CN101108721A - Method of manufacturing magnetic micro-structure - Google Patents
Method of manufacturing magnetic micro-structure Download PDFInfo
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- CN101108721A CN101108721A CNA2007100421049A CN200710042104A CN101108721A CN 101108721 A CN101108721 A CN 101108721A CN A2007100421049 A CNA2007100421049 A CN A2007100421049A CN 200710042104 A CN200710042104 A CN 200710042104A CN 101108721 A CN101108721 A CN 101108721A
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Abstract
The invention relates to a fabrication method of the magnetic microstructure, which is characterized in that the invention comprises the fabrication of multilayer mould and the fabrication of the magnetic microstructure. The former is that the standard RCA cleaning process is used to clean silicon chips; multi layers of SU-8 photoresist are coated by rotating on the silicon chip surfaces and the multi layers of SU-8 mould are gotten after prebaking, photoetching, post baking and developing, and then the invention forms the magnetic microcolumn structure in the chip while molding dying the PDMS chip through directly filling the magnetic powders in the multilayer mould. Adopting the provided fabrication method can dispense with the electroplating process and fabricate the magnetic microstructure in the microfluid chip rapidly. The microstructure height is fabricated between micrometers less than ten and hundred of micrometers, which is determined by the photoresist layers of the rotating coating SU-8 and the magnetic microstructure is any one of the microcolumn, microline, microring or microcoil.
Description
Technical field
The present invention relates to the preparation method of a kind of magnetic micro-structure (as microtrabeculae, little lines, little ring, little coil etc.), belong to the Micrometer-Nanometer Processing Technology field.
Background technology
Immunomagnetic bead technique is a class new material that rises the seventies in 20th century.Magnetic bead is the microballoon that is surrounded by magnetic oxide in the ball, in magnetic microsphere expoeridium monoclonal antibody, can combine specifically with the target material that contains corresponding antigens and form new compound.This compound has the magnetic responsiveness different with other component in magnetic field, under magneticaction, this compound generation mechanics moves, thereby reaches the purpose of separating antigen.This process that is separated with other component is called immunomagnetic isolation method (Immuno-Magnetic Separation).
When the size of magnetic bead reaches nanometer scale, the small-size effect of nanometer magnetic bead will cause it the special magnetic property of macroscopic magnetization material to occur being different from.Under nanoscale, when the size of magnetic-particle was reduced to critical dimension, magnetic domain also may rearrange at normal temperatures, its coercive force vanishing, this moment, material can change paramagnetism into, even was in super-paramagnetic state, and this plays an important role in the separation of magnetic bead.When externally-applied magnetic field, magnetic bead can be magnetized and be adsorbed on the magnetic pole, and when removing externally-applied magnetic field, the magnetic of magnetic bead disappears, and magnetic bead is dispersed in the solution again, rather than flocks together.Because nanometer magnetic bead has good response to external magnetic field, therefore can be by the external magnetic field effect, utilize nanometer magnetic bead to carry out operations such as the separation of biological sample and location, thereby realize the integrated and automation of bio-sensor system.
The MEMS device obtains more and more widely application with advantages such as its volume is little, in light weight, low in energy consumption, speed is fast, sensitivity height in engineering fields such as machinery, communication, biomedicines.And along with little plane electromagnetism is made, the continuous development of immunomagnetic bead technique, electromagnetism MEMS technology has also obtained application more and more widely gradually in biomedical engineering, outstanding behaviours is driving with mangneto and separating detection, drug delivery etc. based on the albumen of magnetic bead surfaces immune response or DNA.
