CN100465621C - Micro-fluid control chip with surface enhanced Raman spectral active substrate and producing method thereof - Google Patents
Micro-fluid control chip with surface enhanced Raman spectral active substrate and producing method thereof Download PDFInfo
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- CN100465621C CN100465621C CNB2006100087674A CN200610008767A CN100465621C CN 100465621 C CN100465621 C CN 100465621C CN B2006100087674 A CNB2006100087674 A CN B2006100087674A CN 200610008767 A CN200610008767 A CN 200610008767A CN 100465621 C CN100465621 C CN 100465621C
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Abstract
The present invention relates to a microfluidic chip, in particular, it relates to a microfluidic chip with surface enhanced Raman spectrum (SERS) active substrate and its preparation method. On the microfluidic chip, at least a microchannel is set, on the total or partial inner wall surface of said microchannel is set a layer of rough metal film with SERS activity. Besides, said invention also provides the concrete steps for preparing said microfluidic chip.
Description
Technical field
The present invention relates to a kind of micro-fluidic chip, particularly relate to a kind of micro-fluidic chip at the bottom of the Surface enhanced raman spectroscopy active group and preparation method thereof that has.
Background technology
Micro-fluidic chip is minisize reaction or the analytic system that a class has the microchannel network, usually by glass or macromolecular material, as polymethylmethacrylate (PMMA), polycarbonate (PC) and dimethyl silicone polymer (PDMS) etc., be prepared from through technological processes such as over etching or plastic compression and bondings.Be characterized in having the microchannel of diameter below 200 μ m.Because size is little, micro-fluidic chip has that use cost is low, the reagent consumption is little, rapidly and efficiently, advantage such as easy of integration and robotization, be widely used in fields such as biomedical and environment pharmacy.But because the size of micro-fluidic chip is little, this has also caused the difficulty that detects.Therefore, detection system is the key component of decision micro-fluidic chip applicability.Micro-fluidic chip uses more detection method that laser-induced fluorescence (LIF) (LIF), uv absorption, galvanochemistry and mass spectrum etc. are arranged at present, and wherein LIF's is most widely used.But do not modify because most samples itself do not have fluorescence and are difficult to carry out fluorescence, its range of application is comparatively narrow, and can't obtain the detailed structural information of sample.Uv absorption is because light path is short, and poor sensitivity, quantity of information are not abundant yet, thereby use less.Though Electrochemical Detection is integrated easily, cost is low, and range of application is wideless, and quantity of information very little.The mass spectrum quantity of information is abundant, but can't carry out the detection of original position.Raman spectroscopy can obtain group and chemical bond and the microenvironment information to sample structure influence from molecular level, and test sample and obtain its finger-print, and its signal in real time can not disturbed by water, so is particularly suitable for the detection of biomolecule.But Raman signal especially a little less than, need strengthen by certain methods during application, normally used Enhancement Method has two classes, one class strengthens Raman for resonance, promptly excite, testing molecule is resonated, thereby obtain strong Raman signal with laser with molecules detected absorbing light co-wavelength, these class methods are had relatively high expectations to LASER Light Source, and once can only be used to detect the molecule of same absorbent.The method of another kind of enhancing Raman signal then is to use coarse metal surface, i.e. Surface enhanced raman spectroscopy (SERS).In system to be detected, add coarse coin family metal (as gold, silver or copper) or its nano particle, can improve the signal of Raman spectrum greatly.Therefore, preparation has the precondition that the rough surface that strengthens the Raman spectrum activity is realization SERS detection.
The main both at home and abroad at present rough surface that preparation has enhancing Raman spectrum activity in micro-fluidic chip by the following method: (1) feeds the aaerosol solution of coin family metal nanoparticle in micro-fluidic chip, as Taehan Park (Taehan Park, Lab Chip, 2005,5:437-442) Bao Dao the potpourri with silver sol and two kinds of oligonucleotides pours into raceway groove, detects after the mixing.The advantage of this method is to obtain fresh surface, but difficulty is all compared in the preparation of even metal nano particle and storage, and is easy to assemble the sedimentation instability, and range of application is very limited; (2) use complicated electronic technology to prepare coarse chip, re-use the extremely thin metal level of electron beam transpiration.As (Gang L Liu, et al, Appl.Phys.Lett. such as Gang L.Liu, 2005,87,074101) the local PDMS that has hemispherical projection of the use photoetching technique of report preparation, deposited by electron beam evaporation local deposits 20nm silver film then obtains the micro-fluidic chip at the bottom of the tool SERS active group.This method needs expensive equipment and numerous and diverse step.
