CN203929645U - Micro-fluidic surface-enhanced Raman test chip - Google Patents

Micro-fluidic surface-enhanced Raman test chip Download PDF

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Publication number
CN203929645U
CN203929645U CN201420232065.4U CN201420232065U CN203929645U CN 203929645 U CN203929645 U CN 203929645U CN 201420232065 U CN201420232065 U CN 201420232065U CN 203929645 U CN203929645 U CN 203929645U
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China
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hard substrate
metal
metal column
test chip
column
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CN201420232065.4U
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Chinese (zh)
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尹彦
叶通
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中国科学院物理研究所
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Abstract

The utility model discloses a kind of micro-fluidic surface-enhanced Raman test chip.This chip comprises: the first hard substrate; The second hard substrate, arranges with the first hard substrate opposing parallel; And the metal level being formed by the metal material with SERS activity, be arranged between the first hard substrate and the second hard substrate, and extend to the second hard substrate by the first hard substrate; Wherein, metal level comprises the metal column group who is formed by multiple metal columns, each metal column extends along the thickness direction from the first hard substrate to the second hard substrate, and between any two adjacent metal columns, forms for treating the fluid channel that fluid measured is passed through in metal column group.The utility model arranges the metal column group with three-dimensional gain cylinder by the detection zone at test chip, greatly increased the contact area of detection zone and testing molecule, has significantly promoted gain coefficient and detection sensitivity.

Description

Micro-fluidic surface-enhanced Raman test chip
Technical field
The utility model relates to the Raman detection technical field of microfluid, particularly relates to a kind of micro-fluidic surface-enhanced Raman test chip.
Background technology
Surface enhanced Raman technique (Surface Enhanced Raman Scattering, SERS) refers to that it can make Raman signal strengthen 10 by the technology of the Raman signal of roughened metal surface or metal Nano structure enhancing absorption molecule 10~10 11doubly, this means that it can detect individual molecule.Due to its sensitivity with superelevation, SERS technology has been widely used in the fields such as chemistry, biology, medical science.
Micro-fluidic chip technology (Microfluidic Chip, MC) refer to the operating units such as sample preparation related in the fields such as chemistry, biology and medical science, reaction, separation and detection are integrated on the chip of micro-meter scale, by microchannel network consisting, run through whole system with controlled fluid, thereby replace the technology of the various functions of conventional biomedicine or chemical laboratory.Micro-fluidic chip is also known as chip lab (Lab on achip), and it is analyzed in can carrying out a hundreds of sample within even shorter time a few minutes.Compared with traditional analytical approach, it has that analysis efficiency is high, reagent consumption is little and volume is little is easy to the advantages such as integrated.
Integrated and microminiaturized along with micro-fluidic chip, the volume of the microfluid of its processing reduces gradually, from nL (10 -9l) to pL (10 -12l) even arrive fL (10 -15l), so the volume of trace makes being detected as a difficult problem of sample molecule.Just can solve this difficult problem but there is supersensitive SERS technology, so the micro-fluidic chip based on SERS detection technique arises at the historic moment.
Current this chip is still in conceptual phase, and also ununified name, is generally called micro-fluidic surface-enhanced Raman test chip (Microfluidic SERS Chip, MSC).The combination of SERS technology and MC technology makes the defect of himself also obtain overcoming, than traditional SERS technology, MSC technology has following several large advantage: 1) overcome the problem of tested molecule in gain media surface distributed inequality, greatly improved the reliability of data and the repeatability of test; 2) solve the problem that local heats, avoided molecule decomposes in test process; 3, can be used for the real-time SERS monitoring of fluid.