Although electromagnetism MEMS (micromechanics electronic system) and biomedical engineering are better compatible, in application, also there are some problems, mainly be that the fuel factor of bringing because of electrical current may be to the destruction of biological sample.Be operated in 37 ℃ as the most of enzyme require in the biologic applications, surpassing 60 ℃ will inactivation, and this has proposed the temperature control requirement to electromagnetism BioMEMS (biological micromechanics electronic system) device.On the one hand, be the current-carrying fuel factor of minimizing driving and test section electromagnetic device, and do not lose magnetic property, must increase sectional area of wire to pass through bigger electric current.And because the requirement of system's physical dimension, the lead live width can not infinitely increase, and this just makes that making the thick lead of little live width necessitates, and corresponding on technology, electroplating technology is made super thick little lines plain conductor becomes first-selection, and resistance is little, allows electric current big; On the other hand, when selecting the material of insulating barrier, microfluidic circuit and reaction microcavity etc., should select perfect heat-dissipating for use, if necessary, adopt suitable external thermal component.
Existing existing researching and proposing in fluid chip, utilize and electroplate or the method for electro-deposition, make some magnetic micro-structures, polarize by external magnetic field, produce local high-gradient magnetic field at chip internal and catch magnetic bead, although the fuel factor that this method can avoid the plane electric coil gradually to give birth to, but it still needs to adopt electroplating technology, the flow process complexity, and the height of the magnetic micro-structure of making is limited by electroplating technology, and generally all can only below 50 μ m, limit further application and the development of magnetic micro-structure in micro-fluidic chip.
Summary of the invention
The object of the invention provides a kind of fast method for preparing of magnetic micro-structure.The preparation method that is provided is a kind of electroplating technology that need not, and makes the method for magnetic micro-structure in micro-fluidic chip.Specifically, adopt polymer chip moldings formed therefrom technology then, form micro-structural with superparamagnetism and high-aspect-ratio by in multiple layers of molds, being filled into Magnaglo in advance.In described technology, adopt SU-8 to make multiple layers of molds, in the polymer chip moldings formed therefrom, finish the making of magnetic micro-structure, this chip can be used as the Magnetic Isolation in micro-fluidic chip of immune magnetic microsphere.
The making step of chip of the present invention is on silicon chip, utilize MEMS (micromechanics electronic system) fabrication techniques to go out the mould of multilayer SU-8 micro-structural, in the SU-8 mould, fill Magnaglo then, at polymer (as dimethyl silicone polymer (Polydimethylsiloxane, PDMS)) during moldings formed therefrom, Magnaglo is shifted and be cast in the micro-structural of polymer chip, thereby on micro-fluidic chip, need not electroplating technology, form magnetic micro-structure.
Specifically, the invention provides a kind ofly, make multiple layers of molds, then filling Fe in the mould of making based on SU-8 photoresist (SU-8 used herein is the SU-8 series of products of Microchem company, below all with)
3O
4Magnaglo is fitted PDMS and glass substrate material, be made into the micro-fluidic chip that includes magnetic micro-structure behind bonding, and the height of micro-structural and complex structure degree can realize by the number of plies that increases SU-8, and concrete feature is as follows:
1) making of multiple layers of molds
With standard RCA cleaning cleaning silicon chip, get rid of at silicon chip surface and to be coated with multilayer SU-8 photoresist, preceding baking, photoetching, the back baking is developed and is obtained multilayer SU-8 mould, and concrete manufacturing process comprises following step:
(a) by standard RCA cleaning, cleaning silicon chip, oven dry;
(b) the silicon chip front is got rid of and is coated with ground floor SU-8 photoresist;
(c) exposure is transferred to the microchannel figure on first mask version on the photoresist;
(d) the good substrate back baking that exposes that will expose makes to be cooled to room temperature by be exposed partial cross-linked;
(e) get rid of again on ground floor SU-8 surface and be coated with one deck SU-8 photoresist
(f) exposure is for the second time transferred to the microtrabeculae figure on second mask plate on the second layer SU-8 photoresist;
(g) curing after exposing makes the partial cross-linked of second layer SU-8 exposure, is cooled to room temperature;
(h) repeating step (e)-(g) is finished until all SU-8 structure fabrications, and the concrete number of plies can be set according to structure of making and requirement for height;
(i) multilayer SU-8 structure is developed simultaneously, rinse well, nitrogen dries up;
So promptly finish the purpose of on silicon chip, making multilayer SU-8 mould.