In sum, above listed method or easy sedimentation instability, or complex process, cost is higher.
Summary of the invention
The objective of the invention is to provides micro-fluidic chip of a kind of textured metal film at the bottom of partly or entirely having the SERS active group and preparation method thereof at existing problem at the bottom of the active group of micro-fluidic chip use surface-enhanced Raman detection needs.The technical solution used in the present invention is sputter or an assembling coin family (gold on all or part of inwall of level and smooth micro-fluidic chip passage (raceway groove or pipeline), silver, copper) film, by galvanochemistry or chemical method roughening, preparation has the micro-fluidic chip at the bottom of the Surface enhanced raman spectroscopy active group again.
Of the present invention have micro-fluidic chip at the bottom of the Surface enhanced raman spectroscopy active group for to be provided with at least one microchannel on micro-fluidic chip, and all or part of inner wall surface in the microchannel has one deck to have the textured metal film of Surface enhanced raman spectroscopy activity.
The material of described chip is a glass, dimethyl silicone polymer (PDMS) or polymethyl acrylate (PMMA) etc.; Metal is a gold, silver or copper etc.; Described microchannel is little raceway groove or microchannel, and the diameter of microchannel is less than 200 μ m.Can be provided with at least 2 liquid storage tanks on chip, liquid storage tank communicates with the microchannel.Described film is fine and close solid film or metallic particles single thin film or the multilayer film that are assembled into by metal nanoparticle.Described coarse be the roughness of metal nanoparticle itself or through the roughness of chemistry or electrochemical treatment.
Described film is a gold, the continuous homogeneous film of silver or copper; Described film is a gold, the film that silver or copper nano-particle are assembled into.Described gold, the diameter of the nano particle of silver or copper are 5～500nm.
Described Surface enhanced raman spectroscopy is active to be to make the Raman signal intensity of surface adsorption species increase more than 10 times than smooth surface.
The preparation method of the micro-fluidic chip of the textured metal film at the bottom of the SERS of the having active group of the present invention the steps include:
1) utilizes technology such as MEMS or Laser Processing, machined grooves on glass or macromolecular material thin slice;
2) in all or part of zone of groove, the method by physical evaporation, sputter or chemogenic deposit prepares coin family metallic film in conjunction with mask technique, and described coin family metal is selected from gold, silver or copper;
3) pass through chemical method or electrochemical method with coin family metallic film roughening;
4) will carry out thermal bonding or plasma-activated bonding with the thin slice of groove and the thin slice in hole with holes, obtain having the micro-fluidic chip of complete airtight little raceway groove.
Described step 3) and 4) poly-order can be put upside down two steps.
As use then step 2 of metal nanoparticle) and 3) be combined into a step: in all or part of zone of groove, prepare the component film of coin family metal nanoparticle in conjunction with mask technique by the method for chemistry or physics assembling.Described metal nanoparticle is that diameter is the metallic particles of 1～1000nm.
The chemical method of described textured metal film is as follows: add the nitric acid of 0.1～10mol/L in the micro-fluidic chip passage of metallic film is arranged, behind immersion 1～60min acid solution is rinsed well.
The electrochemical process of described textured metal film is as follows: for silver-colored film, in the KCl of 0.1～10mol/L solution, at first CONTROLLED POTENTIAL is at-0.25V, step is to 0.18V then, and after stopping 5～60s under this current potential, get back to-0.25V with slower speed, all be reduced, obtain flaxen villous surface at last up to the surface.For gold thin film, then be swept to 1.25V, stop 1～30s then from-0.3V with the sweep velocity of 0.1～10V/s, sweep velocity with 0.1～10V/s is swept to-0.3V again, stop 1～100s, circulate 1～50 time, obtain dark-brown coarse gold surface with high SERS activity.As for the copper film, in the KCl of 0.1～10mol/L solution, after carrying out 3～60 steps between current potential-0.4V to 0.4V, under-0.4V current potential, take out electrode and can obtain brown active surface.