At present, micro-fluidic surface-enhanced Raman test chip roughly can be divided into two kinds: particle type chip and base type chip.Particle type chip refers to the chip that utilizes the SERS nano-particle reinforcement Raman signal disperseing.As the people such as Taylor have prepared the MSC of particle type using nano-Ag particles as detecting reagent.Because the preparation of particle type chip is easy, the mixing raceway groove that only need to design the entrance raceway groove of nano particle reagent and mix with sample solution, so it also becomes the method that research group of various countries generally adopts.Although prepared by particle type chip simple, with low cost, it also has self shortcoming, for example: 1) in test process, nano particle is constantly loss along with flowing of liquid, has caused so great waste; 2) it must design bending mixing raceway groove impel solution to be measured and detect reagent fully mix, so just extended the test duration, reduced efficiency; 3) because the easy sedimentation of nano particle and reunion, so it must preparation at once before test, or through chemical modification to keep disperse state.
Base type chip refers to the chip that utilizes fixing SERS substrate to strengthen Raman signal, utilize the micro-processing methods such as photoetching, deep reactive ion bundle etching, chemical vapor deposition and hot evaporation to prepare the MSC taking nano column array as SERS substrate as people such as Mao, its gain coefficient can reach 5.2 × 10 5, and the SERS base type chip of preparing has good consistance in the time of test.Weak point is, this base type chip is mainly taking the top end face of nano-pillar as gain surface, and this makes the lifting of its gain coefficient limited, and complicated process of preparation, with high costs, is unfavorable for large-scale production.
In sum, although the preparation process of base type chip is more complex, its test signal consistance is good and use simple and conveniently, does not have the problems referred to above of particle type chip.Therefore, how to improve promoting its gain coefficient based on base type chip and may become the main flow of future market.
Utility model content
The purpose of this utility model aims to provide a kind of micro-fluidic surface-enhanced Raman test chip, the detection zone of this test chip arranges the metal column group with three-dimensional gain face structure, increase and the contact surface area of testing molecule, thereby significantly promoted the sensitivity of gain coefficient and detection.
According to an aspect of the present utility model, a kind of micro-fluidic surface-enhanced Raman test chip is provided, comprising: the first hard substrate; The second hard substrate, arranges with the first hard substrate opposing parallel; And the metal level being formed by the metal material with SERS activity, be arranged between the first hard substrate and the second hard substrate, and extend to the second hard substrate by the first hard substrate; Wherein, metal level comprises the metal column group who is formed by multiple metal columns, each metal column extends along the thickness direction from the first hard substrate to the second hard substrate, and between any two adjacent metal columns, forms for treating the fluid channel that fluid measured is passed through in metal column group.
Further, metal column is being of a size of nanometer scale perpendicular to the cross section on its bearing of trend.
Further, the first hard substrate is made up of the material of transparent and electrically conductive, and metal column group extends towards the thickness direction of the second hard substrate since the first hard substrate.
Further, metal level also comprises the metal covering film between metal column group and the second hard substrate, and metal covering film and metal column group are integrally formed.
Further, also comprise the first tack coat being separately positioned between the first hard substrate and metal level, and be arranged on the second tack coat between the second hard substrate and metal level; The first tack coat is formed by electrically conducting transparent cementing agent.
Further, metal column group is perpendicular to the first hard substrate and the second hard substrate setting.
Further, in metal column group, the vertical height of each metal column is 3 μ m~12 μ m, is preferably 6 μ m.
Further, the density of metal column is 1 X 10 8individual/cm 2~6 X 10 8individual/cm 2, preferably, when metal column is column structure, the diameter of metal column is 10nm~400nm.
Application the technical solution of the utility model, the metal column group with three-dimensional gain cylinder is set by the detection zone at micro-fluidic surface-enhanced Raman test chip, this structure is with respect to the gain surface structure of traditional base type, greatly increase the contact area of detection zone and testing molecule, thereby significantly promoted gain coefficient and detection sensitivity.The utility model can also design, adjust according to the diameter of each metal column in set metal column group, metal column group's cycle, and then met the requirement of different measuring condition, had the advantages such as the high conformity of detection and cost are low.Preparation method provided by the utility model is simple to operate.
