CN101143705A - Method for preparing micrometer and submicron probe arrays - Google Patents
Method for preparing micrometer and submicron probe arrays Download PDFInfo
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- CN101143705A CN101143705A CNA2007101345752A CN200710134575A CN101143705A CN 101143705 A CN101143705 A CN 101143705A CN A2007101345752 A CNA2007101345752 A CN A2007101345752A CN 200710134575 A CN200710134575 A CN 200710134575A CN 101143705 A CN101143705 A CN 101143705A
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000003491 array Methods 0.000 title claims description 18
- 239000000523 sample Substances 0.000 title claims description 15
- 239000000835 fiber Substances 0.000 claims abstract description 31
- 229920000642 polymer Polymers 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000005530 etching Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 239000000057 synthetic resin Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 238000010276 construction Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 12
- 238000001338 self-assembly Methods 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 238000005520 cutting process Methods 0.000 abstract 2
- 238000010923 batch production Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000004506 ultrasonic cleaning Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 238000007920 subcutaneous administration Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- ZSIQJIWKELUFRJ-UHFFFAOYSA-N azepane Chemical compound C1CCCNCC1 ZSIQJIWKELUFRJ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000010255 intramuscular injection Methods 0.000 description 1
- 239000007927 intramuscular injection Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
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Abstract
The invention discloses a method of preparing a micrometer and sub-micrometer needle array. The method adopts the self-assembly technology and integrates the filling, cutting and controllable corrosion technologies. First, the self-assembly technology is adopted to technically assemble the micrometer/sub-micrometer fiber; and then the polymeric compound is filled, finally the micrometer and sub-micrometer needle array is prepared by the cutting and the controllable corrosion technologies. The invention has the advantages of low cost, no need of complicate equipments and technologies, capability of quick batch production, large area of needle array, smooth needle surface, adjustable diameter, length and taper, etc., and is widely applicable in the detecting, sensing, optical, biology and medicine fields, etc.
Description
Technical field
The present invention relates to the preparation method of a kind of nanometer and micron fine structure material, the preparation method of particularly a kind of micron and submicron probe arrays.
Background technology
The preparation of micron and submicron probe arrays is a technology with important application background.At optical field, micron/submicron probe arrays can be used as near-field optical probe, obtains near field optic information; At biomedicine field, micron pin array is mainly used in the painful administration of subcutaneous nothing, the painful tissue fluid extraction of subcutaneous nothing etc., overcome oral administration to GI stimulation, intramuscular injection can not continue medication, external application is because the cuticular difficult problems such as being difficult to reach required dosage that stops.Because current micron pin array preparation mainly depends on micro-processing technology, as reactive ion beam etching (RIBE), photoetching etc., thereby preparation cost is high.And in order to prevent to infect, stain etc., a micron pin array all is disposable usually.Therefore, this has greatly limited its application and scope.
Summary of the invention
Goal of the invention: the micron that the purpose of this invention is to provide that a kind of technology is simple, cost is low and the method for making of submicron probe arrays.
Technical scheme: the preparation method of micron of the present invention and submicron probe arrays may further comprise the steps:
1, by self-assembling technique assembling micron, sub-micron fibers, obtains to arrange regular fibre bundle;
2, above-mentioned fibre bundle is formed fiber and polymer complex structure by physics or chemical method packing volume than the polymer that is 0.1～0.6;
3, above-mentioned fiber and polymer complex structure are cut into the thin slice of 1mm～1cm according to different needs;
4, above-mentioned section being put into concentration is 0.01～40% HF acid etching solution, or to put into concentration be 0.01～80% KOH etchant solution, under 10～90 ℃ of temperature, corrodes 10 seconds～72 hours, forms the needle-like array structure.
Said micron and sub-micron fibers are silicon in the step (1), or glass, or ceramic, or fibrous material such as quartz.
Said filled polymer material is a polymethyl methacrylate in the step (2), or polystyrene, or macromolecular material such as natural synthetic resin, and said physics or chemical method are reactive polymeric fill method, heating and melting fill method and solution fill method.
Beneficial effect: the present invention compared with prior art has following outstanding advantage:
1, greatly reduced the preparation cost of micron and submicron probe arrays.
2, do not need expensive complex technology and equipment such as little processing.
3, can be by parameters such as spacing, length of needlepoint, needle point tapering between the pin of telomerized polymer packing volume percentage and corrosion parameter conveniently regulating and controlling micron and submicron probe arrays.
4, technology is simple, and the place environment is had no special requirements.
5, simple to operate, manufacturing cycle is short.
Description of drawings
Fig. 1 is the schematic diagram of preparation process.Wherein (a) fiber self assembly; (b) assembly mechanism schematic diagram; (c) polymer is filled and section; (d) and (e) corrosion process and mechanism schematic diagram; (f) obtain the pin array.
Fig. 2 is the sem photograph of the micron pin array of preparation.
The specific embodiment
The preparation method of micron of the present invention and submicron probe arrays, the design that comprises self assembly and polymer fill process is with definite; Determining of the technology of corrosion and parameter.
Embodiment 1: with the SiO of diameter 8 micron dimensions
2Fiber obtains SiO by self-assembling technique
2Fibre bundle; Put it into then in MMA (polymethyl methacrylate) solution that adds BPO, place water-bath to make polymer cure, SiO in 60 ℃ of heat treatment 24h
2The volume ratio of fibre bundle and polymer cure thing is 0.1; Be cut into the thin slice that thickness is 1mm then, corrode 5min down with 30 ℃ of constant temperature of 40%HF acid solution, the deionized water ultrasonic cleaning can obtain nano needle arrays after the drying.