Use the method at the bottom of surface-enhanced Raman detects the active group that needs to compare with existing at micro-fluidic chip, equipment required for the present invention is simple, and is easy and simple to handle, active high at the bottom of the prepared SERS active group, can obtain very strong Raman signal.
Description of drawings
Fig. 1 is the sem photograph of the silver-colored film of embodiment 1 preparation.
Fig. 2 is the photo in kind of the PDMS micro-fluidic chip with the active coarse silver surface of SERS of embodiment 1 preparation.
Fig. 3 detects the SERS spectrogram (be respectively the SERS signal of aniline and benzaldehyde and both reaction product, if there is not silverskin, then can not detect the SERS signal) that obtains for the coarse silverskin in three places of the PDMS micro-fluidic chip of embodiment 1 preparation.
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
Embodiment 1
The PDMS mask sheet that will be equipped with 3 holes (aperture is 2mm) is attached on the glass sheet that standard cleaning crosses.Use JS2S-80D type sputtering unit (Beijing wound Wei Na company produces), adopt direct current rotatable sputtering pattern, successively with the power sputtered titanium film 7min of 150W, the power sputtering silver film 15min of 160W.Immerse in the 1mol/L KCl solution, it is coarse with CHI631B electrochemical workstation (Shanghai occasion China) the silver-colored film in surface to be carried out electrochemical redox (ORC), detailed process is: at first constant potential is at-0.25V5s, step is to 0.18V then, stop 10s at this current potential, speed with 0.01V/s is slowly got back to-0.25V, and abundant reductase 12 0s under-0.25V all is reduced to faint yellow fine hair shape up to the surface.Take mask off, obtain the glass sheet that the part has rough base.On the PDMS cover plate, process 3 liquid storage tanks with card punch; Use CO
2-50F laser marking machine (source company of Beijing wound section product) machined grooves.Cover plate and the glass sheet that has rough base are placed in the two-tube equipment for burning-off photoresist by plasma vacuum chamber of GP08-2/QJ type, and 1500V is bombardment 15s down, and cover plate and glass sheet surface are fully activated.PDMS cover plate and glass sheet are fit together, leave standstill 5min, promptly obtain a micro-fluidic chip at the bottom of having the Surface enhanced raman spectroscopy active group behind the bonding.
The sem photograph of the silver-colored film that embodiment 1 is prepared is referring to Fig. 1, the prepared photo in kind of the PDMS micro-fluidic chip with the active coarse silver surface of SERS is referring to Fig. 2, the coarse silverskin in three places of prepared PDMS micro-fluidic chip detects the SERS spectrogram that obtains and (is respectively the SERS signal of aniline and benzaldehyde and both reaction product referring to Fig. 3, if there is not silverskin, then can not detect the SERS signal).
Embodiment 2
The PDMS mask sheet that will be equipped with 3 holes (aperture is 2mm) is attached on the fresh PDMS cover plate of peeling off.Adopt direct current rotatable sputtering pattern, successively with the power sputtered titanium film 7min of 150W, the power sputter gold thin film 10min of 150W.Immerse in the 0.1mol/L KCl solution, it is coarse that surperficial gold thin film is carried out ORC, detailed process: at first constant potential is at-0.3V, then with the speed step of 1.0V/s to 1.2V, and stop 1.5s at this current potential, and get back to-0.3V with the speed of 0.5V/s, fully reduce 30s down at-0.3V.With after the said process circulation 20 times under-0.3V current potential taking-up can obtain dark-brown surface with high SERS activity.Take mask off, obtain the PDMS substrate that the part has coarse gold substrate.On the PDMS cover plate, process 3 liquid storage tanks with card punch; Use the laser marking machined recess.PDMS cover plate and the PDMS substrate that has rough base are placed in the equipment for burning-off photoresist by plasma vacuum chamber, and 1500V is bombardment 15s down, and PDMS cover plate and PDMS substrate surface are fully activated.PDMS cover plate and PDMS substrate are fit together, leave standstill 5min, promptly obtain a micro-fluidic chip at the bottom of having the Surface enhanced raman spectroscopy active group behind the bonding.