According to the detailed description to the utility model specific embodiment by reference to the accompanying drawings below, those skilled in the art will understand above-mentioned and other objects, advantage and feature of the present utility model more.
Brief description of the drawings
Hereinafter describe specific embodiments more of the present utility model in detail in exemplary and nonrestrictive mode with reference to the accompanying drawings.In accompanying drawing, identical Reference numeral has indicated same or similar parts or part.It should be appreciated by those skilled in the art that these accompanying drawings may not draw in proportion.In accompanying drawing:
Fig. 1 is according to the structural representation of the micro-fluidic surface-enhanced Raman test chip of a kind of embodiment of the utility model;
Fig. 2 is the plating view of preparing metal column group according to the employing electrochemical deposition method of a kind of embodiment of the utility model; And
Fig. 3 is according to the schematic flow sheet of the micro-fluidic surface-enhanced Raman test chip of the preparation of a kind of embodiment of the utility model;
Fig. 4 is according to the realistic application conditions schematic diagram of the micro-fluidic surface-enhanced Raman test chip of a kind of embodiment of the utility model.
Embodiment
In order to solve gain coefficient and the low problem of detection sensitivity of base type test chip of the prior art, the utility model provides a kind of micro-fluidic surface-enhanced Raman test chip.As shown in Figure 1, this test chip comprises the first hard substrate 20, the second hard substrate 30 and the metal level 40 being formed by the metal material with SERS activity.The second hard substrate 30 and the first hard substrate 20 opposing parallel settings.Metal level 40 is arranged between the first hard substrate 20 and the second hard substrate 30, and extends to the second hard substrate 30 by the first hard substrate 20.Metal level 40 can comprise the metal column group who is formed by multiple metal columns 12, each metal column 12 extends along the thickness direction from the first hard substrate 20 to second hard substrates 30, and between any two adjacent metal columns 12, forms for treating the fluid channel 13 that fluid measured is passed through in metal column group.
The utility model is by arranging metal column group structure in detection zone, and form fluid channel 13 between any two adjacent metal columns 12, in the time detecting, greatly increase by the contact area between test substance and the metal column group surface of fluid channel 13, and then significantly promoted gain coefficient and detection sensitivity.
In an embodiment of the present utility model, as shown in Figure 1, metal level 40, except comprising the metal column group who is formed by metal column 12, also comprises the metal covering film 14 between metal column group and the second hard substrate 30.Wherein metal covering film 14 is integrally formed with metal column group.By integrated metal covering film 14 is set, metal column 12 is connected with the second hard substrate 30 by metal covering film 14, increase metal column group's steadiness; Because integrated metal covering film 14 exists, when test substance flows through from fluid channel 13, also can there is contact area with metal covering film 14 simultaneously, further promote gain coefficient and detection sensitivity while detection.
In a unshowned embodiment of the present utility model, metal level 40 can only comprise the metal column group who is formed by metal column 12.
Metal column 12 can be nanometer scale in the size in the cross section perpendicular on its bearing of trend.In an embodiment of the present utility model, in metal column group, the vertical height of each metal column 12 is 3 μ m~12 μ m, and this height is determined by the thickness of template.The height of metal column 12 is limited in above-mentioned scope, can ensures to there is enough large contact area between the three-dimensional gain face of test substance and metal column, and then ensure the sensitivity detecting.In a preferred embodiment of the present utility model, in metal column group, the vertical height of each metal column 12 is 6 μ m.
Metal column 12 is stochastic distribution, and density is 1 X 10 8individual/cm 2~6 X 10 8individual/cm 2.The metal column group who adopts the metal column 12 in this density range cycle to form has the average headway of about 400nm, not only ensure that test substance flows through smoothly in fluid channel 13, also ensured the contact area of the three-dimensional gain face of test substance and metal column simultaneously, ensure within the scope of minimum hot spot, to have a metal column at least, guaranteed the accuracy, sensitivity and the homogeneity that detect.In a specific embodiment, when metal column 12 is column structure, the diameter of metal column 12 is 10nm~400nm.