2) making of magnetic micro-structure
The present invention in PDMS chip moldings formed therefrom, forms magnetic microtrabeculae structure at chip internal by directly fill Magnaglo in multiple layers of molds.Utilize the method, can save electroplating technology, make magnetic micro-structure apace in micro-fluid chip, detailed process may further comprise the steps:
(a) Magnaglo is filled in the groove of multiple layers of molds;
(b) mixture of aggressiveness before the PDMS and curing agent is poured in the mould solidified;
(c) PDMS chip of taking off from mould and glass substrate are fitted, finish the bonding of chip.
The present invention has the following advantages and effect:
1. the magnetic texure cost of manufacture of integrated form is low;
2. magnetic texure manufacturing process simple and fast does not need to adopt electroplating technology, and is consistent with the mold technology of general polymerization thing micro-fluidic chip, reduced requirement and dependence to equipment;
3. the present invention can make height at several microns magnetic micro-structures to the hundreds of micron by fill the method for Magnaglo in multiple layers of molds, has avoided the restriction of electroplating technology to height.
4. magnetic micro-structure of the present invention be in microtrabeculae, little lines, little ring or the little coil any.
Description of drawings
Fig. 1 is the mask plate of ground floor SU-8 figure, makes the fluid channel structure on mould;
Fig. 2 is the mask plate of second layer SU-8 figure, makes the pairing groove of microtrabeculae structure on mould;
Fig. 3 is the manufacture craft flow process of the micro-fluidic chip that contains the magnetic microtrabeculae that provides of the embodiment of the invention 1.Specifically comprise following 9 processing steps:
(a)-RCA cleaning cleaning, drying meron
(b)-and the substrate front gets rid of and is coated with ground floor SU-8, and SU-8 2050
(c)-preceding baking post-exposure transfer microchannel figure,
(d)-and on ground floor SU-8, getting rid of and be coated with second layer SU-8, SU-8 2100
(e)-preceding baking post-exposure transfer microstructure graph
(f)-SU-8 after baking back develop, obtain multilayer SU-8 mould
(g)-in multilayer SU-8 mould, fill Fe
3O
4Powder
(h)-and the PDMS cast, curing molding
(i)-and peel off the PDMS chip from mould, burrow back and glass substrate are fitted, and finish chip manufacturing
Fig. 4 is provided by the invention with SU-8 multiple layers of molds, Fe
3O
4Powder is that the micro-fluidic chip that contains magnetic micro-structure that material is made is used for the schematic diagram that magnetic bead separates with PDMS
Fig. 5 is the application experiment result of embodiment 1 made micro-fluid chip
Fig. 6 is the cell screening chip schematic diagram that the technology identical with embodiment 1 is made
Among the figure:
1-magnetic microtrabeculae chip ground floor SU-8 mask plate
2-magnetic microtrabeculae chip second layer SU-8 mask plate
The 3-silicon chip
4-ground floor SU-8 photoresist
5-second layer SU-8 photoresist
6-Fe
3O
4Powder
7-PDMS
The 8-glass substrate
9-magnet
10-cell screening chip
The specific embodiment
Embodiment 1:
Setting forth to make in the PDMS chip below in conjunction with accompanying drawing 3 highly is that the magnetic micro-pillar array of 100 μ m is an example, the concrete technological process of this method making micro-fluidic chip is described in detail in detail.This chip can be used for example enrichment, DNA purification, protein capture, online enzyme reaction etc., and specific embodiment comprises following nine steps as shown in Figure 3:
(a) adopt standard RCA cleaning, promptly use Piranha washing lotion (H respectively
2SO
4: H
2O
2), RCA1 (NH
3H
2O:H
2O
2: H