Embodiment 3
The PDMS mask sheet that will be equipped with 3 holes (aperture is 2mm) is attached on the glass sheet that standard cleaning crosses.Adopt direct current rotatable sputtering pattern, successively with the power sputtered titanium film 7min of 150W, the power sputter copper film 10min of 150W.Immerse in the 0.1mol/L KCl solution, taking-up can obtain brown SERS active surface under-0.4V current potential after step between current potential-0.4V to 0.4V 5 times.Take mask off, obtain the glass substrate that the part has the roughened copper substrate.Processing 3 liquid storage tanks of processing on the reeded cover glass by the wet etching method with laser marking machine.Put into high temperature furnace after cover plate and the glass substrate that has rough base fitted, speed with 10 ℃/min is warming up to 620 ℃, insulation 3.5h again with the cooling of the speed of 10 ℃/min, promptly obtains a micro-fluidic chip at the bottom of having the Surface enhanced raman spectroscopy active group.
Embodiment 4～6
The PDMS mask sheet that will be equipped with 3 holes (aperture is 2mm) is attached on the glass sheet that standard cleaning crosses.Adopt direct current rotatable sputtering pattern, successively with the power sputtered titanium film 7min of 150W, the coin family metal (gold, silver, copper) that certain power and time sputter are required.Immerse in the certain density salpeter solution and react certain hour, take out, wash (specifically as shown in table 1) with 3 water loggings.Take mask off, obtain the glass sheet at the bottom of the part has the SERS active group.On the PDMS cover plate, process sample holes with card punch; Use CO
2-50F laser marking machine (source company of Beijing wound section product) machined grooves.Cover plate and the glass sheet that has rough base are placed in the two-tube equipment for burning-off photoresist by plasma vacuum chamber of GP08-2/QJ type, and 1500V is bombardment 15s down, and cover plate and glass sheet surface are fully activated.PDMS cover plate and glass sheet are fit together, leave standstill 5min, promptly obtain a micro-fluidic chip at the bottom of having the Surface enhanced raman spectroscopy active group behind the bonding.
Table 1
| Metal species | Sputtering power (W) | Sputtering time (min) | Concentration of nitric acid (mol/L) | Reaction time (min) |
| Silver | 160 | 15 | 5 | 7 |
| Gold | 150 | 10 | 7 | 8 |
| Copper | 150 | 10 | 2 | 10 |
Embodiment 7
The PDMS mask sheet that will be equipped with 3 holes (aperture is 2mm) is attached on the PMMA.5h in the polylysine aqueous solution of immersion 5% takes out with putting into silver sol self assembly 12h after the high purity water flushing, takes out with the high purity water flushing again, and nitrogen dries up, Nano silver grain of its surface formation one deck purple.Take mask off, obtain the PMMA substrate that partial groups is equipped with Nano silver grain.PMMA cover plate with laser marking machined recess and liquid storage tank is cleaned 5min in deionized water for ultrasonic, the ultrapure water flushing, dry up, put into laminating machine after fitting with PMMA substrate (the ultrapure water flushing dries up) again, apply suitable pressure, under 90 ℃, constant temperature and pressure 10min takes out after being cooled to room temperature, promptly obtains a micro-fluidic chip at the bottom of having the Surface enhanced raman spectroscopy active group.
Embodiment 8
The PDMS mask sheet that will be equipped with 3 holes (aperture is 2mm) is attached on the glass sheet that standard cleaning crosses.The glass sheet that will have groove immerses coupling molecule solution (3-sulfydryl propyl group-trimethyl silane: three water: isopropyl alcohol=1:1:40) take out behind the middle 24h, clean with isopropyl alcohol, three water respectively, nitrogen dries up, 110 ℃ of insulation 30min, taking-up is ultrasonic 5min in three water, and nitrogen dries up.Put into aurosol, take out after leaving standstill 12h, ultrasonic 5min in three water, nitrogen dries up.All the other steps are similar to Example 1.