In the time detecting, in order to make light to pass through smoothly the first hard substrate 20, in one embodiment, the first hard substrate 20 is made up of the material of transparent and electrically conductive, is preferably made up of electro-conductive glass.The position of metal column 12 on the first hard substrate 20 can be set as required.In a preferred embodiment, metal column group arranges perpendicular to the first hard substrate 20 and the second hard substrate 30.Metal column group extends towards the thickness direction of the second hard substrate 30 since the first hard substrate 20.In other embodiment, metal column group also can arrange at an angle with the first hard substrate 20 and the second hard substrate 30.
As shown in Figure 1, in a specific embodiment, this test chip can also comprise the first tack coat 50 being separately positioned between the first hard substrate 20 and metal level 40, and is arranged on the second tack coat 60 between the second hard substrate 30 and metal level 40.Wherein, the first tack coat 50 is formed by electrically conducting transparent cementing agent.
According on the other hand of the present utility model, a kind of preparation method of micro-fluidic surface-enhanced Raman test chip is also provided, can comprise some steps described below.
In step S1, provide a template 10, the thickness direction that this template 10 has upper surface and lower surface and extends between upper surface and lower surface.Wherein, template 10 has multiple isolated through holes, and each through hole penetrates template 10 along the thickness direction of template 10.Wherein, through hole is of a size of nanometer scale on perpendicular to thickness direction.Set after template 10, in template 10, prepare SERS detection architecture.Electroplate for convenient, need to be connected on the first hard substrate 20 of a transparent and electrically conductive at the lower surface of template 10.
In step S2, adopt the metal material with SERS activity to form metal column 12 in each through hole of multiple through holes of template 10, thereby obtain a metal column group.In a specific embodiment, as shown in Figure 2, adopt electrochemical deposition method plated metal particle in the through hole of template 10, the template 10 of processing by electricity is placed in electroplate liquid and electroplates, and then prepares the metal column group with SERS activity.The electroplate liquid adopting is selected from containing the solution of the solution of the solution of gold ion, silver ion, copper ions with containing one or more in the solution of platinum ion.
In a preferred embodiment, can also on metal column group, continue deposition, thereby on metal column group, form metal covering film 14.Subsequently, the second hard substrate 30 can be set on metal covering film 14.
In step S3, remove the material of template 10, to expose metal column group, thereby between any two adjacent metal columns 12, form the fluid channel 13 of passing through for test substance.The material that preferably adopts corrosive liquid to erode template 10 forms fluid channel 13.In a kind of exemplary embodiments, template 10 can adopt polycarbonate template (Polycarbonate Membrane, PCM), and corrosive liquid can adopt methylene chloride.Can also adopt other some nano-pore mould materials, as adopted in other embodiments anodic oxidation aluminium formwork (Anodic Aluminum Oxide, AAO), now adopting mass percent concentration is 5% H 3pO 4solution is as corrosive liquid.
Step S4, encapsulates the metal column group with fluid channel 13, makes the detection zone of metal column group as micro-fluidic surface-enhanced Raman test chip, thereby obtains micro-fluidic surface-enhanced Raman test chip.
