode is that the cutting speed is 30mm/s, the power is 70 percent, the corner power is 50 percent, the laser frequency is 20kHz, and the sealing length is 0 mm; carrying out hydrophilic treatment on the test strip by using a plasma cleaning machine, and covering a hydrophilic adhesive tape on the test strip; the long axis of the test strip is along the Y direction;
vertically immersing the test strip in water, measuring the volume capacity of the test strip, observing the permeation condition, and taking out the test strip in time when the permeation stops; the volume capacity of the test strip was calculated by measuring the weight of the test strip before and after water absorption, as shown in table 1 and fig. 5;
15 μ L and 12 μ L of the dye solution were dropped on the OSTE test strips of p 350 μm and p 500 μm, respectively, and the results showed that the flow characteristics thereof conformed to the walsh equation, as shown in fig. 6; the experimental data were fitted to the walsh equation to obtain the coefficients of determination and their average flow rates, as shown in table 1.
TABLE 1
*
This example developed a method for rapidly preparing a microcolumn array using a novel polymer OSTE, demonstrating that it can be used as a capillary pump and provide flow rates relevant to clinical assays. The uniform microstructure ensures uniformity of flow from strip to strip. The OSTE micro-column array can be used as a substrate material for lateral chromatography detection, and has wide application prospect in the lateral chromatography detection.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, therefore, the present invention is not limited by the appended claims.
Claims (10)
1. A processing method of a polymer micro-column array is characterized by comprising the following steps:
A. designing a mold: designing a surface micro-column array pattern according to needs;
B. manufacturing a mould: cutting PMMA according to the surface micro-column array pattern to obtain a PMMA mould with a specific surface pattern;
C. and (3) PDMS (polydimethylsiloxane) reverse molding: uniformly pouring the PDMS prepolymer on the surface of the PMMA mould, heating and curing the PDMS prepolymer, and demoulding to obtain a PDMS mould with a specific surface pattern;
D. OSTE reverse mold: and uniformly pouring the OSTE solution on the surface of the PDMS mold, and irradiating, curing and demolding by using an ultraviolet lamp to obtain the OSTE sheet with the surface provided with the micro-column array.
2. The method for processing the polymer micro-column array according to claim 1, wherein the PDMS prepolymer comprises the following components in parts by weight: SYLGARD 184silicon monomer and curing agent were mixed in a mass ratio of 10: 1.
3. The method of claim 1, wherein the amount of mercapto groups of the OSTE groups is more than 40% of the amount of vinyl groups in the OSTE solution.
4. The method of processing a polymer micropillar array according to claim 1, wherein the OSTE solution comprises the following components: thiol group monomer, vinyl monomer and curing agent.
5. The method for processing the polymer microcolumn array according to claim 2 or 4, wherein the curing agent is a photoinitiator Igr 819.
6. The method for processing the polymer microcolumn array according to claim 1, wherein the specific operation of step C is: pouring the prepared PDMS prepolymer on the surface of the PMMA mould uniformly, pumping out bubbles, heating and curing at 70 ℃ for 1 hour, and then stripping off the PMMA mould to obtain the PDMS mould with a specific surface pattern.
7. The method for processing the polymer microcolumn array according to claim 1, wherein the specific operation of step D is: and uniformly pouring the prepared liquid OSTE on the surface of the PDMS mold, irradiating and curing for 2-3 minutes by using an ultraviolet lamp, and then stripping off the PDMS mold to obtain the OSTE sheet with the surface provided with the micro-column array.
8. The method for processing the polymer microcolumn array according to claim 1, further comprising the steps of:
E. the OSTE sheet was further processed to obtain lateral flow strips.
9. The method of processing a polymer micro-column array according to claim 8, wherein the flow characteristics of the lateral flow chromatography test strip conform to the walsh equation.
10. An OSTE sheet having an array of micropillars on its surface obtained by the method of processing a polymer micropillar array as claimed in claim 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114434709A (en) * | 2021-12-28 | 2022-05-06 | 汕头大学 | Quick manufacturing method of concave micro-well and micro-channel |
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| CN114434709B (en) * | 2021-12-28 | 2024-04-30 | 汕头大学 | Quick manufacturing method of concave micro-well and micro-channel |
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