2O), RCA2 (concentrated hydrochloric acid: H
2O
2: H
2O) strict cleaning silicon chip 3 surfaces, after nitrogen dries up, further strict drying [Fig. 3 (a)] on baking oven or hot plate;
(b) get rid of in the silicon chip front and be coated with one deck SU-8 2050 photoresists (MicroChem company provides) 4, preceding baking is solidified and is handled [Fig. 3 (b)];
(c) in litho machine, first mask plate 1 aimed at substrate, ultraviolet exposure, the microchannel figure of micro-fluid chip on the mask plate is transferred on the ground floor SU-8 photoresist, curing after exposing, SU-8 further solidifies, and make be exposed partial cross-linked, be cooled to room temperature [Fig. 3 (c)];
(d) get rid of on ground floor SU-8 surface again and be coated with SU-8 2100 photoresists 5 that one deck MicroChem company provides, preceding baking is solidified and is handled [Fig. 3 (d)];
(e) in litho machine second mask plate 2 aimed at substrate, ultraviolet exposure is transferred to the microtrabeculae figure on the mask plate on the second layer SU-8 photoresist, curing after exposing, second layer SU-8 photoresist solidifies, and exposure partial cross-linked is cooled to room temperature [Fig. 3 (e)];
(f) with SU-8 developer solution (MicroChem company provides) two-layer SU-8 structure is developed simultaneously, the isopropyl alcohol flushing, deionized water rinsing, nitrogen dry up [Fig. 3 (f)];
(g) with Fe
3O
4Powder 6 is poured in the groove of SU-8 double stack mold, brushes away the unnecessary Fe of die surface with soft brush
3O
4Powder [Fig. 3 (g)];
(h) be pumped to no steam bubble after aggressiveness before the PDMS and curing agent are mixed in 10: 1 ratio, then this mixture 7 poured in the mould of filling Magnaglo, put into 65 ℃ of baking ovens, cure 1 hour [Fig. 3 (h)];
(i) PDMS after will solidifying takes off from mould, and punching back and glass substrate 8 are fitted, and transfers to [Fig. 3 (i)] that placement 15min in 80 ℃ of baking ovens finishes bonding then.
The application of present embodiment:
Magnetic bead is fixed on magnetic bead surfaces with the respective ligand (probe, antigen, antibody etc.) of target sample behind overactivation.With micro-injection pump magnetic bead solution is injected microchannel.Be sidelong at chip one and put magnet.Sample solution is fed in the microchannel.Behind the reaction certain hour, targeted biological specimen is imported the cleaning washing lotion and washes away impurity etc. by the magnetic capture around the magnetic microtrabeculae.Fig. 5 is the experimental result (magnetic bead surfaces is sheep anti-mouse igg fixedly) of catching the mouse-anti human IgG albumen of FITC mark in the solution.
Embodiment 2:
The cell screening chip (Fig. 6) of little linear that is magnetic, basic processing technology is with the magnetic micro-pillar array chip among the embodiment 1.
Present embodiment is used:
Mark magnetic bead on target cell, sample solution is fed in the microchannel, be sidelong at chip one and put magnet, after the cell that is marked with magnetic bead is adsorbed on around little lines substantially, remove magnetic field then, continue to feed solution, being marked with the cell of magnetic bead and the cell of unmarked magnetic bead can flow out from obstructed outlet respectively, finishes cell screening.
Claims (9)
1. the preparation method of a magnetic micro-structure is characterized in that adopting polymer chip moldings formed therefrom technology then by be filled into Magnaglo in advance in multiple layers of molds, forms the magnetic micro-structure with superparamagnetism and high-aspect-ratio; In described technology, adopt SU-8 to make multiple layers of molds, in the polymer chip moldings formed therefrom, finish the making of magnetic micro-structure.