Further preparation technology's flow process is described below in conjunction with Fig. 1 to Fig. 3.In a specific embodiment, can first PCM template be fixed on the conducting surface of an electro-conductive glass with electrically conducting transparent glue.Then connect as shown in Figure 2 the negative pole of battery, and be placed in electroplate liquid silver ion mixed solution (10g/L AgNO 3, 5g/L EDTA, 50g/L Na 2sO 3, 20g/L K 2hPO 4) in.The positive pole of battery is connected with a cube electrode, is also placed in electroplate liquid.Reometer in circuit and voltage table are used for monitoring the growing state of metal column 12.In electroplate liquid, contain a large amount of Ag +, in the time of Closing Switch, Ag +attracted in the through hole of PCM template, as the Ag in through hole +while touching negative electrode, will obtain an electronics and be reduced into Ag simple substance.In Fig. 3, arrow A ' and A " represent respectively growth mid-term and the latter stage of silver-colored post.When beginning, deposition of silver is in the through hole of template, and as time goes by, silver-colored post is constantly grown in through hole, the complete filling vias of silver simple substance, and continue afterwards cross growth on the upper surface of template 10, finally join together, form the metal covering film 14 that covers upper surface.The surface that now with the naked eye can observe PCM template is silvery white in color, and this represents that growth course completes, and cut-off switch stops growing.Arrow B in Fig. 3 represents fixing step, adopts binary glue by bonding to metal covering film 14 and the second hard substrate 30 (as glass sheet).The step of C representative corrosion PCM template, will partly become chip to be placed in methylene chloride corrosive liquid and soak approximately 20 minutes, then use successively acetone, alcohol rinsing.Arrow D represents encapsulation step, encapsulating material polydimethylsiloxane and hardening agent is pressed to 10:1 proportion and mix, and then notes in mould, plugs microtubule, at 60 DEG C, heat 60 minutes, after PDMS is dried by its taking-up.PDMS/ micro-tubular structure after moulding and silver-colored rod structure are glued, complete like this encapsulation of micro-fluidic surface-enhanced Raman test chip.
In other embodiments, can also adopt some plastic package materials, as commercially available polymethylmethacrylate (PolymethylMethacrylate, PMMA), polystyrene (Polystyrene), nitrocellulose (Nitrocellulose), tygon (Poly (ethylene)) etc.
Fig. 4 is the realistic application conditions schematic diagram of micro-fluidic surface-enhanced Raman test chip of the present utility model.As shown in Figure 4, fluid molecule to be tested 3 is injected in fluid channel 13 to the surface that fluid molecule 3 can collide or adhere to metal column 12 with metal column 12 in flow process.If laser 1 is focused on to the surface of metal column, can cause that the Electronic Structure of metal column and laser 1 resonate, this doubly strengthens laser 1 and the interaction index of metal column, thereby has strengthened consumingly the Raman signal 2 of fluid molecule 3.Raman signal 2 can again be strengthened by nano-pillar again before scattering out.The enhancing process of this two step makes micro-fluidic surface-enhanced Raman test chip prepared by the utility model have the detection sensitivity of superelevation.The Raman signal 2 that can scatter out by detection like this, we just can monitor the fluid molecule 3 in microfluid.
So far, those skilled in the art will recognize that, illustrate and described of the present utility model multiple exemplary embodiment although detailed herein, but, in the situation that not departing from the utility model spirit and scope, still can directly determine or derive many other modification or the amendment that meet the utility model principle according to the disclosed content of the utility model.Therefore, scope of the present utility model should be understood and regard as and cover all these other modification or amendments.

Claims (10)

1. a micro-fluidic surface-enhanced Raman test chip, is characterized in that, comprising:
The first hard substrate (20);
The second hard substrate (30), with described the first hard substrate (20) opposing parallel setting; And
The metal level (40) being formed by the metal material with SERS activity, be arranged between described the first hard substrate (20) and described the second hard substrate (30), and extend to described the second hard substrate (30) by described the first hard substrate (20);
Wherein, described metal level (40) comprises the metal column group who is formed by multiple metal columns (12), metal column described in each (12) extends along the thickness direction from described the first hard substrate (20) to described the second hard substrate (30), and between any two adjacent described metal columns (12), forms for treating the fluid channel (13) that fluid measured is passed through in described metal column group.
2. test chip according to claim 1, is characterized in that, described metal column (12) is being of a size of nanometer scale perpendicular to the cross section on its bearing of trend.