Embodiment 2: with the SiO of 8 microns of diameters
2Fiber obtains SiO by self-assembling technique
2Fibre bundle; Put it into then in the styrene solution that adds hexamethylene imine base lithium, place water-bath to make polymer cure in 60 ℃ of heat treatment 24h; SiO
2The volume ratio of fibre bundle and polymer cure thing is 0.3; Be cut into the thin slice that thickness is 3mm then; 30 ℃ of constant temperature are down with 20%HF acid solution corrosion 30min, and the deionized water ultrasonic cleaning can obtain nano needle arrays after the drying;
Embodiment 3: the SiO2 fiber of 8 microns of diameters is obtained SiO by self-assembling technique
2Fibre bundle; In the molten resin with 120 ℃ of its immersions, fill the back cooling section that finishes, SiO then
2The volume ratio of fibre bundle and polymer cure thing is 0.6; Slice thickness is 1cm; 40 ℃ of constant temperature are down with 40%HF acid solution corrosion 10min, and the deionized water ultrasonic cleaning can obtain nano needle arrays after the drying, see Fig. 2.
Embodiment 4: the SiO2 fiber of diameter 125 micron dimensions is obtained SiO by self-assembling technique
2Fibre bundle; Put it into then in MMA (polymethyl methacrylate) solution that adds BPO, place water-bath to make polymer cure, SiO in 60 ℃ of heat treatment 24h
2The volume ratio of fibre bundle and polymer cure thing is 0.5; Be cut into the thin slice that thickness is 1cm then, corrode 120min down with 40 ℃ of constant temperature of 40%HF acid solution, the deionized water ultrasonic cleaning can obtain a micron pin array after the drying.
Embodiment 5: the silica fibre bundle of 8 microns of diameters is immersed in 120 ℃ the molten resin, fill the back cooling section that finishes, the volume ratio of silica fibre bundle and polymer cure thing is 0.3; Slice thickness is 3mm; With 80 ℃ of corrosion of 50%KOH solution 30min, the deionized water ultrasonic cleaning can obtain nano needle arrays after the drying.
Embodiment 6: basic step is same as embodiment 1, and different is that micron and sub-micron fibers are selected glass (also can select fibrous materials such as pottery or quartz for use) for use.
Embodiment 7: basic step is same as embodiment 1, and the concentration of etchant solution HF acid that different is is 0.01%, and corrosion temperature is 20 ℃, and etching time is 72 hours.
Embodiment 8: basic step is same as embodiment 1, and the concentration of etchant solution HF acid that different is is 0.1%, and corrosion temperature is 40 ℃, and etching time is 30 hours.
Embodiment 9: basic step is same as embodiment 1, and the concentration of etchant solution HF acid that different is is 5%, and corrosion temperature is 80 ℃, and etching time is 4 hours.
Embodiment 10: basic step is same as embodiment 1, and the concentration of etchant solution HF acid that different is is 20%, and corrosion temperature is 50 ℃, and etching time is 3 hours.
Embodiment 11: basic step is same as embodiment 1, and the concentration of etchant solution HF acid that different is is 40%, and corrosion temperature is 20 ℃, and etching time is 30min.
Claims (4)
1. the preparation method of micron and submicron probe arrays is characterized in that this method may further comprise the steps:
(1) by self-assembling technique assembling micron, sub-micron fibers, obtains to arrange regular fibre bundle;
(2) above-mentioned fibre bundle is filled into polymer by physics or chemical method and forms fiber and polymer complex structure, wherein the volume ratio of fibre bundle and composite construction is 0.1～0.6;
(3) above-mentioned fiber and polymer complex structure are cut into the thin slice of 1mm～1cm;
(4) above-mentioned section being put into concentration is 0.01～40% HF acid etching solution, or to put into concentration be 0.01～80% KOH etchant solution, under 10～90 ℃ of temperature, corrodes 10 seconds～72 hours, forms the needle-like array structure.
2. the preparation method of micron according to claim 1 and submicron probe arrays is characterized in that in step (1), and said micron and sub-micron fibers are silicon, or glass, or pottery, or the quartz fibre material.
3. the preparation method of micron according to claim 1 and submicron probe arrays is characterized in that in step (2), said filled polymer material is a polymethyl methacrylate, or polystyrene, or natural synthetic resin macromolecular material.
4. the preparation method of micron according to claim 1 and submicron probe arrays is characterized in that in step (2) said physics or chemical method are reactive polymeric fill method, heating and melting fill method and solution fill method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101345752A CN101143705B (en) | 2007-11-01 | 2007-11-01 | Method for preparing micrometer and submicron probe arrays |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101345752A CN101143705B (en) | 2007-11-01 | 2007-11-01 | Method for preparing micrometer and submicron probe arrays |
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| Publication Number | Publication Date |
|---|---|
| CN101143705A true CN101143705A (en) | 2008-03-19 |
| CN101143705B CN101143705B (en) | 2010-08-11 |
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| CN2007101345752A Expired - Fee Related CN101143705B (en) | 2007-11-01 | 2007-11-01 | Method for preparing micrometer and submicron probe arrays |
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| AU2573801A (en) * | 1999-11-02 | 2001-05-14 | University Of Hawaii | Method for fabricating arrays of micro-needles |
| AU8511601A (en) * | 2000-08-21 | 2002-03-04 | Cleveland Clinic Foundation | Microneedle array module and method of fabricating the same |
| CN100577349C (en) * | 2002-08-06 | 2010-01-06 | 克斯美库股份有限公司 | Clamp device |
| KR20060089314A (en) * | 2005-02-03 | 2006-08-09 | 삼성전자주식회사 | Method for fabrication of micor needle array |
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2007
- 2007-11-01 CN CN2007101345752A patent/CN101143705B/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN101143705B (en) | 2010-08-11 |
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