2. by the preparation method of the described magnetic micro-structure of claim 1, it is characterized in that preparation method comprises:
(A) making of multiple layers of molds
(a) by standard RCA cleaning, cleaning silicon chip, oven dry;
(b) the silicon chip front is got rid of and is coated with ground floor SU-8 photoresist;
(c) exposure is transferred to the microchannel figure on first mask version on the photoresist;
(d) the good substrate back baking that exposes that will expose makes to be cooled to room temperature by be exposed partial cross-linked;
(e) get rid of again on ground floor SU-8 surface and be coated with one deck SU-8 photoresist;
(f) exposure is for the second time transferred to the microtrabeculae figure on second mask plate on the second layer SU-8 photoresist;
(g) curing after exposing makes the partial cross-linked of second layer SU-8 exposure, is cooled to room temperature;
(h) repeating step (e)-(g) is finished until all SU-8 structure fabrications;
(i) multilayer SU-8 structure is developed simultaneously, rinse well, nitrogen dries up;
(B) making of magnetic micro-structure
(a) Magnaglo is filled in the groove of multiple layers of molds;
(b) mixture of aggressiveness before the dimethyl silicone polymer and curing agent is poured in the mould solidified;
(c) polydimethylsiloxanechip chip of taking off from mould and glass substrate are fitted, finish the bonding of chip.
3. by the preparation method of the described magnetic micro-structure of claim 2, it is characterized in that described SU-8 photoresist is the series of products that provided by MicroChem company.
4. by the preparation method of claim 1 or 2 described magnetic micro-structures, it is characterized in that described magnetic micro-structure is microtrabeculae, little lines, little ring or little coil.
5. by the preparation method of claim 1 or 2 described magnetic micro-structures, the height that it is characterized in that described magnetic micro-structure at nine microns to the hundreds of micron; Complexity realizes with the number of plies of highly passing through increase SU-8.
6. by the preparation method of the described magnetic micro-structure of claim 2, it is characterized in that described magnetic micro-structure is made the presoma of (b) use in (B) and the weight ratio of curing agent is 10: 1,65 ℃ of solidification temperatures, the time is 1 hour.
7. by the preparation method of the described magnetic micro-structure of claim 2, it is characterized in that solidifying the back and close with the glass substrate card from the polydimethylsiloxanechip chip punching back that mould is taken off.
8. by the preparation method of claim 2 or 7 described magnetic micro-structures, it is characterized in that transferring to after dimethyl silicone polymer and glass substrate are fitted that placement 15min finishes bonding in 80 ℃ of baking ovens.
9. by the preparation method of claim 1 or 2 described magnetic micro-structures, it is characterized in that the magnetic micro-structure chip of made is used for the Magnetic Isolation of immune magnetic microsphere.
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| CNA2007100421049A CN101108721A (en) | 2007-06-15 | 2007-06-15 | Method of manufacturing magnetic micro-structure |
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| CNA2007100421049A CN101108721A (en) | 2007-06-15 | 2007-06-15 | Method of manufacturing magnetic micro-structure |
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| CN101530775B (en) * | 2009-03-03 | 2011-06-15 | 南京大学 | Micro-fluidic apparatus integrated with PDMS film, manufacturing method and application thereof |
| CN102249182A (en) * | 2011-04-27 | 2011-11-23 | 中国科学院理化技术研究所 | Method for preparing magnetic/polymer composite material three-dimensional micro/nano device capable of being remotely magnetically driven |
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| CN110668398A (en) * | 2019-10-16 | 2020-01-10 | 武汉大学 | Preparation method and application of extremely progressive rigid-flexible gradient micro-column structure of bionic gecko |
| CN111939992A (en) * | 2020-07-23 | 2020-11-17 | 侯双 | Preparation method of micro-fluidic system for capturing and enriching circulating tumor cells and micro-fluidic device |
| CN112268636B (en) * | 2020-09-22 | 2022-06-03 | 北京航空航天大学 | Liquid temperature sensing system based on whispering gallery mode spherical optical microcavity |
| CN112268636A (en) * | 2020-09-22 | 2021-01-26 | 北京航空航天大学 | Liquid temperature sensing system based on whispering gallery mode spherical optical microcavity |
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