3. test chip according to claim 1 and 2, it is characterized in that, described the first hard substrate (20) is made up of the material of transparent and electrically conductive, and described metal column group starts to extend towards the thickness direction of described the second hard substrate (30) from described the first hard substrate (20).
4. test chip according to claim 1, it is characterized in that, described metal level (40) also comprises the metal covering film (14) being positioned between described metal column group and described the second hard substrate (30), and described metal covering film (14) is one-body molded with described metal column group.
5. test chip according to claim 1, it is characterized in that, described micro-fluidic surface-enhanced Raman test chip also comprises the first tack coat being separately positioned between described the first hard substrate (20) and described metal level (40), and is arranged on the second tack coat between described the second hard substrate (30) and described metal level (40); Described the first tack coat is formed by electrically conducting transparent cementing agent.
6. test chip according to claim 1, is characterized in that, described metal column group arranges perpendicular to described the first hard substrate (20) and described the second hard substrate (30).
7. test chip according to claim 1, is characterized in that, in described metal column group, the vertical height of each described metal column (12) is 3 μ m~12 μ m.
8. test chip according to claim 7, is characterized in that, in described metal column group, the vertical height of each described metal column (12) is 6 μ m.
9. test chip according to claim 1, is characterized in that, the density of described metal column (12) is 1 X 10 8individual/cm 2~6 X 10 8individual/cm 2.
10. test chip according to claim 1, is characterized in that, when described metal column (12) is column structure, the diameter of described metal column (12) is 10nm~400nm.
CN201420232065.4U 2014-05-07 2014-05-07 Micro-fluidic surface-enhanced Raman test chip CN203929645U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104774756A (en) * 2015-04-23 2015-07-15 东南大学 Chip and method for microfluidic drug screening on basis of SERS (surface-enhanced Raman scattering) detection technology
CN104792767A (en) * 2015-05-08 2015-07-22 厦门大学 Microfluidic chip for SERS (surface-enhanced Raman scattering) detection by sol method and using method of microfluidic chip
CN105092555A (en) * 2014-05-07 2015-11-25 中国科学院物理研究所 Micro-fluidic surface enhanced Raman test chip and preparation method thereof
CN106153599A (en) * 2015-04-22 2016-11-23 吴世法 One has, without receptor nano titania metal film Raman chip and manufacture method
CN106323945A (en) * 2016-11-14 2017-01-11 无锡艾科瑞思产品设计与研究有限公司 Solid-phase-extraction-column-integrated surface-enhanced Raman detection chip

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105092555B (en) * 2014-05-07 2018-05-29 中国科学院物理研究所 Micro-fluidic surface-enhanced Raman test chip and preparation method thereof
CN105092555A (en) * 2014-05-07 2015-11-25 中国科学院物理研究所 Micro-fluidic surface enhanced Raman test chip and preparation method thereof
CN106153599B (en) * 2015-04-22 2019-12-10 大连世佩达光谱智能检测科技有限公司 receptor-containing and receptor-free titanium dioxide nano metal film Raman chip and manufacturing method thereof
CN106153599A (en) * 2015-04-22 2016-11-23 吴世法 One has, without receptor nano titania metal film Raman chip and manufacture method
CN104774756A (en) * 2015-04-23 2015-07-15 东南大学 Chip and method for microfluidic drug screening on basis of SERS (surface-enhanced Raman scattering) detection technology
CN104792767B (en) * 2015-05-08 2017-11-17 厦门大学 A kind of micro-fluidic chip and its application method for sol method SERS detections
CN104792767A (en) * 2015-05-08 2015-07-22 厦门大学 Microfluidic chip for SERS (surface-enhanced Raman scattering) detection by sol method and using method of microfluidic chip
CN106323945A (en) * 2016-11-14 2017-01-11 无锡艾科瑞思产品设计与研究有限公司 Solid-phase-extraction-column-integrated surface-enhanced Raman detection chip

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