Claims (9)
1, has micro-fluidic chip at the bottom of the Surface enhanced raman spectroscopy active group, it is characterized in that being provided with on micro-fluidic chip at least one microchannel, all or part of inner wall surface in the microchannel has one deck to have the textured metal film of Surface enhanced raman spectroscopy activity; Described coarse be the roughness of metal nanoparticle itself or through the roughness of chemistry or electrochemical treatment.
2, the micro-fluidic chip that has at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that described chip is a glass-chip, polydimethylsiloxanechip chip or polymethyl acrylate chip.
3, the micro-fluidic chip that has at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that described metal is gold, silver or copper.
4, the micro-fluidic chip that has at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that described microchannel is little raceway groove or microchannel, and the diameter of microchannel is less than 200 μ m.
5, the micro-fluidic chip that has at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that being provided with at least 2 liquid storage tanks on chip, and liquid storage tank communicates with the microchannel.
6, the micro-fluidic chip that has at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that described film is fine and close metal solid film or single-layer metal particle film or the multiple layer metal particle film that is assembled into by metal nanoparticle.
7, the micro-fluidic chip that has at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that described film is:
Gold, the continuous homogeneous film of silver or copper; Or
Gold, the film that silver or copper nano-particle are assembled into, described gold, the diameter of the nano particle of silver or copper are 5～500nm.
8, the preparation method with the micro-fluidic chip at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that may further comprise the steps:
1) utilizes MEMS or laser processing technology, machined grooves on glass or macromolecular material thin slice;
2) in all or part of zone of groove, the method by physical evaporation, sputter or chemogenic deposit prepares coin family metallic film in conjunction with mask technique, and described coin family metal is selected from gold, silver or copper;
3) pass through chemical method or electrochemical method with coin family metallic film roughening;
4) will carry out thermal bonding or plasma-activated bonding with the thin slice of groove and the thin slice in hole with holes, obtain having the micro-fluidic chip of complete airtight little raceway groove.
9, the preparation method with the micro-fluidic chip at the bottom of the Surface enhanced raman spectroscopy active group as claimed in claim 1 is characterized in that may further comprise the steps:
1) utilizes MEMS or laser processing technology, machined grooves on glass or macromolecular material thin slice;
2) in all or part of zone of groove, the method by the assembling of chemistry or physics prepares the component film of coin family metal nanoparticle in conjunction with mask technique, and described metal nanoparticle is that diameter is the metallic particles of 1～1000nm;
3) will carry out thermal bonding or plasma-activated bonding with the thin slice of groove and the thin slice in hole with holes, obtain having the micro-fluidic chip of complete airtight little raceway groove.
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| CN102285629B (en) * | 2011-05-05 | 2014-03-26 | 厦门大学 | Preparation method for surface-enhanced Raman spectrum active substrate |
| CN102788777B (en) * | 2011-05-19 | 2015-08-19 | 北京大学 | Micro-fluidic Surface enhanced raman spectroscopy detection means and preparation method thereof and application |
| CN102877094A (en) * | 2011-07-15 | 2013-01-16 | 中国科学院合肥物质科学研究院 | Ordered hole array with gold-nanoparticle-based micro-nanometer composite structure and preparation method for ordered hole array |
| CN103389297A (en) * | 2013-08-07 | 2013-11-13 | 苏州扬清芯片科技有限公司 | Quick preparation method of SERS (surface-enhanced Raman scattering) active substrate with inverted cone |
| CN103575720B (en) * | 2013-11-05 | 2015-11-18 | 中国科学院城市环境研究所 | There is surface enhanced Raman substrate of pliability and light transmission and preparation method thereof |
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| CN104655608B (en) * | 2015-03-12 | 2017-03-22 | 首都师范大学 | System and method for surface enhancement Raman detection |
| CN105352935B (en) * | 2015-11-16 | 2018-06-12 | 中北大学 | Controllable layer assembly nano-particle SERS substrates of a kind of performance and preparation method thereof |
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